Varian GC450 User Manual English PDF

Varian BV
Herculesweg 8
4330 EA Middelburg
The Netherlands
450-GC
User Manual
North/South America
2700 Mitchell Drive
Walnut Creek
94598 California, USA
Tel: ++(1)9259392400
Fax: ++(1)9259452360 or
++(1)9259452344
2008 Varian, Inc. All Rights Reserved
Europe
P.O. Box 8033
4330 EA Middelburg
The Netherlands
Tel: ++(31)118671000
Fax: ++(31)118623193
Produced in the Netherlands
Australia/East Asia
679 Springvale Road
Mulgrave, Victoria 3171
Australia
Tel: ++(61)395607133
Fax: ++(61)395607950
CP501411 Rev:1.1
March 2008
Warranty
Read Before Operating

Important Safeguards
The following items are frequently not recognized or are overlooked by new users while learning
to operate a Gas Chromatograph.
They are brought to your attention to safeguard against damage to your equipment.
1. Carrier gas must be flowing through the column before heating the column
oven. Carefully evaluate columns that have been heated with no carrier gas
flowing through and discard, if damaged. Ensure the Injector contains a septum
and there is a positive flow of carrier gas before heating the column.
2. Become familiar with the location and identity of Injector and detector options
prior to making settings at the GC keyboard and pneumatics panel. For
example, determine the physical location of the Injector you want to use (front,
middle, or rear) and identify the specific pneumatic controls associated with it
(Electronic Flow Control). Similarly, determine the physical location of the
detector you want to use and identify the specific pneumatic controls for this
detector.
3. Heating an ECD to elevated temperatures without carrier or make-up gas
flowing through it can damage the ECD cell. This can happen inadvertently
especially when the ECD is not in use. For this reason, it is recommended that
a low flow of carrier or make-up gas be maintained through an ECD at all times.
4.
If your system has a TCD, gas must be flowing through both channels to protect
the filaments. Turn power to filaments off when not in use.
Important Tips Regarding 450-GC Operation
Page:II
If a potentially hazardous Error is detected, such as a thermal runaway, the

450-GC shuts down the affected component and reports the Error on page 84.
After correcting the Error, normal operation is restored by powering the 450-GC
OFF then ON.
Using cryogenic column oven cooling, on page 73 leave always the Injectror(s)
/ Detector(s) heating ON (enable) and at a temperature of at least 100 C.
User Manual 450-GC
Varian, Inc.
Warranty
VARIAN ANALYTICAL INSTRUMENT WARRANTY

For Instrument Warranty in German, French, Italian or Spanish please refer to the 430-GC,
431-GC and 450-GC User Manual CD-rom (CP501414) which is included with the GC.
HARDWARE PRODUCTS
All analytical instruments sold by Varian are warranted to be free from defects in material and workmanship for the periods specified and
in accordance with the terms on the face of Varian's quotation or as otherwise agreed upon in writing between Varian and the Customer.
The warranty period begins on the date of shipment from Varian to the original Customer. However, where installation is paid for by the
Customer or included in the purchase price, the warranty period begins upon completion of installation. If the Customer schedules
installation to start later than 30 days after delivery or if such delay is caused through the Customer's inability to provide adequate
facilities or utilities or through failure to comply with Varian's reasonable pre-installation instructions or through other omissions by
Customer, then the warranty period starts on the 31st day from date of shipment. Moreover Varian will charge the Customer for labor and
other expenses involved in making multiple or follow-up installation service calls.
SOFTWARE PRODUCTS
Where software is provided within the frame of a license agreement concluded between the Customer and Varian, any warranty shall be
strictly in accordance with the terms of such agreement.
In the absence of a license agreement and unless an alternate warranty period is agreed upon in writing between Varian and the
Customer, the warranty period is as specified on the face of Varian's quotation. Varian warrants such software products, if used with and
properly installed on Varian hardware or other hardware as specified by Varian to perform as described in the accompanying Operator's
Manual and to be substantially free of those defects which cause failure to execute respective programming instructions; however, Varian
does not warrant uninterrupted or error-free operation.
REMEDIES
The sole and exclusive remedy under hardware warranty shall be repair of instrument malfunctions which in Varian's opinion are due or
traceable to defects in original materials or workmanship or, at Varian's option, replacement of the respective defective parts, provided
that Varian may as an alternative elect to refund an equitable portion of the purchase price of the instrument or accessory.
Repair or replacement under warranty does not extend the original warranty period.
Repair or replacement under warranty claims shall be made in Varian's sole discretion either by sending a Customer Support
Representative to the site or by authorizing the Customer to return the defective accessory or instrument to Varian or to send it to a
designated service facility. The Customer shall be responsible for loss or damage in transit and shall prepay shipping cost. Varian will
return the accessory or instrument to the Customer prepaid and insured. Claims for loss or damage in transit shall be filed by the
Customer. To correct software operation anomalies, Varian will issue software revisions where such revisions exist and where, in
Varian's opinion, this is the most efficient remedy.
LIMITATION OF WARRANTY
This warranty does not cover software supplied by the Customer, equipment and software warranted by another manufacturer or
replacement of expendable items and those of limited life, such as but not limited to: Filters, glassware, instrument status lamps, source
lamps, septa, columns, fuses, chart paper and ink, nebulizers, flow cells, pistons, seals, fittings, valves, burners, sample tubes, probe
inserts, print heads, glass lined tubing, pipe and tube fittings, variable temperature dewars, transfer lines, flexible discs, magnetic tape
cassettes, electron multipliers, filaments, vacuum gaskets, seats and all parts exposed to samples and mobile phases.
This warranty shall be void in the event of accident, abuse, alteration, misuse, neglect, breakage, improper operation or maintenance,
unauthorized or improper modifications or tampering, use in an unsuitable physical environment, use with a marginal power supply or use
with other inadequate facilities or utilities. Reasonable care must be used to avoid hazards.
This warranty is expressly in lieu of and excludes all other express or implied warranties, including but not limited to warranties
of merchantability and of fitness for particular purpose, use or application and all other obligations or liabilities on the part of
Varian, unless such other warranties, obligations or liabilities are expressly agreed to in writing by Varian.
LIMITATION OF REMEDIES AND LIABILITY

The remedies provided herein are the sole and exclusive remedies of the Customer. In no case will Varian be liable for
incidental or consequential damages, loss of use, loss of production or any other loss incurred.
Varian, Inc.
User Manual 450-GC
Page: III
Safety Information
SAFETY INFORMATION
For Safety Information in German, French, Italian or Spanish please refer to the 430-GC,
431-GC and 450-GC User Manual CD-rom (CP501414) which is included with the GC.
INFORMATION
To prevent any injury to the user or any damage to the instrument it is essential that you
read the information in this chapter and the GC user manual.
If this manual is not in your native language and if you have problems understanding the
text, we advise you to contact your Varian office for assistance. Varian cannot accept
responsibility for any damage or injury caused by misunderstanding of the information in
this manual.
OPERATING INSTRUCTIONS
This user manual is provided to help you establish operating conditions, which will
permit safe and efficient use of your equipment.
Special considerations and precautions are described in the manual, which appear in
the form of NOTES, CAUTIONS and WARNINGS as described on the next page.
It is important that you operate your equipment in accordance with this user manual and
any additional information, which may be provided by Varian. Address any questions
regarding the safe and proper use of your equipment to your local Varian office.
Page: IV
User Manual 450-GC
Varian, Inc.
Safety information
Information to aid you in

obtaining optimal
performance from your
instrument.
Warning Symbol
Alerts you to situations that

may cause moderate injury
and/or equipment damage
and how to avoid these
situations.
Alerts you to potentially

hazardous situations that
could result in serious injury
and how to avoid these
situations.
Warning Description
Hazardous voltages are present inside instrument.
Disconnect from main power before removing screwattached panels.
Hazardous chemicals may be present. Avoid contact,
especially when replenishing reservoirs. Use proper eye
and skin protection.
Very hot or cryogenically cold surfaces may be exposed.
Use proper skin protection.
Eye damage could occur either from flying particles,
chemicals, or UV radiation. Use proper eye and face
protection.
The potential for fire may be present. Follow manual
instructions for safe operation.
The potential for explosion may exist because of type of

gas or liquid used.
Ionizing radiation source is present. Follow manual

instructions for safe operation.
Keep hands and fingers away.
Varian, Inc.
User Manual 450-GC
Page: V
Safety Information
GENERAL SAFETY PRECAUTIONS

Follow these safety practices to ensure safe equipment operation.
Perform periodic leak checks on all supply lines and pneumatic plumbing.
Do not allow gas lines to become kinked or punctured. Place lines away
from foot traffic and extreme heat or cold.
Store organic solvents in fireproof, vented and clearly labeled cabinets so

they are easily identified as toxic and/or flammable materials.
Do not accumulate waste solvents. Dispose of such materials through a

regulated disposal program and not through municipal sewage lines.
This instrument has been tested per applicable requirements of
EMC Directive as required to carry the European Union CE Mark.
This instrument is designed for chromatographic analysis of
appropriately prepared samples. It must be operated using
appropriate gases and/or solvents and within specified maximum
ranges for pressure, flows and temperatures as described in this
manual. If the equipment is used in a manner not specified by the
manufacturer, the protection provided by the equipment may be
impaired.
It is the responsibility of the Customer to inform Varian Customer
Support Representatives if the instrument has been used for the
analysis of hazardous biological, radioactive, or toxic samples,
prior to any instrument service being performed or when an
instrument is being returned to the Service Center for repair.
Page: VI
User Manual 450-GC
Varian, Inc.
Safety information
ELECTRICAL HAZARDS
Disconnect the instrument from all power sources before removing protective
panels to avoid exposure to potentially dangerous voltages.
When it is necessary to use a non-original power cord plug, make sure the
replacement cord adheres to the color coding and polarity described in the preinstallation manual (P/N: CP01410) all local building safety codes.
Replace blown fuses with fuses of the size and rating stipulated on the fuse panel
or in the manual on page 44.
Make sure that voltage sources and line voltage match the value for which the
instrument is wired.
Replace faulty or frayed power cords immediately with the same type and rating.
COMPRESSED GAS CYLINDERS
Store and handle compressed gases carefully and in strict adherence to

safety codes.
Secure cylinders to an immovable structure or wall.
Store and move cylinders in an upright, vertical position. Before transport,

remove regulators and install cylinder cap.
Store cylinders in a well-ventilated area away from heat, direct sunshine,

freezing temperatures and ignition sources.
Mark cylinders clearly so there is no doubt as to their contents.
Use only approved regulators and connections.
Use only connector tubing that is chromatographically clean (Varian Part Number
03-918326-00) and has a pressure rating significantly greater than the highest
outlet pressure from the regulator.
Varian, Inc.
User Manual 450-GC
Page: VII
Safety Information
GC SAFETY PRACTICES
Exhaust System
No special exhaust ducting is necessary for GC detectors installed in a well-ventilated room
except when the detectors are used to test hazardous chemicals. If you do install ducting:
Use only fireproof ducting.
Install a blower at the duct outlet.
Secure air duct intakes such that their vibration or air movement does not effect
detector operation.
Check periodically for proper operation of the duct.

Ensure proper ventilation in lab area.
Radioactive Source Detectors

Read carefully and comply with all NOTES, CAUTIONS and WARNINGS in the Ni63 ECD
section on page 329 of this manual.
Perform the tests for removable radioactive contamination described in the Ni63 ECD
radiation manual (P/N: 03-913999-00). Comply with leak test schedules and procedures.
Burn Hazard
Heated or cryogenically cooled zones of the GC can remain hot or cold for a considerable
time after instrument power is turned off. To prevent painful burns, ensure that all heated or
cooled areas have returned to room temperature or wear adequate hand protection before
you touch potentially hot or cold surfaces.
Page: VIII
User Manual 450-GC
Varian, Inc.
Safety information
SPARE PARTS AVAILABILITY
SERVICE AVAILABILITY
It is the policy of Varian to provide operational spare parts for any instrument and
major accessory for a period of five (5) years after shipment of the final production
run of that instrument. Spare parts will be available after this five (5) year period
but on an as available basis. Operational spare parts are defined as those
individual electrical or mechanical parts that are susceptible to failure during their
normal operation. Examples include relays, lamps, temperature probes, detector
elements, motors, etc. Sheet metal parts, structural members or assemblies and
castings, printed circuit boards and functional modules are normally capable of
being rebuilt to like-new condition throughout their useful life and therefore will be
supplied only on an as available basis after the final production run of the
instrument.
Varian provides a variety of

services to support its customers
after warranty expiration. Repair
service can be provided by
attractively priced service
contracts or on a time and
material basis. Technical
support and training can be
provided by qualified personnel
on both a contractual or asneeded basis.
Varian Analytical Instruments Sales Offices

For Sales or Service assistance and to order Parts and Supplies, contact your local Varian
office. For the latest information visit www.varianinc.com.
Argentina
Buenos Aires
Tel. +54.11.4.783.5306
France
Les Ulis Cdex
Tel. +33.1.6986.3838
Russian Federation
Moscow
Tel. +7.095.937.4280
Australia
Mulgrave, Victoria
Tel. +61. 3.9560.7133
Germany
Darmstadt
Tel. +49.6151.7030
Spain
Madrid
Tel. +34.91.472.7612
Austria
Poettelsdorf
Tel. +43.2626.20090
India
Mumbai
Tel.
+91.22.2570.8595/97
Sweden
Solna
Tel. +46.8.445.1620
Benelux
Middelburg
Tel. +31.118.671500
Brazil and Latin America (S)
So Paulo
Tel. +55.11.32380400
Canada
Mississauga, Ontario
Tel. 800.387.2216
China
Beijing
Tel. +86.106310.8550
Europe
Middelburg, The Netherlands
Tel. +31.118.671.000
Varian, Inc.
Italy
Torino
Tel. +39.011.997.9111
Japan
Tokyo
Tel. +81.3.5232.1239
Korea
Seoul
Tel. +82.333.665.5171
Mexico and Latin
America (N)
Mexico City
Tel.
+52.5.55.5239465/026
United States
Walnut Creek, California,
USA
Tel. +1.800.926.3000
(GC and GC/MS)
Tel. +1.800.367.4752 (LC)
Switzerland
Steinhausen
Tel. +41.848.803.800
Taiwan
Shih-Chi
Tel. +886.22.698.9555
United Kingdom and
Ireland
Oxford
Tel. +44.1865.291500
http://www.varianinc.com/
Venezuela
Caracas
Tel.
+58.212.285.0320/2494
User Manual 450-GC
Page: IX
Safety Information
CE DECLARATION OF CONFORMITY
Page: X
User Manual 450-GC
Varian, Inc.
Table of Contents
TABLE OF CONTENTS
VARIAN ANALYTICAL INSTRUMENT WARRANTY................................................................. III
HARDWARE PRODUCTS .............................................................................................................. III
SOFTWARE PRODUCTS ............................................................................................................... III
REMEDIES .................................................................................................................................. III
LIMITATION OF WARRANTY .......................................................................................................... III
LIMITATION OF REMEDIES AND LIABILITY ...................................................................................... III
SAFETY INFORMATION.............................................................................................................IV
INFORMATION .............................................................................................................................IV
OPERATING INSTRUCTIONS .........................................................................................................IV
GENERAL SAFETY PRECAUTIONS ................................................................................................VI
ELECTRICAL HAZARDS ...............................................................................................................VII
COMPRESSED GAS CYLINDERS ..................................................................................................VII
GC SAFETY PRACTICES ...........................................................................................................VIII
Exhaust System.................................................................................................................VIII
Radioactive Source Detectors ...........................................................................................VIII
Burn Hazard.......................................................................................................................VIII
SPARE PARTS AVAILABILITY ........................................................................................................IX
SERVICE AVAILABILITY ................................................................................................................IX
CE DECLARATION OF CONFORMITY ..............................................................................................X
TABLE OF CONTENTS...............................................................................................................XI
FIGURES.................................................................................................................................. XXV
TABLES ................................................................................................................................. XXVII
INTRODUCTION ........................................................................................................................... 1
GUIDE TO THE 450-GC USER MANUAL ......................................................................................... 1
Abbreviations ........................................................................................................................ 1
BRIEF DESCRIPTION OF THE 450-GC ........................................................................................... 2
CONFIGURATION AND OPTIONS .................................................................................................... 3
INSTALLATION ............................................................................................................................ 5
NOTES ABOUT SETTING UP AND USING YOUR 450-GC................................................................. 5
PREPARING FOR INSTALLATION .................................................................................................... 5
Inspection ............................................................................................................................. 5
Unpacking............................................................................................................................. 5
Remove Protective Devices ................................................................................................. 6
Connect Data Handling Peripherals ..................................................................................... 6
Select Gases ........................................................................................................................ 7
Hydrogen as Carrier Gas...................................................................................................... 8
Varian, Inc.
User Manual 450-GC
Page: XI
Table of Contents
General laboratory precautions........................................................................................ 9

Operating precautions ...................................................................................................... 9
Install Gas Regulators and Set Pressures.......................................................................... 10
Connect Gases ................................................................................................................... 10
Installing the CP-8400/8410 AutoSampler ......................................................................... 11
Connect GC to Power .................................................................................................... 12
COLUMN INSTALLATION AND CONDITIONING ................................................................................ 13
Nuts and Ferrules for Capillary Columns............................................................................ 14
Connect Capillary Column to Injector ................................................................................. 15
Tips for Tightening Column Ferrules.............................................................................. 17
Nuts and Ferrules for Packed Columns.............................................................................. 18
Connect a Packed Column to the Injector .......................................................................... 18
Varian Test Column ............................................................................................................ 19
Identify Carrier Gas Controls and Turn on Flow................................................................. 19
Split Vent Flow and Septum Purge Flow ............................................................................ 20
Septum purge calibration ............................................................................................... 20
Set Carrier Gas Flow Rate to Condition Column................................................................ 22
Injector Conditioning ........................................................................................................... 22
Column Conditioning .......................................................................................................... 23
New Columns ................................................................................................................. 23
Used Columns................................................................................................................ 23
Connect Capillary Column to Detector ............................................................................... 24
Column Insertion Depths for Varian Detectors................................................................... 24
Connect Metal Packed Column to Detector ....................................................................... 25
Check for Leaks.................................................................................................................. 25
BASIC OPERATION ..................................................................................................................... 26
Setting Carrier and Detector Gas Flow Rates .................................................................... 26
Condition the GC System ................................................................................................... 28
Build a Method to Analyze a Test Sample.......................................................................... 28
Method to Analyze a Varian Test Sample on a Varian Test Column ................................. 29
Prepare the Test Sample.................................................................................................... 30
Solvents for GC .................................................................................................................. 31
Sample Volume and Injection Rate .................................................................................... 32
Inject the Test Sample ........................................................................................................ 32
REFERENCE .............................................................................................................................. 33
PERIPHERAL CONNECTORS................................................................................................... 33
PERIPHERAL CONNECTORS........................................................................................................ 34
J504/J505 S.I.D. 1 AND 2 ......................................................................................................... 35
J401 ANALOG OUT................................................................................................................... 36
J302 TEMPERATURE PROBES .................................................................................................... 37
J45/J46 AUXILIARY 1 AND 2....................................................................................................... 38
J44 CRYO VALVES (3) ............................................................................................................... 39
J42/J43 EXTERNAL EVENTS ...................................................................................................... 40
J41 HEATER CONNECTIONS ....................................................................................................... 41
REAR PANEL ............................................................................................................................ 42
OPTION BOARD ......................................................................................................................... 43
FUSES COMMON ....................................................................................................................... 44
Page: XII
User Manual 450-GC
Varian, Inc.
Table of Contents
Fuses .................................................................................................................................. 44
DISPLAY AND KEYBOARD ...................................................................................................... 45
STATUS INDICATION LEDS ........................................................................................................ 46
Overview Analytical Phases ............................................................................................... 46
Error LED............................................................................................................................ 47
MOST USED FUNCTIONS ............................................................................................................ 48
Status page......................................................................................................................... 49
Version Information............................................................................................................. 50
ADVANCED FUNCTIONS .............................................................................................................. 51
DISPLAY.................................................................................................................................... 52
Title Bar............................................................................................................................... 53
Main Operation screen ....................................................................................................... 54
Sample Delivery Screen ..................................................................................................... 55
Injector Screen.................................................................................................................... 57
Pressure and Flow screen .................................................................................................. 58
Oven Screen....................................................................................................................... 60
Methods Screen.................................................................................................................. 61
Detector Screen.................................................................................................................. 62
Analog Output ................................................................................................................ 63
Setup/Calibration ................................................................................................................ 64
Calibration ...................................................................................................................... 64
Setup .............................................................................................................................. 65
Configuration Tab........................................................................................................... 66
External Device .............................................................................................................. 67
Sample Delivery Tab ...................................................................................................... 68
Oven Tab........................................................................................................................ 73
Column Tab .................................................................................................................... 74
Detector Tab................................................................................................................... 75
Injector Tab..................................................................................................................... 77
Preferences Tab............................................................................................................. 78
System Tab .................................................................................................................... 79
Touch Screen Calibration............................................................................................... 81
Error/Log Handling.............................................................................................................. 84
LOCAL AUTOMATION............................................................................................................... 87
COMMUNICATIONS................................................................................................................... 89
Introduction ......................................................................................................................... 89
Ethernet Communications .................................................................................................. 89
How to set IP address in Galaxie Workstation using BOOTP (DHCP) .......................... 90
How to set a Fixed IP address in the 450-GC................................................................ 93
ANALOG CABLES ....................................................................................................................... 94
SAMPLE INTRODUCTION......................................................................................................... 97
AUTOSAMPLERS........................................................................................................................ 97
LIQUID INJECTORS ..................................................................................................................... 97
SAMPLING VALVES .................................................................................................................... 99
Heated Zones for Valves.............................................................................................. 100
Varian, Inc.
User Manual 450-GC
Page: XIII
Table of Contents
External Sample Introduction Systems............................................................................. 101

Pneumatic Systems .......................................................................................................... 101
CP-8400/8410 AUTOSAMPLER .............................................................................................. 103
INTRODUCTION ........................................................................................................................ 103
INSTALLING THE CP-8400/8410 .............................................................................................. 105
SAMPLER FIRST START UP ....................................................................................................... 110
LARGE SOLVENT / WASH VIAL .................................................................................................. 111
CALIBRATION .......................................................................................................................... 112
Vial calibration .................................................................................................................. 113
GC Injector calibration ...................................................................................................... 116
SYRINGE CHECK/REPLACE ...................................................................................................... 119
SYRINGE SIZE CHANGE ........................................................................................................... 120
OPERATION ............................................................................................................................. 121
PARAMETERS AND QUICK REFERENCE ..................................................................................... 121
SAMPLER CONFIGURATION ...................................................................................................... 122
SAMPLE DELIVERY PARAMETERS ............................................................................................. 123
Standard On-Column and Standard Split/Splitless Sampling Modes .............................. 124
Neat Sampling Mode ........................................................................................................ 126
Viscous Sampling Mode ................................................................................................... 128
Volatile Sampling Mode .................................................................................................... 129
User Defined Sampling Mode........................................................................................... 131
Page 1 .......................................................................................................................... 131
Page 2 .......................................................................................................................... 135
Page 3 .......................................................................................................................... 138
SPME Sampling Mode...................................................................................................... 140
INSTALLATION OF THE SPME MODE.......................................................................................... 142
Injector Insert .................................................................................................................... 145
Injector Temperature ........................................................................................................ 146
Sample Vials and Septa ................................................................................................... 146
Agitation Strokes............................................................................................................... 146
Sample Penetration Depth (%) .................................................................................... 147
SPME Adsorption Time ................................................................................................ 147
Number of Agitation Strokes ........................................................................................ 148
INSTALLATION OF THE LIQUID SAMPLING MODE ......................................................................... 149
THE 1177 SPLIT/SPLITLESS CAPILLARY INJECTOR ......................................................... 153
Features of the 1177 Injector............................................................................................ 154
Automatic Start Switch...................................................................................................... 154
1177 Injector Inserts ......................................................................................................... 154
1177 Modes of Injection.................................................................................................... 155
Split Mode..................................................................................................................... 155
Splitless Mode .............................................................................................................. 155
1177 Injector Screen......................................................................................................... 156
1177 Electronic Flow Control (EFC) ................................................................................. 157
1177 Manual Pneumatics ................................................................................................. 160
Operation of the 1177 Injector .......................................................................................... 160
Column Installation....................................................................................................... 160
Condition the Column................................................................................................... 160
Page: XIV
User Manual 450-GC
Varian, Inc.
Table of Contents
Column Installation in Detector .................................................................................... 160

Setting 1177 Gas Flow Rates........................................................................................... 161
EFC Pneumatics............................................................................................................... 161
Constant Column Flow ..................................................................................................... 162
Pressure Pulse ................................................................................................................. 163
Gas Saver......................................................................................................................... 164
Septum Purge Calibration ................................................................................................ 165
Manual Pneumatics .......................................................................................................... 166
Tools and equipment needed....................................................................................... 166
1177 Modes of Operation ................................................................................................. 167
Split Injection ................................................................................................................ 167
Splitless Injection .............................................................................................................. 168
Testing the 1177 Injector Performance ............................................................................ 169
1177 Injector Assembly .................................................................................................... 170
Maintenance ..................................................................................................................... 171
Tools Required ............................................................................................................. 171
Remove the Glass Insert .................................................................................................. 171
Replace the Glass Insert .................................................................................................. 172
Injector body cleaning....................................................................................................... 173
THE 1079 PTV INJECTOR ....................................................................................................... 175
Features of the 1079 PTV Injector.................................................................................... 176
1079 PTV Injector Inserts ................................................................................................. 176
1079 PTV Injector Assembly ............................................................................................ 177
1079 PTV Modes of Injection ........................................................................................... 178
Temperature Ramp Splitless Mode.............................................................................. 178
Large Volume ............................................................................................................... 178
Split Mode..................................................................................................................... 179
Isothermal Splitless Mode ............................................................................................ 179
On-Column Modes ....................................................................................................... 179
1079 Injector Screen......................................................................................................... 180
1079 PTV Electronic Flow Control (EFC) ......................................................................... 181
1079 PTV Manual Pneumatics ......................................................................................... 183
Operation of the 1079 PTV Injector .................................................................................. 183
Setting 1079 PTV Gas Flow Rates................................................................................... 184
EFC Pneumatics............................................................................................................... 184
Constant Column Flow ................................................................................................. 185
Pressure Pulse ................................................................................................................. 186
Gas Saver......................................................................................................................... 187
Manual Pneumatics .......................................................................................................... 189
Tools and equipment needed....................................................................................... 189
1079 PTV Modes of Operation ......................................................................................... 190
Isothermal Split Injection .............................................................................................. 190
Isothermal Splitless Injection........................................................................................ 191
Varian, Inc.
User Manual 450-GC
Page: XV
Table of Contents
Temperature Ramped Splitless Injection ..................................................................... 191

On-column Injection ..................................................................................................... 192
Large Volume Injection................................................................................................. 193
Testing the 1079 PTV Injector Performance .................................................................... 194
Maintenance ..................................................................................................................... 195
Tools Required ............................................................................................................. 195
CHROMATOPROBE .................................................................................................................. 198
How to Assemble the ChromatoProbe ............................................................................. 198
How to Install the ChromatoProbe.................................................................................... 198
Using the ChromatoProbe ................................................................................................ 200
How to Perform Analysis with the ChromatoProbe ...................................................... 200
Analysis of Thermally Labile Samples ......................................................................... 201
Using the ChromatoProbe Along with Traditional GC/MS ........................................... 202
Using the ChromatoProbe as a Dirty Sample Inlet ...................................................... 202
Cleaning............................................................................................................................ 204
Recommended Reading ................................................................................................... 204
THE 1041 ON-COLUMN INJECTOR........................................................................................ 205
1041 Injector Insert ........................................................................................................... 206
Injector Assembly and Insert ............................................................................................ 207
EFC Pneumatics............................................................................................................... 211
Flow Rates for Operation ............................................................................................. 212
Capillary Mode ............................................................................................................. 212
Packed Mode ............................................................................................................... 212
1041 Operation ................................................................................................................. 213
1041 Injector Method.................................................................................................... 213
Testing the 1041 Injector .................................................................................................. 214
Maintenance ..................................................................................................................... 215
Hardware Replacement and Cleaning Procedures...................................................... 215
Septum Replacement................................................................................................... 215
Needle/ Syringe Cleaning............................................................................................. 216
Leak Checking .................................................................................................................. 216
Syringe Leak Checking ................................................................................................ 217
THE 1061 FLASH VAPORIZATION INJECTOR...................................................................... 219
1061 Injector Insert ........................................................................................................... 224
Column Installation ........................................................................................................... 224
Page: XVI
User Manual 450-GC
Varian, Inc.
Table of Contents

EFC Pneumatics............................................................................................................... 225
Flow Rates for Operation ............................................................................................. 226
Capillary Mode ............................................................................................................. 226
Packed Mode ............................................................................................................... 226
1061 Flash Injector Operation .......................................................................................... 227
1061 Flash Injector Method.......................................................................................... 227
Testing the 1061 Flash Injector ........................................................................................ 228
MAINTENANCE ......................................................................................................................... 229
Replacing the 1061 Glass Insert ...................................................................................... 229
1093 SEPTUM-EQUIPPED PROGRAMMABLE INJECTOR (SPI) ......................................... 231
1093 Injector Parts............................................................................................................ 234
Glass Insert....................................................................................................................... 237
Syringe.............................................................................................................................. 237
Mounting the Column........................................................................................................ 238
Column Installation ........................................................................................................... 238
Condition the Column ....................................................................................................... 238
Column Installation in Detector......................................................................................... 238
Connecting CO2 to the 1093 Injector................................................................................ 238
Connecting LN2 to the 1093 Injector ................................................................................ 239
EFC Pneumatics............................................................................................................... 241
1093 Injector Operation .................................................................................................... 242
Testing the 1093 Injector Performance ............................................................................ 243
Maintenance ..................................................................................................................... 245
Septum Replacement ....................................................................................................... 245
Removal of Glass Insert ............................................................................................... 245
Removal ....................................................................................................................... 245
Re-assemble ................................................................................................................ 246
Leak Checking .................................................................................................................. 247
Leak Checking the Injector Only .................................................................................. 247
Gas Leak Checking ...................................................................................................... 247
Visual Leak Checking................................................................................................... 248
Syringe Leak Checking ................................................................................................ 248
Injector and Column Conditioning .................................................................................... 248
Baking Out the Injector................................................................................................. 248
SAMPLE PRECONCENTRATION TRAP (SPT) ...................................................................... 251
Description........................................................................................................................ 251
SPT temperature zone...................................................................................................... 252
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Two trap sizes available ................................................................................................... 253

Using the SPT................................................................................................................... 253
Trapping Methodology.................................................................................................. 253
Trapping Media ............................................................................................................ 253
Trap Dimensions .......................................................................................................... 254
Trap Temperature ........................................................................................................ 254
Trapping and Desorption.............................................................................................. 254
Electrical System .............................................................................................................. 255
Circuit breaker .............................................................................................................. 256
LCO2 Option...................................................................................................................... 257
System Description ...................................................................................................... 257
Theory of Operation ..................................................................................................... 258
Characteristics of LCO2 as a Coolant........................................................................... 258
Inadequate Cooling ...................................................................................................... 258
Transfer Line ................................................................................................................ 259
Recommended Supply Conditions............................................................................... 259
LN2 Option ........................................................................................................................ 260
Description.................................................................................................................... 260
Recommended Supply Conditions............................................................................... 261
Recommended temperature ranges ............................................................................ 261
Configuring the SPT ......................................................................................................... 262
Building an SPT method ................................................................................................... 263
Replacing the Trap Assembly........................................................................................... 264
SPT System Components ................................................................................................ 265
Remove the SPT Cover.................................................................................................... 266
Detach Trap Assembly ..................................................................................................... 267
Remove Cryo Nozzle Assembly ....................................................................................... 268
Installing the Trap Assembly ............................................................................................ 269
Trap Conditioning ............................................................................................................. 273
Replacement SPT traps.................................................................................................... 274
SPT replacement parts ..................................................................................................... 275
Troubleshooting ................................................................................................................ 276
DETECTORS ............................................................................................................................ 279
INTRODUCTION ........................................................................................................................ 279
ANALOG OUTPUT .................................................................................................................... 280
FLAME IONIZATION DETECTOR (FID) .................................................................................. 283
Initial Set-Up ..................................................................................................................... 284
Operation .......................................................................................................................... 285
FID auto-Ignite flow diagram ............................................................................................ 287
Installation/Disassembly ................................................................................................... 288
Exploded View.............................................................................................................. 288
Disassemble the FID .................................................................................................... 289
Reassemble the FID..................................................................................................... 290
MAINTENANCE ......................................................................................................................... 292
Clean the Flame Tip and Internal Parts............................................................................ 292
Replace the Flame-Tip Ferrule......................................................................................... 293
FID Test Chromatogram ................................................................................................... 293
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Table of Contents
PULSED DISCHARGE HELIUM IONIZATION DETECTOR (PDHID)..................................... 295

HELIUM IONIZATION (PDHID)................................................................................................... 296
Cable overview ................................................................................................................. 297
Exploded View .................................................................................................................. 298
Gas Connections .............................................................................................................. 299
Installation......................................................................................................................... 299
General Precautions ......................................................................................................... 300
Installing and Purging the Helium Purifier ........................................................................ 300
Connecting the Discharge Gas to the Detector................................................................ 301
Capillary Column Connection ........................................................................................... 301
Packed Column Connection ............................................................................................. 302
Testing for Leaks .............................................................................................................. 303
THERMIONIC SPECIFIC DETECTOR (TSD) .......................................................................... 305
Initial Set-Up ..................................................................................................................... 306
Operation and Operating Recommendations................................................................... 307
Bead Conditioning ........................................................................................................ 307
Optimization of the TSD Using the Varian Test Sample .............................................. 309
Determining Optimum Hydrogen Flow ......................................................................... 309
Maintaining Optimum Conditions ................................................................................. 310
Column Bleed ............................................................................................................... 311
Solvent Considerations ................................................................................................ 311
Chlorinated Solvents .................................................................................................... 311
Effect of Silylation Reagents ........................................................................................ 312
TSD Assembly .................................................................................................................. 313
Exploded view .............................................................................................................. 313
TSD disassembly ......................................................................................................... 314
TSD Re-assembly ........................................................................................................ 315
MAINTENANCE ......................................................................................................................... 317
Cleaning / Maintenance .................................................................................................... 317
Bead Cleaning .................................................................................................................. 317
Flame Tip and Internal Parts Cleaning ............................................................................. 317
Replace the Flame-Tip Ferrule......................................................................................... 318
Test Chromatogram.......................................................................................................... 318
THERMAL CONDUCTIVITY DETECTOR (TCD) ..................................................................... 319
Before Operating the TCD................................................................................................ 320
Initial Set-Up ..................................................................................................................... 320
TCD Adjustments ......................................................................................................... 322
Operation .......................................................................................................................... 323
Range Setting............................................................................................................... 325
Low Currents (100-150 mA) ......................................................................................... 325
High Currents (300 mA) ............................................................................................... 326
Calculate Detector Sensitivity....................................................................................... 327
Calculate Detector Detectivity ...................................................................................... 328
Adjust TCD Carrier Gas Flow Rates................................................................................. 328
MAINTENANCE ......................................................................................................................... 328
TCD Test Chromatogram ................................................................................................. 328
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ELECTRON CAPTURE DETECTOR (ECD) ............................................................................ 329

Initial Set-up...................................................................................................................... 330
ECD Adjustments ............................................................................................................. 331
Cell-Current .................................................................................................................. 331
Time Constant Switch .................................................................................................. 331
Setting the Contact Potential........................................................................................ 332
ECD Operation ............................................................................................................. 333
Column and Septum Bleed .......................................................................................... 333
Column Conditioning .................................................................................................... 333
Column Oven and Detector Oven Temperature Selection .......................................... 333
ECD Pneumatics .............................................................................................................. 334
Installation/Disassembly ................................................................................................... 335
Exploded View .................................................................................................................. 335
ECD Installation ................................................................................................................ 337
MAINTENANCE ......................................................................................................................... 340
Thermal Cleaning With Carrier Gas ................................................................................. 340
PULSED FLAME PHOTOMETRIC DETECTOR (PFPD)......................................................... 343
Description........................................................................................................................ 343
Basic Components of the PFPD....................................................................................... 343
Features of the PFPD Assembly ...................................................................................... 344
Features of the PFPD Electrometer Board....................................................................... 346
Theory of Operation of the PFPD ..................................................................................... 346
Stages of Flame Pulsation................................................................................................ 347
How Does the PFPD Achieve its Greater Detectivity and Selectivity?............................. 348
Background Emission in a Pulsed-flame...................................................................... 348
Time-dependence of Emission Profiles........................................................................ 348
Emission Profiles.......................................................................................................... 348
Concentration (in time) of the Emitted Light................................................................. 349
Separation of the Element Emission from Background Emission................................ 349
Effect of Gate Control................................................................................................... 350
Adjustment of the Gas Composition............................................................................. 351
PFPD Flow Path ............................................................................................................... 351
References ....................................................................................................................... 352
Specifications.................................................................................................................... 352
Installation......................................................................................................................... 354
Inspecting the PFPD......................................................................................................... 354
PFPD Accessory Kit ......................................................................................................... 354
PFPD Diffusion Source Kit ............................................................................................... 355
Installing a Chromatographic Column .............................................................................. 356
Prepare the Column End .................................................................................................. 356
Disassemble the PFPD..................................................................................................... 357
Remove the Detector Tower (Optional)............................................................................ 359
Insert the Column ............................................................................................................. 360
Reassemble the PFPD ..................................................................................................... 361
Operation ......................................................................................................................... 363
Adjusting the Gas Flow Rates .......................................................................................... 363
Split Valve......................................................................................................................... 363
PFPD Gas Flow Diagram with EFC15.............................................................................. 364
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Adjust the Gas Flow Rates ............................................................................................... 365

Calibrating the Flow Controllers ....................................................................................... 366
Optimizing the PFPD ........................................................................................................ 368
Detectivity ......................................................................................................................... 368
Selectivity.......................................................................................................................... 368
Throughput ....................................................................................................................... 368
Suggested Fuel Gas Flow Rates...................................................................................... 369
Optimization Criteria ......................................................................................................... 370
Establishing Tick-Tock...................................................................................................... 375
Photomultiplier Tube (PMT) High Voltage ........................................................................ 378
Adjusting the Photomultiplier Tube (PMT) Voltage .......................................................... 378
Optimizing the PFPD ........................................................................................................ 379
Repeated Injections of Standard ...................................................................................... 379
Continuous Infusion of Standard ...................................................................................... 381
Testing the PFPD Performance........................................................................................ 382
PFPD Test Chromatogram: Sulfur Performance.............................................................. 385
PFPD Test Chromatogram: Phosphorus Performance .................................................... 386
Detectivity ......................................................................................................................... 386
PFPD Test Chromatogram: Sulfur Detectivity .................................................................. 387
PFPD Test Chromatogram: Phosphorus Detectivity ........................................................ 388
Using the Gate Delay and Gate Width Parameters.......................................................... 388
Setting the Trigger Level................................................................................................... 390
Setting Gate Delay and Gate Width ................................................................................. 392
Set Gate Width ................................................................................................................. 393
Building a GC Method....................................................................................................... 394
Building a GC Workstation Method .................................................................................. 395
Quantitation ...................................................................................................................... 396
Peak Area Quantitation..................................................................................................... 396
Peak Height Quantitation.................................................................................................. 397
Peak Resolution with the PFPD ....................................................................................... 397
Quantitation in the Sulfur Mode ........................................................................................ 397
Square Root Function....................................................................................................... 398
How to Minimize Quenching of Sulfur Response ............................................................. 398
Advanced Operation ......................................................................................................... 399
Theory of Operation.......................................................................................................... 399
Table of Optimum Flow Rates .......................................................................................... 400
Installation of the Nitrogen Mode Parts ............................................................................ 400
Nitrogen Mode Operation ................................................................................................. 402
Parts and Supplies (Nitrogen Mode) ................................................................................ 403
Phosphorus Mode Operation............................................................................................ 403
Sulfur Mode Operation...................................................................................................... 403
Options to Aid Optimization with Other Elements ............................................................ 403
Multi-element Detection .................................................................................................... 404
Arsenic Selective Detection.............................................................................................. 404
Emission Wavelengths ..................................................................................................... 404
Emission Timing ............................................................................................................... 404
Flame Composition........................................................................................................... 404
Filters ................................................................................................................................ 405
Selenium Selective Detection........................................................................................... 405
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Table of Contents

Emission Timing ............................................................................................................... 406
Filters ................................................................................................................................ 406
Tin Selective Detection ..................................................................................................... 406
Emission Timing ............................................................................................................... 407
Filters ................................................................................................................................ 407
Manganese Selective Detection ....................................................................................... 407
Emission Timing ............................................................................................................... 408
Filters ................................................................................................................................ 408
Maintaining the PFPD....................................................................................................... 409
Replacing the Optical Filter .............................................................................................. 409
Changing the Combustor Size.......................................................................................... 411
Replacing a Dirty Combustor............................................................................................ 411
Ordering Parts and Supplies for the PFPD....................................................................... 412
Troubleshooting ................................................................................................................ 414
Overview........................................................................................................................... 414
Flame Does Not Ignite ...................................................................................................... 414
Baseline Noise is Too High .............................................................................................. 415
Baseline is Erratic (tick-tock) ............................................................................................ 417
DETECTOR TEST CHROMATOGRAMS................................................................................. 419
FID Test Mix ..................................................................................................................... 420
TSD Test Mix .................................................................................................................... 421
TCD Test Mix.................................................................................................................... 422
ECD Test Mix.................................................................................................................... 423
PFPD P Mode................................................................................................................... 424
PFPD S Mode................................................................................................................... 425
GENERAL GC MAINTENANCE............................................................................................... 427
Overview........................................................................................................................... 427
General GC Maintenance ................................................................................................. 428
Check and Renew Gas Supplies ................................................................................. 428
Leak Check....................................................................................................................... 428
Gas Purifier Replacement................................................................................................. 430
Injector Maintenance ........................................................................................................ 432
Septum Replacement................................................................................................... 432
Instructions for High-Temperature bakeout of Injectors............................................... 433
Injector specified maintenance ......................................................................................... 436
Detector specified maintenance ....................................................................................... 436
Pencil Filter ....................................................................................................................... 437
SHIPPING, CLEANING AND DISPOSAL INSTRUCTIONS.................................................... 439
SHIPPING INSTRUCTIONS ......................................................................................................... 439
CLEANING INSTRUCTIONS ........................................................................................................ 439
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Varian, Inc.
Table of Contents
DISPOSAL INSTRUCTIONS......................................................................................................... 439

REPLACEMENT PARTS.......................................................................................................... 441
Injector Liners/Inserts ....................................................................................................... 443
Liner/Insert Descriptions ................................................................................................... 445
TECHNICAL TIPS..................................................................................................................... 457
CHROMATOGRAPHIC INTERPRETATIONS ................................................................................... 458
TO BLEED OR NOT TO BLEED THAT IS THE QUESTION ............................................................ 461
The baseline below 250 C............................................................................................... 461
Injector contamination....................................................................................................... 462
The Column ...................................................................................................................... 463
Gas Impurities................................................................................................................... 465
CHOOSING THE RIGHT GC INJECTION TECHNIQUE ..................................................................... 466
Direct Injection .................................................................................................................. 467
Description ............................................................................................................... 467
Split Injection .................................................................................................................... 467
Description ............................................................................................................... 467
Splitless Injection .............................................................................................................. 468
Description ............................................................................................................... 468
Cool on-column................................................................................................................. 470
Description ............................................................................................................... 470
Programmed Temperature Vaporizer (PTV) .................................................................... 470
Description ............................................................................................................... 470
Cold Split Injection........................................................................................................ 471
Cold Splitless Injection ................................................................................................. 471
Solvent Venting ............................................................................................................ 471
GC LINER LABYRINTH - HOW TO CHOOSE THE RIGHT INJECTOR INSERT ...................................... 472
Liner Types ....................................................................................................................... 472
Liner volume ..................................................................................................................... 473
Injector heat capacity........................................................................................................ 473
Discrimination effects........................................................................................................ 474
Liners for splitless injections ............................................................................................. 475
Straight liner ................................................................................................................. 475
Gooseneck ................................................................................................................... 475
Gooseneck with wool ................................................................................................... 475
Double Gooseneck....................................................................................................... 475
Recessed Gooseneck .................................................................................................. 476
Liners for split injections ................................................................................................... 476
Frit Splitter .................................................................................................................... 476
Inverted -or Laminar Cup Splitter ................................................................................. 476
Baffle Splitter ................................................................................................................ 476
Liners for direct injections ................................................................................................. 477
Straight tube ................................................................................................................. 477
Gooseneck ................................................................................................................... 477
APPENDIX A: ERROR CODES .............................................................................................. 479
APPENDIX B: PUBLIC STATEMENT..................................................................................... 491
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Varian, Inc.
Table of Contents
FIGURES
FIGURE 1: COLUMN ENDS .............................................................................................................. 15
FIGURE 2: CONNECTORS FOR PERIPHERAL EQUIPMENT .................................................................. 34
FIGURE 3: CONNECTOR J504-J505................................................................................................ 35
FIGURE 4: CONNECTOR J401......................................................................................................... 36
FIGURE 5: CONNECTOR J302......................................................................................................... 37
FIGURE 6: CONNECTOR J45/J46 .................................................................................................... 38
FIGURE 7: CONNECTOR J44........................................................................................................... 39
FIGURE 8: CONNECTOR J42/J43 .................................................................................................... 40
FIGURE 9: CONNECTOR J41........................................................................................................... 41
FIGURE 10: OPTION BOARD ........................................................................................................... 43
FIGURE 11: 450-GC BACK-PANEL ETHERNET CONNECTION ............................................................ 89
FIGURE 12: PNEUMATIC SYSTEMS FOR LIQUID INJECTORS AND SAMPLING VALVES ......................... 101
FIGURE 13: TOP-COVER FOR SAMPLER ........................................................................................ 105
FIGURE 14: SPME SYRINGE AND HOLDER FIGURE 15: SPME/STANDARD SWITCH ....................... 142
FIGURE 16: SPME SYRINGE ........................................................................................................ 145
FIGURE 17: LIQUID SAMLING SYRINGE AND HOLDER FIGURE 18: SPME/STANDARD SWITCH ....... 149
FIGURE 19: EFC21 AND 1177 IN SPLIT MODE FLOW DIAGRAM....................................................... 157
FIGURE 20: EFC21 AND 1177 IN SPLITLESS MODE FLOW DIAGRAM ............................................... 158
FIGURE 21: EFC25 AND 1177 FLOW DIAGRAM ............................................................................. 159
FIGURE 22: 1177 INJECTOR ASSEMBLY ........................................................................................ 170
FIGURE 23: 1079 PTV INJECTOR ASSEMBLY ................................................................................ 177
FIGURE 24: EFC21 AND 1079 IN SPLIT MODE FLOW DIAGRAM....................................................... 181
FIGURE 26: CHROMATOPROBE ASSEMBLY .................................................................................... 199
FIGURE 27: 1041 ON-COLUMN INJECTOR WITH INSERT ................................................................. 207
FIGURE 30: 1061 FLASH VAPORIZATION INJECTOR WITH INSERT .................................................... 221
FIGURE 33: 1093 INJECTOR ASSEMBLY ........................................................................................ 234
FIGURE 36: CONNECTION CO2 TANK TO GC.................................................................................. 238
FIGURE 37: SPT ELECTRICAL DIAGRAM........................................................................................ 256
FIGURE 38: LCO2 COOLANT FLOW DIAGRAM ................................................................................ 257
FIGURE 39: LN2 COOLANT FLOW DIAGRAM ................................................................................... 260
FIGURE 40: SPT COMPONENTS (SHORT TRAP ASSEMBLY, LCO2 OPTION SHOWN.......................... 265
FIGURE 41: REMOVING SPRINGS FROM TRAP ASSEMBLY ............................................................... 267
FIGURE 42: CRYO NOZZLE ASSEMBLY .......................................................................................... 268
FIGURE 43: FID AUTO-IGNITE FLOW DIAGRAM ............................................................................... 287
FIGURE 44: FID EXPLODED VIEW ................................................................................................. 288
FIGURE 45: ORIENTATION OF IGNITOR PROBE ELEMENTS IN FID TOWER ........................................ 291
FIGURE 46: FID CROSS-SECTIONAL VIEW ..................................................................................... 291
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FIGURE 47: SCHEMATIC OF THE PDHID DETECTOR ...................................................................... 296

FIGURE 48: PDHID CABLE OVERVIEW.......................................................................................... 297
FIGURE 49: PDHID EXPLODED VIEW............................................................................................ 298
FIGURE 50: PDHID GAS CONNECTIONS OVERVIEW ...................................................................... 299
FIGURE 51: STRUCTURE OF COMPONENTS IN THE TSD TEST SAMPLE & CHROMATOGRAM EXAMPLES
........................................................................................................................................... 310
FIGURE 52: TSD EXPLODED VIEW ................................................................................................ 313
FIGURE 53: TSD CROSS-SECTIONAL VIEW ................................................................................... 316
FIGURE 54: TCD SENSITIVITY AND AMPLIFICATION ........................................................................ 326
FIGURE 55: ECD EXPLODED VIEW ............................................................................................... 335
FIGURE 56: RADIOACTIVE CAUTION LABEL GENERAL LICENSE DEVICE ........................................ 338
FIGURE 57: RADIOACTIVE CAUTION LABEL SPECIFIC LICENSE ..................................................... 338
FIGURE 58: RADIOACTIVE CAUTION LABEL .................................................................................... 339
FIGURE 59: PFPD ASSEMBLY ...................................................................................................... 344
FIGURE 60: FID TEST MIX CHROMATOGRAM ................................................................................. 420
FIGURE 61: TSD TEST MIX CHROMATOGRAM ............................................................................... 421
FIGURE 62: TCD TEST MIX CHROMATOGRAM ............................................................................... 422
FIGURE 63: ECD TEST MIX CHROMATOGRAM ............................................................................... 423
FIGURE 64: PFPD P MODE TEST MIX CHROMATOGRAM................................................................ 424
FIGURE 65: PFPD S MODE TEST MIX CHROMATOGRAM................................................................ 425
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User Manual 450-GC
Varian, Inc.
Table of Contents
TABLES
TABLE 1: HYDROGEN AS CARRIER GAS DURING POWER OFF.............................................................. 8
TABLE 2: GAS INLET PRESSURE ...................................................................................................... 10
TABLE 3: FACTORY-INSTALLED INJECTOR INSERTS .......................................................................... 13
TABLE 4: 1/16 COLUMN FERRULES................................................................................................ 14
TABLE 5: MAXIMUM INSERT DEPTH FOR CAPILLARY COLUMN IN INJECTOR ........................................ 16
TABLE 6: GENERAL TIGHTENING AND RE-TIGHTENING FOR COMMON FERRULES ............................... 17
TABLE 7: VARIAN TEST COLUMNS ................................................................................................... 19
TABLE 8: INJECTOR AND EFC TYPE COMBINATION ........................................................................... 19
TABLE 9: COLUMN CONDITION HEAD PRESSURE ............................................................................... 22
TABLE 10: FLOW RATES FOR CARRIER AND DETECTOR GASES ........................................................ 26
TABLE 11: DETECTOR MANUAL FLOW RATES ................................................................................... 27
TABLE 12: VARIAN TEST SAMPLES ................................................................................................. 29
TABLE 13: VARIAN TEST SAMPLE 1041 AND 1061 CONDITIONS ....................................................... 29
TABLE 14: VARIAN TEST SAMPLE 1177 AND 1079 CONDITIONS ....................................................... 30
TABLE 15: RECOMMENDED SOLVENTS FOR GAS CHROMATOGRAPHY ............................................... 31
TABLE 16: USED FUSES ................................................................................................................. 44
TABLE 17: STATUS INDICATION LED'S ............................................................................................ 46
TABLE 18: ERROR LED.................................................................................................................. 47
TABLE 19: INJECTOR EFC MODULES .............................................................................................. 59
TABLE 20: DETECTOR EFC MODULES ............................................................................................ 63
TABLE 21: SAMPLER/INJECTOR POSITION ........................................................................................ 69
TABLE 22: VALVE TYPE NAMES ...................................................................................................... 72
TABLE 23: ANALOG CABLES ........................................................................................................... 95
TABLE 24: INJECTION MODE PARAMETERS FOR ON-COLUMN .......................................................... 125
TABLE 25: INJECTION MODE PARAMETERS FOR SPLIT-/SPLITLESS .................................................. 126
TABLE 26: INJECTION MODE PARAMETERS FOR NEAT ..................................................................... 128
TABLE 27: INJECTION MODE PARAMETERS FOR VISCOUS ............................................................... 129
TABLE 28: INJECTION MODE PARAMETERS FOR VOLATILE............................................................... 130
TABLE 29: SPLIT INJECTION TYPICAL CONDITIONS ......................................................................... 167
TABLE 30: SPLITLESS INJECTION METHOD PARAMETERS ............................................................... 168
TABLE 31: DETECTOR TEST SAMPLES .......................................................................................... 169
TABLE 32: 1177 COLUMN FERRULES 1/16"................................................................................... 170
TABLE 33: 1079 COLUMN FERRULES 1/16"................................................................................... 177
TABLE 34: SPLIT INJECTION TYPICAL CONDITIONS ......................................................................... 190
TABLE 35: ISOTHERMAL SPLITLESS INJECTION METHOD PARAMETERS ........................................... 191
TABLE 36: TEMPERATURE RAMPED SPLITLESS INJECTION ............................................................. 192
TABLE 37: ON-COLUMN INJECTION ............................................................................................... 193
TABLE 38: LARGE VOLUME INJECTION .......................................................................................... 194
TABLE 39: 1079 PTV TEST SAMPLES ........................................................................................... 194
TABLE 40: 1041 COLUMN FERRULES 1/16" X 0.8 MM .................................................................... 207
TABLE 41: CARRIER GAS FLOW RATES FOR 1041 ......................................................................... 212
TABLE 42: 1041 INJECTOR CHROMATOGRAPHIC TESTING CONDITIONS ........................................... 214
TABLE 43: 1061 COLUMN FERRULES 1/16" X 0.8 MM .................................................................... 221
TABLE 44: CARRIER GAS FLOW RATES FOR 1061 FLASH INJECTOR ............................................... 226
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TABLE 45: 1061 FLASH INJECTOR CHROMATOGRAPHIC TESTING CONDITIONS................................ 228

TABLE 47: DETECTABLE GAS LEAK CHECKING .............................................................................. 247
TABLE 48: SPT RECOMMENDED OPERATING RANGES .................................................................... 261
TABLE 49: SPT TRAP CONDITIONING ............................................................................................ 273
TABLE 50: SPT REPLACEMENT TRAPS .......................................................................................... 274
TABLE 51: SPT REPLACEMENT PARTS ......................................................................................... 275
TABLE 52: ECD GASES, PRESSURES, PURITY AND FLOW RATES ................................................... 334
TABLE 53: SPECIFICATIONS PFPD ............................................................................................... 352
TABLE 54: SPECIFICATIONS NITROGEN MODE PFPD..................................................................... 353
TABLE 55: ACCESSORY KIT PFPD ............................................................................................... 354
TABLE 56: DIFFUSION SOURCE KIT PFPD .................................................................................... 355
TABLE 57: FLOW RATES PFPD .................................................................................................... 369
TABLE 58: PRESET VALUES PFPD ............................................................................................... 389
TABLE 59: RECOMMENDED SETTINGS FOR COMMON ELEMENTS ..................................................... 392
TABLE 60: OPTIMUM FLOW RATES PFPD...................................................................................... 400
TABLE 62: MAINTENANCE FREQUENCY ......................................................................................... 427
TABLE 63: VARIAN GAS CLEAN FILTERS ....................................................................................... 431
TABLE 64: INJECTOR BAKEOUT PARTS .......................................................................................... 433
Page: XXVIII
User Manual 450-GC
Varian, Inc.
Introduction
INTRODUCTION
GUIDE TO THE 450-GC USER MANUAL
The purpose of this User Manual is to provide instructions for the safe
installation and operation of the Varian 450-GC (Gas Chromatograph).
Abbreviations
The following abbreviations can appear in this Manual:
Varian, Inc.
AC
DC
alternating current
direct current
ECD
EFC
FID
PFPD
TCD
TSD
Electron Capture Detector

Electronic Flow Control
Flame Ionization Detector
Pulsed Flame Photometric Detector
Thermal Conductivity Detector
Thermionic Specific Detector
GC
GC/MS
Gas Chromatograph
Gas Chromatograph/Mass Spectrometer
ID
OD
Inner Diameter
Outer Diameter
P/N
Part Number
LUI
S.I.D.
Local User Interface

Sample Introduction Device connector
kPa
psi
Kilo Pascal gauge

Pounds per squari inch gauge
User Manual 450-GC
Page: 1
Introduction
BRIEF DESCRIPTION OF THE 450-GC

The following are some of the key features of the 450-GC:
Page: 2
Injectors, columns and detectors can be installed and operated simultaneously.
The 1079 PTV Injector provides 5 modes of injection - isothermal split and splitless,
temperature ramped splitless, on-column and large volume.
Electronic or manual control of carrier and detector gas.
Ethernet communications with full networking capability.
A full suite of universal and selective detectors - FID, TCD, ECD, TSD (N, P), PFPD
(S, P, N, C, Metals), PDHID and Ion Trap MS.
Large, swing-out pneumatics for easy access.
7 heated zones and 7 external events (24 Volt) for maximum flexibility and custom
configurations.
Option board with 8 external events (24 Volt) available, also 3 analog outputs with
output voltage 0-1 and 0-10 Volt.
Up to 99 separately programmed and stored analytical methods.
Intuitive, function-based keyboard, LCD display with touch-screen for ease of use in
instrument handling.
Built-in Custom Solutions capability - valved systems, custom plumbing, six-position

valve oven, methanizer.
Large column oven for easy access and installation of up to three analytical
columns.
A complete range of GC automation and sample preparation techniques - , the

CP-84X0 AutoSamplers, Solid Phase MicroExtraction, Purge and Trap, Heated
Headspace and the Archon Purge and Trap AutoSampler.
User Manual 450-GC
Varian, Inc.
Introduction
CONFIGURATION AND OPTIONS

The 450-GC has seven heated zones, one of which is always configured as the column
oven. The following options may be configured in the other 6 available heated zones:
1177 Split/Splitless Capillary Injector.
1079 PTV Injector.
1041 On-Column Injector for wide bore (0.53 mm ID) or packed columns.
1061 Flash Vaporization Injector for wide bore or packed columns.
Single, dual, or multi-position Valve Oven.
Flame Ionization Detector (FID).
Pulsed Discharge Helium Ionization Detector (PDHID).
Thermal Conductivity Detector (TCD).
Electron Capture Detector (ECD).
Thermionic Specific Detector (TSD).
Pulsed Flame Photometric Detector (PFPD).
Methanizer.
Any combination of three Injectors may be installed on the 450-GC. If a valve oven is
installed, it normally replaces 2 physical Injector positions.
Any combination of three detectors can be installed with the following exceptions: Only
2 TCD or PFPD detectors can be installed. If 2 standard TCDs are installed, no other
detectors can be accommodated (physical space). However, a dual TCD (two cells in
one housing) is available as a Custom Solution which allows installation of another
detector, such as an FID, behind it.
The methanizer typically occupies the same location as one of the detectors.
Installed options on the 450-GC are generally identified by their location. The options
mounted on the top of the instrument, such as those listed above, are designated as
Front, Middle and Rear to coincide with their relative location or the location of their
respective electronic control modules.
Varian, Inc.
User Manual 450-GC
Page: 3
Introduction
Page: 4
User Manual 450-GC
Varian, Inc.
Installation
INSTALLATION
NOTES ABOUT SETTING UP AND USING YOUR 450-GC
The purity of the gases used with your 450-GC are essential for optimum
operation.
Varian Gas Clean Filter Kit (CP736530) is highly recommended.
All GCs require regular maintenance in order to operate at their highest
efficiency.
You want to change the Injector septum, Injector liner, FID flame tip, gas filters
and AutoSampler vials, wash bottle septa, syringes and solvents regularly.
Varian has an extensive supply of quality maintenance parts for your 450-GC
and all of your chromatography needs including a comprehensive selection of
the highest quality capillary columns available to chromatographers. Please
visit the Varian internet site (www.varianinc.com), contact your Varian sales
representative, or call your local Varian distribution center.
PREPARING FOR INSTALLATION

Refer to the Pre-Installation Instructions (CP501410) for site preparation and
unpacking information.
Inspection
The GC will arrive packed in one large palletized box and one or more smaller
cartons. Inspect the cartons carefully for damage or signs of rough handling.
Report damage to the carrier and to your local Varian office.
Unpacking
Unpack the GC and accessories carefully and transfer to the work area, using
proper handling techniques. The GC should be lifted from the bottom. Inspect
the GC and accessories and immediately report any damage to the carrier and
your local Varian office.
Avoid back strain or injury by following all safety precautions when lifting
heavy objects.
Varian, Inc.
User Manual 450-GC
Page: 5
Installation
Remove Protective Devices

The instrument has been protected during shipment by various caps, plugs and
restraints. Prior to operating, remove:
Transport clamp for oven fan motor

from hole in GC rear panel.
Detector tower plugs under

Detector cover.
Gas bulkhead fitting plugs on rear

panel.
Any plastic plugs, tape or plastic

material inside the column oven.
Connect Data Handling Peripherals

Workstations and other data handling devices are connected to the cable
connectors on the back panel or the top of the instrument.
Page: 6
The Varian Workstation of Galaxie with 450-GC control must be installed.

The hardware installation simply involves making a data-connection, on
page 89, from the computer (or hub) to the Ethernet connector on the rear
panel of the GC on page 42.
If an analog output signal (optional) is being used, follow the specific

installation instructions provided with the analog interface kit.
User Manual 450-GC
Varian, Inc.
Installation
Select Gases
The following gases are commonly used in Gas Chromatography for the
following functions. Note that the recommended purity for carrier make-up and
detector fuel gases is 99.999%. In addition, the use of gas filters to remove
hydrocarbons, oxygen and water from carrier gases is recommended.
Gas
He, N2, H2, Ar, Ar/CH4
H2, Air
He, N2, Ar/CH4
Air
LN2, LCO2
Function
Carrier gas
Detector fuel gases
Make-up gas for capillary column use
AutoSampler operation
Cryogenics
Do not exceed MAXIMUM inlet pressures listed on the rear panel of the
instrument.
Varian, Inc.
User Manual 450-GC
Page: 7
Installation
Hydrogen as Carrier Gas

The use of hydrogen as a GC carrier gas is potentially dangerous.
Hydrogen (H2) is a commonly used GC carrier gas. Hydrogen, however, is
potentially explosive and has other characteristics that make it dangerous.
Hydrogen is combustible over a wide range of concentrations. At

atmospheric pressure, hydrogen is combustible at concentrations from
4% to 74.2% by volume.
Hydrogen has the highest burning velocity of any gas.
Hydrogen has very low ignition energy.
Hydrogen temperature increases as the gas expands.
Hydrogen that is allowed to expand rapidly from high pressure can self
ignites.
Hydrogen burns with a no luminous flame which can be invisible under

bright light.
Hydrogen is potentially explosive. Take extreme care when using

hydrogen as the GC carrier gas in a GC system.
All users should be aware of the mechanisms by which hydrogen can

accumulate. They should also know what precautions to take if they know, or
suspect, that hydrogen has accumulated.
Mechanism
Results
GC off
A GC can be shut down deliberately. It can also be shut down accidentally by an

internal or external failure.
If a GC equipped with Electronic Flow Control (EFC) is shut off, the EFC does stop the
flow of carrier gas.
Power failure
If the power fails, the GC shuts down. The carrier gas is shut down (in case of EFC).
Table 1: Hydrogen as Carrier Gas during Power off
Page: 8
User Manual 450-GC
Varian, Inc.
Installation
General laboratory precautions
Avoid leaks in the carrier gas lines. Use leak-checking equipment to

periodically check for hydrogen leaks.
Eliminate from your laboratory as many ignition sources as possible (open

flames, devices that can spark, sources of static electricity, etc.).
Do not allow hydrogen from a high pressure cylinder to vent directly to

atmosphere (danger of self ignition).
Use a hydrogen generator instead of bottled hydrogen.
Operating precautions
Varian, Inc.
Turn off the hydrogen at its source any time you shut down the GC.
Turn off the hydrogen at its source if a power failure occurs.
User Manual 450-GC
Page: 9
Installation
Install Gas Regulators and Set Pressures

Carrier gas, air and H2 supplied from cylinders or manifolds should have a twostage regulator having a 0 to100 psi low-pressure stage. Set cylinder regulator
pressure to match the GC gas inlet pressures, listed below:
Gas Inlet
Pressure
Carrier gas
500 kPa, 5 Bar, 80 psi (maximum 1000 kPa/ 10 Bar / 150 psi)
Make-up
Air
H2
300 kPa, 3 Bar, 40 psi (maximum 650 kPa/ 6.5 Bar / 100 psi)
Table 2: Gas inlet pressure
Calculate a GC pressure drop (restrictions, tubing and EFC) of about 200 kPa,
2 Bar, 30 psi for well working EFCs.
Example: Column pressure needed 100 kPa + 200 kPa (pressure drop) = Inlet
pressure needed at least 100+200= 300kPa.
Maximum Inlet Pressure:

Air/N2/He/Ar: 1000 kPa / 10 Bar / 150 psi
H2: 650 kPa / 6.5 Bar / 100 psi
Connect Gases
Follow the steps below to connect gas supplies to your GC:
1. Cut required lengths of chromatographically-cleaned 1/8 copper tubing
(P/N: 03-918326-00) for the carrier and fuel gas plumbing. Clean the ends
of the tubing with a metal file.
2. Slide a 1/8 Swagelok nut, back ferrule and front ferrule over one end of the
copper tubing and attach to the outlet fitting on the cylinder regulator.
3. Push the copper tubing into the outlet fitting as far as it will go, then pull
back very slightly and tighten 3/4-turn past finger-tight with a 7/16 wrench.
Page: 10
User Manual 450-GC
Varian, Inc.
Installation
4. Slide a 1/8 Swagelok nut, back ferrule and front ferrule over the other end
of the copper tubing and connect it to the corresponding gas inlet on the
GC rear panel.
1/8" Copper Tubing
Cylinder
Regulator
5. Push the copper tubing into the bulkhead fitting as far as it will go, then pull
back very slightly and tighten 3/4-turn past finger-tight with a 7/16" wrench.
6. Make sure the gas supply control valve, which controls gas pressure to the
GC, is completely closed. Open this valve slowly and monitor the pressure
gauges on the dual stage regulator. The first pressure gauge should now
read the pressure of the cylinder.
7. Cautiously turn the regulator valve to supply gas to the GC. Watch the
pressure gauge closely and adjust the pressure according to Table 2 on
page 10.
8. Leak checks all fittings.
Installing the CP-8400/8410 AutoSampler

To install your CP-8400/8410 on a 450-GC, first unpack the AutoSampler and
verify that all of the parts required are present.
Inspect the GC and accessories and immediately report any damage to the
carrier and your local Varian office.
For a detailed installation instructions please refer to the CP-8400 AutoSampler
and CP-8410 AutoInjector section in this manual, on page 103.
It is important that the CP-8400/8410 is switched on prior to
powering up the GC.
A flashing green LED at the rear of the AutoSampler is indicating
that there is communication between GC and the Sampler.
Varian, Inc.
User Manual 450-GC
Page: 11
Installation
Connect GC to Power
Plug the GC power-cord into an appropriate source of power.
Varian supplies a number of power-cords qualified to be used
with the power load of the GC. Depending on the local
electrical network different power-cords are available.
Do not use power-cords with to low capacity. This may result in
overheating of the power-cord.
Turn on the GC power switch located at the top left of the GC.
The GC top cover (power switch) of the GC must be free of any obstacles.
This will give in case of emergency quick access to the power switch.
The 450-GC automatically enters the OPERATION screen after power up.
Press the SETUP
configuration.
key and select Configuration to verify the 450-GC
Your GC is shipped from the factory with default settings. The following is
relevant information on the factory default states and settings:
Page: 12
When the GC is turned the first time on, all installed heated zones except
for the column oven default to power OFF.
The column oven defaults to power ON and a set temperature of 50C.
When installed components that use a heated zone are turned ON in the
active method, they default set to a temperature of 50C.
User Manual 450-GC
Varian, Inc.
Installation
COLUMN INSTALLATION AND CONDITIONING

Your GC arrives ready for installation of an analytical column. On first
installation, a new column needs to be conditioned.
Conditioning is performed with the detector end of the column not

connected.
You may need to install and condition a new column after your GC has been in
use for some time. Reset all Injector, detector and column ovens to 50C to
avoid burn hazards when connecting column to Injector and detector parts
inside the oven. See also Column Conditioning on page 23.
Prior to installing your column, check that the factory-installed Injector is
equipped with the proper insert for your application. Factory-installed Injectors,
other than the 1041, have a glass insert suitable for a variety of applications. If
your application calls for a different insert, replace the factory-installed insert
prior to installing your column. Refer to the Injector section of the Manual for
instructions to replace the insert on page 97.
The factory-installed inserts for the Injectors are shown below, more Injector
insert you can find here, on page 443.
Injector
Insert Information
Part Number
1061
1079
PTV
1093
Flash Injector Liner, 0.53 mm ID Capillary columns
03-92611943
3.4 mm unpacked Injector insert
03-92611945
0.8mm ID, 0.5mm restriction SPI deactivated Injector Liner
1041
Insert for 0.53 mm ID columns
03-92543101
1177
Glass Injector, 4 mm ID, unpacked, single gooseneck
03-92611927
SG092034
Table 3: Factory-Installed Injector Inserts
Varian, Inc.
User Manual 450-GC
Page: 13
Installation
Nuts and Ferrules for Capillary Columns

Capillary columns are generally installed with a capillary
column nut (P/N 03-949551-00) and a single reversed ferrule,
as shown in the diagram. For connection to the TCD, a
special capillary adapter (P/N 03-925605-01) is used.
A Quick Connect Kit (P/N 03-925355-90) facilitates easy
connection of capillary column to Injector and detector. The
kit comes with instructions and contains: column depth scale,
knurled split nuts (2) and graphite jacketed ferrules (2 each of
0.4, 0.5 and 0.8 mm ID, for 250 m, 320 m and 530 m
columns respectively).
Reversed
Ferrule
Capillary
Column
Nut
Fused Silica
Column
Three types of ferrules are common: graphite, Vespel or polyimide and

graphite/Vespel.
Do not use graphite with ECD or GC/MS systems.
Ferrule ID is based on the diameter of the capillary column. See table

below for 1/16 ferrules.
Teflon
Column ID
0.18 mm ID and smaller
0.25 mm ID
0.32 mm ID
0.53 mm ID
Page: 14
Holes
1
1
2
1
1
2
1
Vespel
40% Graphite
/60% Vespel
Max 250C
Max 350C
Max 400C
CR214103
CR212103
CR213103
CR214104
CR212104
CR213104
CR212124
CR213124
CR214105
CR212105
CR213105
CR212125
CR213125
CR214108
CR212108
CR213108
Table 4: 1/16 Column Ferrules
User Manual 450-GC
Graphite
SilTite
Max 450C
CR211104
CR211124
CR211105
CR211125
CR211108
Metal, GC/MS
SG073300
SG073301
SG073302
Varian, Inc.
Installation
Connect Capillary Column to Injector

When a capillary column is used in combination with an Injector, alignment of
the column is critical. Use the following steps to precisely align the capillary
column. Unless this procedure is followed, the injection syringe may damage
the top of the column or peak tailing may result.
To ensure a leak-free connection of capillary columns, the ends of the column
must be cut squarely and as smoothly as possible. To achieve this, a proper
scoring tool is required. A ceramic scoring wafer (01-900158-00) is
recommended.
1. Cut off sealed section at each end of new column.
2. Uncoil 10 cm at Injector end of column.
3. Slide appropriate column nut and ferrule on each end of column. on page
14.
4. Make a clean cut with the cutting tool 1-2 (2-4 cm) from end of the column.
Inspect the cut to verify it is square and smooth.
1
2
3
4
5
Capillary column nut

Fused silica column
Capillary column ferrule
Properly cut column end
Improperly cut column ends
Figure 1: Column Ends
Varian, Inc.
User Manual 450-GC
Page: 15
Installation
5. Move the nut and ferrule to within 3 cm of column end.

6. Measure the mark point (see Table 5) from the end of the column and mark
this distance with a felt pen or typewriter fluid. The use of Column Scale
tool (03-92575001, available in Capillary Column Quick Connect Kit on
page 17, 03-925751-90) or EZ-Griptm supplied with each standard GC
capillary column is highly recommended.
DO NOT allow the column nut and ferrule to fall past the mark
because the ink or correction fluid can contaminate the ferrule.
Insert depth
Mark at
1041
1061
1177
1079 PTV
Maximum*
None
Maximum*
None
3.7 cm
2.7 cm
7.5 cm
5 cm
1093
On-Column
8.6 cm
5 cm
Table 5: Maximum insert depth for Capillary Column in Injector
7. * Only for 1041 and 1061Injectors, for the other Injectors continue at 12.
8. Gently push the column fully up into the Injector (9 cm) until the column
comes to a firm stop. This correctly positions the column against the upper
end of the Injector insert. The column must go in the full distance. If it goes
not, the Injector will not function properly. Tighten the column nut just
enough to prevent column movement.
9. Manually insert the syringe that will be used with the column into the 1041
Injector, checking that the syringe goes into the Injector completely with no
binding or interference. If interference occurs, repeat the above column
insertion procedure until the syringe moves smoothly into the Injector.
10. Continue to hold the column firmly in place as you tighten the column nut
carefully and only enough to hold the column firmly in place and obtain a
good seal. Remove the syringe from the Injector.
11. After the column is installed at the Injector end, make several dry injections
to ensure that the needle enters the column easily.
12. Partially insert the column into the lower end of the Injector. Thread up the
capillary column nut and ferrule finger-tight.
Page: 16
User Manual 450-GC
Varian, Inc.
Installation
13. Gently push the column into the Injector until the mark on the column is
aligned with the bottom edge of the column nut.
14. Tighten the column nut by hand until it is finger-tight. Hold the column and
use a 5/16" wrench to tighten the column nut in place. Tighten the column
nut only enough to seal the column and hold it firmly in place.
An optional Capillary Column Quick Connect Kit is available that
simplifies the installation of a capillary column into Injectors and
detectors. It contains split capillary column nuts, re-usable graphite
ferrules (for 250 m, 320 m, 530 m ID columns) and a column
depth scale. The ferrule is set on the column using this depth scale.
No felt pen or typewriter correction fluid is needed (The part number
of the Quick Connect Kit is 03-925751-90).
Tips for Tightening Column Ferrules

Refer to the Table 6 below for instructions to tighten the capillary column nut
with a variety of ferrule types. Do not over tighten capillary column nuts use a
new ferrule if the column does not seal. Over tightening capillary nuts can
destroy some ferrules, particularly graphite.
Ferrule Type
Recommendation
Comments
- to -turn past finger-tight may be
required to achieve a seal.
If a different size of column is used,
more tightening may be required.
May require retightening after first or
second programmed run. Over
tightening will destroy ferrule and seal.
New graphite ferrule
- turn past finger-tight
Used graphite ferrule
New graphite-Vespel
ferrule
- to -turn past finger-tight
Used graphite-Vespel
ferrule
Re-use only on same size column.
1177/1079 PTV: - to -turn past

finger-tight.
May require retightening after first or

second programmed run.
New Vespel ferrule

Not recommended for 1041/1061/1093
1177/1079 PTV: -turn past fingertight.
Reuse only on same size column
Used Vespel ferrule

Not recommended for 1041/1061/1093
Table 6: General Tightening and Re-tightening for Common Ferrules
Varian, Inc.
User Manual 450-GC
Page: 17
Installation
Nuts and Ferrules for Packed Columns
Metal packed columns are usually installed with a

metal 2-piece ferrule. (A commonly used metal
packed column is 1/8" OD stainless steel. It uses a
1/8" ID stainless steel ferrule)
A
B
C
D
E
F
Two Piece Ferrule

Column Nut
Back Ferrule
Front Ferrule
Column Nut
Metal Back Ferrule
Installed Backwards
G Graphite Ferrule
Glass packed columns are 1/4" OD and are

installed with a graphite front ferrule and a metal
back ferrule installed backwards.
Connect a Packed Column to the Injector

Follow the steps below to install a new packed column into your 1041 or 1061
Injector. Note that the Injector must first be converted for packed column use by
installing the appropriate adapters.
Page: 18
Place nuts and ferrules on both ends of column as shown.

If your column is metal, insert it into the Injector fitting and gently push until
it stops. Manipulate the column so the detector end points to the detector
OR
If your column is glass, insert it into the Injector, rotate it slightly so the
detector end is out of alignment with the detector and push gently until the
end is near but not touching the oven ceiling.
Hold the column in place and thread the nuts by hand.
Tighten the nut finger-tight and then give it a further 3/4-turn with a small
wrench.
User Manual 450-GC
Varian, Inc.
Installation
Varian Test Column

At points throughout this manual, specific values and conditions are given for
the analysis of Varian Test Samples on Varian Test Columns. Table 7 provides
information on Varian Test Columns.
Column Description
10% SE30 WHP 80/100 1mx1/8" UM 1041 PREC
For use with

Injector Models
1041/1061
Packed Adapters
Part Number
-
Capillary 15M x 0.25id VF-1ms, df=0.25um
1177 or 1079 PTV
CP8907
VF-1ms FS 15 x .25mm Df=0.25m
1177 or 1079 PTV
CP8907 (ECD)
1041/1061
CP7620
Capillary 10M x 530 id CP-Sil 5 CB fused silica

Table 7: Varian Test Columns
Identify Carrier Gas Controls and Turn on Flow

Gases are plumbed at the factory through the rear bulkhead fittings into the
inlet manifold, then to the pneumatic controls in the pneumatics compartment.
The pneumatic controls can be either electronically controlled (EFC) or
manually controlled and are different for each Injector system.
If your Injector
model is a ...
1041/1061
1177/1079
PTV/1093
Carrier gas flow is regulated by a ...

Type EFC23 or type EFC24 with valving or Flow controller
(controls flow into Injector) and a Back pressure regulator
(controls flow through column)
Type EFC21/EFC25 or Flow controller (controls flow into Injector)
and a Back pressure regulator (controls flow through column)
Table 8: Injector and EFC type combination
Carrier gas flow is adjusted at the user interface for EFC or at the
pneumatics panel for manual pneumatics. For manual pneumatics carrier
gas systems, identify the controls for carrier gas flow at the pneumatics
panel for your Injector system. These pneumatic controls are identified by
their location, i.e. front, middle, rear.
Turn on carrier gas flow by adjusting the manual flow controller or setting a
positive pressure or flow on the EFC system.
Verify that there is a positive pressure on the pneumatics panel pressure

gauge or FLOW/PRESSURE page Press
Varian, Inc.
User Manual 450-GC
Page: 19
Installation
Split Vent Flow and Septum Purge Flow

Whether you are making an injection in the split or splitless mode, a split vent
flow rate needs to be set. In this example the column flow is set to 1 mL/min,
the split vent flow is set to 100 mL/min corresponding to a split ratio of 100. A
split ratio of 100 means that for every mL of gas through the column, 100 mL/s
will flow out the vent. The split state is set in the Injector section of the 450-GC
method in case an EFC is installed or in the VALVE TABLE section of SAMPLE
DELIVERY in case an manual pneumatics is installed. In addition to a split state
a septum purge flow rate should also be set. The following information is for
setting a split vent flow rate with EFC installed. For either a 1177 or 1079 PTV
with manual pneumatics see the Injector section of the Operators Manual on
page 97 for further information.
key and set the appropriate head
1. Press the FLOW / PRESSURE
pressure for your analytical column.
2. Press the INJECTOR
Injector by location.
key and select either the 1177 or the 1079 PTV
3. When EFC is installed, in addition to programming the split state, the split
ratio can also be programmed.
4. Set the initial split state to ON and set the split ratio to 100.
key. Turn the column oven off by pushing
5. Press the COLUMN OVEN
on the button Turn Oven Power Off.
6. Allow the oven to cool down. Open the column
oven door and adjust the septum purge needle
valve located above the column oven until the
flow rate is in the range 3 - 5 mL/min. For EFC
equipped systems this value has to be entered
in the septum purge calibration routine.
Septum purge calibration
Page: 20
Select the SETUP
key and select CALIBRATION.
User Manual 450-GC
Varian, Inc.
Installation
Select the Injector you are setting up by specifying the location (front,
middle or rear) or type.
Press the Calibrate button.
Typical 3-5 mL/min
Varian, Inc.
You will be prompted to enter the Column Head Pressure and Adjusted
Septum Purge Flow Rate. Fill in the column head pressure and adjust and
measure the Septum Purge Flow rate.
Fill in the actual Septum Purge Flow and press the OK button.
User Manual 450-GC
Page: 21
Installation
Set Carrier Gas Flow Rate to Condition Column

To condition the column, flow rates need only be approximate. For packed
columns and wide bore (0.53 mm ID) capillary columns set the flow rate to
key, select the appropriate
10 - 20 mL/min. Press the FLOW / PRESSURE
Injector by location and set the initial flow to 10 - 20 mL/min (15 mL/min for a
wide bore column and 20 mL/min for a packed column).
Use the following guide to set an appropriate column flow for either the 1177 or
the 1079 PTV Injector with narrow bore capillary columns. With manual
pneumatics the pressure is set using either the 1177 or the 1079 PTV back
pressure regulator on the pneumatics panel. If the Capillary Injector has EFC
key, select the appropriate Injector by
press the FLOW / PRESSURE
location and set the pressure according the table:
Column ID
Head Pressure
250 m
170 kPa (25 psi)
320 m
100 kPa (15 psi)
530 m
35 kPa (5 psi)
Table 9: Column condition head pressure
For capillary columns, the gasflow through the column is verified by

dipping the detector end of column into a beaker containing a
solvent, such as isopropanol. Positive carrier gas flow should be
indicated by a stream of bubbles.
Injector Conditioning
It may be necessary to bake out the Injector if it has become contaminated
during the re-assembly process, i.e. if the internal parts were placed on dirty
surfaces or touched with bare hands. Then, both the Injector and column
should be conditioned. See section Maintenance, Instructions for HighTemperature bakeout of Injectors on page 433.
To prevent contamination and overheating of the fused silica
column, the column must NOT be connected to the Injector during
the Injector bake-out procedure.
Page: 22
User Manual 450-GC
Varian, Inc.
Installation
Column Conditioning
In general the column should be conditioned at 20C above the maximum
temperature used in the analytical method, or 20C below the maximum
operating temperature of the column, whichever is lower. Check with the
column supplier for the correct conditioned details.
New Columns
To minimize chemical contamination of the detector, all new columns should be
baked out before they are connected to the detector. Refer to the supplier's
recommendations for temperatures.
Used Columns
Periodically (especially during extended isothermal operation), the column
should be baked out to remove accumulated contaminants. Column
conditioning is required when column efficiency begins to fall off, i.e. loss of
resolution, peak tailing, severely drifting baseline, retention of extra peaks, etc.
For fused silica columns, it is recommended that 1 to 2 turns at the beginning of
the column (approximately 1/2 meter) be cut off prior to reconditioning, as this is
the end part of the column where the stationary phase has most likely been
disturbed. Attach the column to the Injector and, with carrier gas flowing, bake
out the column for a minimum of 3 hours.
It is important to establish the maximum recommended conditioning
temperature for the installed column. This information is provided with the
column or can be obtained from the column manufacturer. The maximum
allowable temperature for the column does not have to be used for conditioning
purposes.
A GC column may be irreversibly damaged if it is heated with air or
moisture present in the pneumatic system. It is important to purge the
column with inert carrier gas before heating the column. After the
column flow is established, allow the carrier gas to purge through the
column for 15 - 20 minutes before heating it.
Varian, Inc.
User Manual 450-GC
Page: 23
Installation
Connect Capillary Column to Detector

After the column has been conditioned, follow the steps below to connect the
capillary column to the detector.
Hot surfaces are exposed
Check that the capillary column nut and ferrule are installed on the column.
Note that if the TCD is used with capillary columns, a special capillary
adapter (PN 03-925605-01) is used on the TCD inlet.
DO NOT use graphite ferrules with the ECD.
Uncoil about 20 cm from end of column.

Move the column nut and ferrule to within 5 cm of the column end. Find the
column insertion depth for your detector in Figure below. Measure the
correct distance from the end of the column and mark this distance. Refer
to diagram below for correct distances. DO NOT let the column nut and
ferrule fall past this mark. The marking medium can contaminate the ferrule.
Column Insertion Depths for Varian Detectors
Figure 2: Column Insertion Depths for Detectors
Page: 24
User Manual 450-GC
Varian, Inc.
Installation
Place the column into the base of the detector.

Turn the capillary column nut and ferrule finger-tight.
Gently slide the column into the detector until the mark on the column
aligns with the bottom edge of the column nut.
Continue to hold the column as you tighten the nut just enough to hold the
column firmly in place and to create a good seal.
Connect Metal Packed Column to Detector

After the column has been conditioned, follow the steps below to connect your
metal packed column to the detector. Note that the appropriate packed column
adapter must be installed.
Hot surfaces are exposed
If using a detector other than TCD, locate the packed column detector
adapter in the Packed Column Kit and install on the inlet to the detector.
The TCD inlet is designed for packed column installation.
Insert the open end of the packed column into the detector inlet or adapter
and push until it reaches a stop.
Hold the column in place and finger-tighten the column nut. Then, using 2
7/16 wrenches, tighten 3/4-turn past finger-tight. On subsequent
installations, tighten the nut 1/4 to 1/2-turn past finger-tight.
Check for Leaks

Inspect your GC system for leaks before heating. An electronic leak detector is
the most reliable method to check the Injector and detector fittings for carrier
gas leaks.
Never use soaps, such as Snoop. These may contaminate the
system and cause permanent damage to capillary columns. If a
liquid leak detector is desired, try a 50/50 mixture of
isopropanol/water.
Varian, Inc.
User Manual 450-GC
Page: 25
Installation
BASIC OPERATION
At points throughout this section, specific values and conditions are given
for analysis of the Varian test samples on Varian test columns. Your
analytical column and application may require different values and
conditions. Please ascertain the range of operating temperatures for your
analytical column and make sure your settings are within this range.
Setting Carrier and Detector Gas Flow Rates

The following table indicates the typical values for carrier and detector gas flow
rates. For practical purposes a generalized carrier gas flow rate of 2 mL/min is
used for capillary columns. Note that the carrier gas and make-up combined
flow is typically 30 mL/min.
Detector
Carrier
Gas
FID
N2, H2 or
He
Carrier Gas Flow Rate

(mL/min)
Packed
Capillary
20 1
PDHID
1 - 15
Make-Up
Gas
Make-Up + Detector Detector Detector

Carrier Gas
Gas
Gas
Gas
Flow Rate
Air 1
Air 2
H2
(mL/min) (mL/min) (mL/min) (mL/min)
N2 or He
30 1
300 10
30 1
For more details see Installation Manual PDHID
TSD
N2 or He
20 1
1 - 15
Same as
Carrier
Gas
30 1
175 10
4 0.2
TCD a
N2, He or
H2
20 1
1 - 15
Same as
Carrier
Gas
30 1
ECD
N2 or
Ar/CH4
20 1
1 - 15
N2 or
Ar/CH4
30 1
PFPD
N2, He or
H2
20 1 b
1 - 10
None
__
17 1
10 1
13 1
Table 10: Flow rates for Carrier and Detector Gases
a TCD Reference Flow The flow rate for carrier gas through the reference cell is 30 1 mL/min.
b PFPD with packed columns An effluent splitter is used to reduce the carrier flow to the detector to < 5
mL/min.
Page: 26
User Manual 450-GC
Varian, Inc.
Installation
Follow the steps below to set all gas flow rates on the 450-GC.
Flows are typically set with carrier gas first followed by detector make-up and
fuel gases. The most convenient way to measure or verify gas flows is at the
detector exit.
Adapters are provided in the individual detector accessory kits for this purpose.
Note, however, that the most accurate method to determine FID and TSD flows
is at the flame tip after removing the tower.
Detector
Attach a bubble or digital flowmeter to the detector outlet using the

appropriate adapter.
Turn off make-up and detector gases at the pneumatics panel. For a needle
valve this is accomplished by turning the needle valve cartridge knob fully
clockwise. For a flow controller this is accomplished by turning the flow
controller knob fully counter-clockwise or until the turns counting dial reads
zero.
Observe reading on flowmeter. Ensure it is within the range described in
the table for carrier gas flow rates.
Adjust the carrier gas flow using the manual pneumatics controls on the
pneumatics panel or by adjusting the Electronic Flow Control to achieve the
desired flow rate.
For a capillary system, turn on the make-up needle valve and adjust to
achieve the desired flow rate. The combined carrier and make-up flow
should be 30 mL/min. Adjustment is done with a small flat screwdriver
inside the needle valve cartridge knob.
Turn on the relevant detector fuel gases in the sequence hydrogen followed
by air. Use the table below to calculate the combined flows for the specific
detector. For the TSD adjust the hydrogen flow controller until the turns dial
reads 400.
Carrier +
make-up
Carrier + make-up + Carrier + make-up +

hydrogen
hydrogen + air1
FID
30
60
360
TSD
30
34
209
PFPD
15
32
Carrier + make-up +
hydrogen +air1 + air2
42
Table 11: Detector manual Flow rates
Varian, Inc.
User Manual 450-GC
Page: 27
Installation
Condition the GC System

As the Injector and column were conditioned earlier, this procedure represents
a quick conditioning of the entire GC system including the detector. Follow the
steps below to build an analytical method to condition the GC system.
key and verify that the Injector temperature is

Press the INJECTOR
250C. If the Injector is either a 1177 or a 1079 PTV verify that the initial
split state is ON and that there is no split time program. Set the split ratio
to 100.
Press the COLUMN OVEN

temperature to 250C.
key and set the detector oven temperature to

Press the DETECTOR
300C. If the detector is an FID, wait for the detector zone to get above
100C (check here on page 287 for more Ignite conditions) and then press
the ignite button to ignite the flame.
Allow the system to condition for one hour.
key and set the initial column oven
Build a Method to Analyze a Test Sample

The conditions for running a test sample depend on the sample chosen. The
test sample is typically one of the following:
Page: 28
The column test mixture supplied by the column manufacturer,
a Varian Test Sample, or
a test mixture you select as an indicator of system performance for a

particular analysis.
User Manual 450-GC
Varian, Inc.
Installation
Method to Analyze a Varian Test Sample on a Varian Test Column

Test Sample
Part Number
Concentrations of Test Compounds
TCD
82-005048-01
3.00 g/L of C14, C15 and C16 in iso-octane.
ECD
82-005048-02
33.0 pg/L of lindane and aldrin in iso-octane.
PFPD
82-005048-03
20.0 ng/L of n-dodecanethiol, tributylphosphate, methyl

parathion; 4000 ng/L of n-pentadecane in iso-octane.
TSD
82-005048-04
2.00 ng/L of azobenzene, methyl parathion; 4.00 ng/L

malathion and 4.00 g/L C17 in iso-octane.
FID (Capillary Column)
82-005048-07
30 ng/L of C14, C15 and C16 in iso-octane.
FID (Packed Column)
82-005048-00
Note: If the FID test sample is not available, the TCD test sample can be used if first diluted 100:1.
Table 12: Varian Test Samples
Note:
These conditions may not conform to the requirements of your analytical column. Do not exceed your
columns Tmax. See Column Manufacturers specifications for your column.
For 1041 and 1061 Injectors

ECD
FID
TCD a
TSD
PFPD
Initial column oven temp (C)
80
80
80
80
80
Initial column oven hold time (min)
Program 1 ramp rate (C/min)
20
20
20
20
20
Final column oven temp (C)
200
200
200
200
200
Final column hold time (min)
190
140
140
175
175
15
15
15
15
15
Injector temp (C)
220
220
220
220
220
Detector temp (C)
300
300
220
300
300 b
12
0.05
12
10 c
On
On
On
On
On

(Isothermal operation)
(Isothermal operation)
Range
Initial Autozero
3.0 0.3
TSD bead current (amps)
Table 13: Varian Test Sample 1041 and 1061 Conditions
a TCD Reference Flow Rate for carrier gas flow through the reference cell is 20 1 mL/min.
b Depends on application: S-mode 200C, P-mode 300C and N-mode 250C.
c Normal range: 10 if Varian testmix is being used.
User Manual 450-GC
Varian, Inc.
Page: 29
Installation
For 1177 and 1079 PTV Injectors

ECD
FID
TCD a
TSD
PFPD
80
80
80
80
80
Program 1 column oven final temp (C)
200
200
200
200
200
Program 1 column oven ramp rate (C/min)
20
20
20
20
20
Program 1 column oven hold time (min)
Injector temp (C)
220
220
220
220
220
Detector temp (C)
300
300
220
300
300 b
12
0.05
12
10
On
On
On
On
On
3.0 0.3
Range
Initial Autozero
TSD bead current (amps)
Injection mode
Splitless
Initial split state
ON
Step 1 time (min)
0.01
Step 1 split state
OFF
Step 2 time (min)
1.00
Step 2 split state
ON
Step 2 split ratio
20
Table 14: Varian Test Sample 1177 and 1079 Conditions
Prepare the Test Sample

You are now ready to prepare your sample. For preparation of samples for
automated injection, please refer to the CP-8400 AutoSampler section on page
121.
You may inject your sample neat or diluted in a solvent. The Varian PFPD test
sample should be diluted 1:30 in iso-octane if you intend to use it for a splitless
injection. The choice of solvents depends on a number of factors, including
component solubility, type of detector and polarity of the analytical column.
Select solvents that match the polarity of your column.
a TCD Reference Flow Rate for carrier gas flow through the reference cell is 20 1 mL/min.
b Depends on application: S-mode 200C, P-mode 300C and N-mode 250C.
Page: 30
User Manual 450-GC
Varian, Inc.
Installation
Solvents for GC
Following are some recommended solvents for non-polar, intermediate and
polar phase columns.
Boiling Point ( C)
Column Phase
Recommended Solvent
Non-Polar
Pentane
36.1
100% Methyl
n-Hexane
69.0
5% Phenyl, 95% Methyl
Cyclohexane
80.7
Iso-octane
99.3
Benzene
80.1
Toluene
110.6
Ethyl Ether
34.6
Methyl tert-butyl ether
55.2
Methylene Chloride
39.8
Chloroform
61.2
Carbon Disulfide
46.5
Intermediate
Ethyl Acetate
77.0
50% Phenyl, 50% Methyl
Acetone
56.5
Methyl iso-butyl ketone
127.0
Acetonitrile
81.6
Polar
Methanol
64.7
Polyethyene Glycol
Ethanol
78.5
2-Propanol
82.5
n-Butanol
117.7
Table 15: Recommended Solvents for Gas Chromatography
Varian, Inc.
User Manual 450-GC
Page: 31
Installation
Sample Volume and Injection Rate

The quality of your chromatogram can be greatly affected by the sample
volume and injection rate. These vary according to the type of Injector and
column you are using.
See also in section: Technical Tips, Choosing the right GC Injection technique,
on page 466. Shown below are some recommended sample volumes and
injection rates. Draw the appropriate volume of sample into your syringe and
inject at specified rate.
Injector
Column
Sample
Volume in L
Injection Rate,
in L/sec
On-Column, Flash
Vaporizing (1041/1061)
Wide bore Capillary Columns
(0.53 mm ID)
Packed Columns
0.12 Wide bore Capillary
1-5 Packed Columns
0.5-5 Wide bore Capillary
Column
Split
(1079 PTV, 1177)
Splitless
(1079 PTV, 1177)
All Capillary
Columns
All Capillary Columns
0.2-2
0.2-1
25-50 for
CP-8400/8410 A/S
1 for
CP-8400/8410 A/S
Inject the Test Sample

Use 1L of the Varian test sample for all detectors. In addition, if you are using a
PFPD, make a 1:20 dilution of the test sample in iso-octane. With the READY
light on at the GC and the appropriate volume of test sample in your injection
syringe, you are ready to make your injection. For automated injection of
samples, please refer to the CP-8400 AutoSampler section.
To inject your sample, insert the syringe needle into the Injector inlet, press
the syringe barrel against the Injector switch and depress it completely,
simultaneously pressing down the syringe plunger. Remove the syringe from
the Injector immediately.
The blue RUN light starts to blink until the analysis ends. The run may be
stopped by pressing the STOP
Compare the resulting chromatogram with your known test chromatogram.
If you are analyzing the Varian Test Sample on a Varian Test Column, you
may compare your resulting chromatogram with the appropriate test
chromatogram in the Detector Test Chromatograms, on page 419. The
retention times will be close to those shown in the example chromatogram.
The peak heights may be considerably different.
Page: 32
key.
Failure to duplicate the results you expected may indicate an installation,

operation or instrument problem. This problem must be corrected before
proceeding.
User Manual 450-GC
Varian, Inc.
Peripheral Connectors
REFERENCE
PERIPHERAL CONNECTORS
The 450-GC Gas Chromatograph is equipped with various connectors on the rear panel and top
of the instrument intended for use with peripheral equipment such as AutoSamplers and data
handling devices. The following are the standard connectors on the 450-GC and their intended
uses:
Varian, Inc.
User Manual 450-GC
Page: 33
Top View
PERIPHERAL CONNECTORS
Peripheral connectors are located underneath the detector cover.
Lift the detector cover up at the on/off power-switch and slide
the cover to the rear of the GC. Lift the cover up and remove it.
Fuse F4, 6.3A, T see on page 44

J504/J505 S.I.D. 1 and 2
Sample Introduction Device,
used for autosampler control,
See on page 35.
J45/J46 Auxiliary 1 and 2

24 VAC output, see on page 38
J44 Cryo Valves (3)
24 VDC Cryo valve connection,
See on page 39
J42/J43 External Events
Timed Events contacts
See on page 40
J301 Analog IN
Not in use
J41 Heater Connections

Line-Voltage Heater connections
See on page 41
J401 Analog OUT

Analog signals for Integrators
(option)
See on page 36
Fuse F3, 10A, F see on page 44

J302 Temperature Probes

Thermocouples for the
Heaters
See on page 37
Figure 3: Connectors for Peripheral Equipment
Page: 34
User Manual 450-GC
Varian, Inc.
J504/J505 S.I.D. 1 AND 2

Sample Introduction Device, used for AutoSampler control.
AutoSampler CP-84XX ONLY on connector S.I.D. 2, CombiPal on connector S.I.D. 1
or S.I.D. 2.
Top View
Figure 4: Connector J504-J505

Varian, Inc.
User Manual 450-GC
Page: 35
Top View
J401 ANALOG OUT

Analog signals for Integrators
Figure 5: Connector J401
If an Integrator or other device is connected, the 450-GC is waiting (not ready on

display) for Ready-In signal (pin-1) to start.
In the Setup tab Configuration, on page 67 the Ready-In Closed Contact checkbox must
be checked! Available Analog cables on page 94.
0 1 Volt default range used for all detectors except the FID (0 10 Volt).
Page: 36
User Manual 450-GC
Varian, Inc.
Top View
J302 TEMPERATURE PROBES

Temperature probe connectors for Heaters

Varian, Inc.
User Manual 450-GC
Page: 37
J45/J46 AUXILIARY 1 AND 2

Top View
24 VAC output used for power supply AutoSampler CP-8400 or AutoInjector

CP-8410.
See Fuses on page 44

Figure 7: Connector J45/J46
Page: 38
User Manual 450-GC
Varian, Inc.
J44 CRYO VALVES (3)

24 VDC Cryo valve connections
Top View
Varian, Inc.
User Manual 450-GC
Page: 39
Top View
J42/J43 EXTERNAL EVENTS

Timed 24 Volt (DC) contacts (7) connector, for more
(optional) contacts see Option Board on page 43.
Page: 40
Figure 9: Connector J42/J43

User Manual 450-GC
Varian, Inc.
J41 HEATER CONNECTIONS
Top View
Line-Voltage Heater connections

Varian, Inc.
User Manual 450-GC
Page: 41
Rear View
REAR PANEL
Switch between DHCP and Fixed IP.

The Dynamic Host Configuration Protocol (DHCP) is a set of rules
used by a communications device such as a 450-GC to allow the device
to request and obtain an IP address from a server which has a list of
addresses available for assignment.
Fixed IP, (Internet Protocol address) is a unique fixed address that the
450-GC uses in order to identify and communicate with a computer
network.
See
Setup, tab System for more details.
Contact the network administrator for more information.
Not in use.
Not in use.
Ethernet RJ45-style connector, used to connect the 450-GC to a

computer, network or other devices.
Green led: cable correct connected
Yellow led: Transmit/Receive data.
Page: 42
User Manual 450-GC
Varian, Inc.
OPTION BOARD
The Option Board is situated below the top-cover in the Option Slot.
The Option Board have 8 Time-Events contacts (24 Volt DC) available, also 3
Analog Outputs are present and available via connector J401 Analog Out.
Top View
Figure 11: Option Board

Varian, Inc.
User Manual 450-GC
Page: 43
FUSES COMMON
Fuses have been installed within the instrument for the protection of major
power circuits.
They are designed to open as quickly as possible to prevent damage to other
components within the circuit.
Occasionally, an opened fuse may have been caused by a short one-time
surge; however, it is far more common that a component within the protected
circuit has failed.
When an open fuse is noticed, replace it.

If the replacement blows, suspect a component failure.
Before replacing fuses, turn off the oven and any heated zones and
let them cool down. Turn off any detector gases at their supply.
Then turn off the main power switch and unplug the power cord.
Fuses
The major fuses are located on the power module.
There are 4 fuses on the power module on page 34
Fuse F5 is an electronic fuse and situated on the electronic main board (not
accessible or replaceable).
ID
Description
F1
Glass/Type T
F2
System
Power Rating
Partnumber
24VDC External Events
6.3A/250V 5 x 20 mm
5550033400
Glass/Type T
24VDC External Events
6.3A/250V 5 x 20 mm
5550033400
F3
Glass/Type F
Heaters/Ovenfan (except
column oven)
10A/250V 5 x 20 mm
5550034800
F4
Glass/Type T
24 VAC Auxiliary connectors

(Sampler)
6.3A/250V 5 x 20 mm
5550033400
F5
Electronic
+5 VDC SID 1 and SID 2
0.5 A
Table 16: Used Fuses
Page: 44
User Manual 450-GC
Varian, Inc.
Display and Keyboard
DISPLAY AND KEYBOARD

The 450-GC Touch Screen and Keyboard is an integrated user interface
designed for maximum ease of learning and ease of use. This section
describes the keyboard and display layout and functions.
on page 46
on page 54
on page 51
on page 48
on page 52
The 450-GC is carried out with a so-called touch screen. Touch simplifies
the human / machine interface by enabling the operator reactions to be
natural and intuitive. Varian touch solution also helps reduce the complexity
of operations by eliminating the often cumbersome traditional operator
interfaces. They simplify the task and reduce training time for operators while
adding more capabilities to the machine itself.
Touching the display (with Stylus-Pen or Finger) will simplified the operation
of the 450-GC.
Varian, Inc.
User Manual 450-GC
Page: 45
STATUS INDICATION LEDS

The GC status indication LEDs are situated in the upper right corner of the
Keyboard/Display. The LEDs will make it possible to monitor the GC status
from some distance.
Overview Analytical Phases

Analytical Phase
Status on Main
Screen
LED
Not Ready
LED
Ready
LED
Run
Creation
Creating
ON
OFF
OFF
Initialization
Initialization
ON
OFF
OFF
Equilibration
Not Ready
ON
OFF
OFF
Stabilization
Stabilizing
BLINKING
OFF
OFF
Monitor
Monitor
BLINKING
OFF
OFF
Pre-Run
PreRun
BLINKING
OFF
OFF
Sample Preparation
Sample Prep
OFF
BLINKING
OFF
Ready
Ready
OFF
ON
OFF
Run - Hardware ready
Run
OFF
OFF
BLINKING
Run - Hardware Not Ready
Run / Not Ready
ON
OFF
BLINKING
Standby
Standby
ON
OFF
OFF
Fault
Error
ON
OFF
OFF
Table 17: Status Indication LED's
Page: 46
User Manual 450-GC
Varian, Inc.
Error LED
For detailed error description on page 84

Error State
Led
Error
Event
OFF
Alert
BLINKING
Error
ON
Table 18: Error LED
Varian, Inc.
User Manual 450-GC
Page: 47
MOST USED FUNCTIONS

Throughout the push-buttons direct access is possible to the most used GC
functions.
Main operation page, on page 54.
Status Instrument Page, on page 49.
Version information, on page 50 will show (detailed) firmware version

information
Start/Stop GC Run
Pause (Pause automation GC is running in automation mode, else ignored)
Page: 48
User Manual 450-GC
Varian, Inc.
Status page
Allows the user to view the current status of the various components of the
450-GC.
It gives an overview about the status of the GC components, split up in the
positions front, middle and rear.
All components visible are hyperlinked. Touching the display (with

Stylus-Pen or Finger) in the area where more information/control is
needed, the desired page will be shown.
The colored dots indicate the status of the component:
Varian, Inc.
The
The
The
The
green dot indicates the component is Ready.

yellow dot indicates the component is Not Ready.
empty dot indicates the component is switched off.
red dot indicates the component is in ERROR.
User Manual 450-GC
Page: 49
Version
Information
This screen will give information about the Software Versions used in the
450-GC. The About 450GC tab shows the Hostname and IP- and MAC
address.
The Detailed tab give detailed firmware information about Hardware (mainand displayboard) Injector and detector EFCs, AutoSampler (if present)
firmware.
Page: 50
User Manual 450-GC
Varian, Inc.
ADVANCED FUNCTIONS
Throughout the keyboard direct access is possible to advanced GC functions.
Sample delivery section of the Sampler

(and VLV-table), on page 55.
Injector screen, on page 57.
Pressure and Flow screen, on page 58.
Oven Screen, on page 60.
Detector screen, on page 62.
Setup/Calibration screen, on page 64.
Add line, adds a new line at the end of
the table.
Insert line, adds a new line before the
selected line.
Delete line, deletes the selected line in
the table. When a line is deleted, then
the table reformats to move the
succeeding rows up.
Delete Table, clear all entries in the
table except for the initial line.
Tab
Back space
Enter
Varian, Inc.
User Manual 450-GC
Page: 51
DISPLAY
The display is a LCD screen in combination with a touch-screen.
By touching the display (Stylus-Pen or finger) it is possible to control the GC.
The use of the Stylus-Pen is advised, it is more accurate and will
keep the display free of fingerprints. The Stylus-Pen is located at
the bottom right side of the Display/Keyboard, on page 45.
The display is split up in 4 sections:
Title Bar, on page 53.
Main Operation screen, on

page 54
Button Bar, in principle all buttons

related to the active page will be visible in
this bar.
Message Bar, messages related to

the active page or component will be
displayed.
Page: 52
User Manual 450-GC
Varian, Inc.
Title Bar
This bar is always visible with identical information, only the page name will
change.
Name of the active screen

Active Method Name
GC actual run time
GC total run time
Automation Indicator
GC under remote control,for

instance Galaxie
GC under local automation
Varian, Inc.
User Manual 450-GC
Page: 53
Main Operation screen

The main operation screen show the operation status, in which the most
important parameters are visible.
Oven information, actual
oven temperature and Oven
ramping graphic is visible
Run indicator, fill up with blue

when runtime is increasing.
Touching the indicator will reverse
the indicator. During stabilization
the indicator will be yellow and an
hour-glass will be visible.
Local Automation,
run 2 of 20 is busy
Sampler information,
indicating run sample
Status information, GC status

identical as status indication LEDs
Detector information, detector

type and actual detector signal.
Goto GC Log
Needs customer attention
on page 84
Goto Methods page,
method open, save page,
on page 61
Page: 54
User Manual 450-GC
Varian, Inc.
Sample Delivery Screen

Sample Delivery method parameters are accessible via the SampleDelivery
on the 450-GC keyboard. The Sample Delivery section can consists
key
of multiple tabs, CP-8400/8410 AutoSampler, if present and Valve Table.
The CP-8400/8410 section have multiple pages represent the most frequently
used parameters, however, predefined modes of operation limit the need to
access all parameters. See Sample Delivery Parameters on page 123 for more
information.
Varian, Inc.
User Manual 450-GC
Page: 55
The Valve Table screen gives timed control over the valves (defined in the
Setup/Sample Delivery).
All valves are connected (hardware) to connector J42/J43 External
events, on page 40 or to the option board connector J302/J30,on page 43.
The position of the valve is indicated by its energized (+) or de-energized (-)
state.
Only the enabled (on page 71) valves are visible.
Page: 56
User Manual 450-GC
Varian, Inc.
Injector Screen
screen allows you to modify the Injector parameters and
The INJECTOR
view the status of individual Injectors. If more than one Injector is installed,
pressing the corresponding tab will guide you to other Injector page.
The above example is for an 1177 Injector. Further details for programming
Injectors can be found in the Injector screen on page 97 of this manual.
Varian, Inc.
User Manual 450-GC
Page: 57
Pressure and Flow screen

EFC (Electronic Flow Control) method parameters and status are accessible via
key on the 450-GC keyboard. If more than one
the FLOW/PRESSURE
EFC module is installed, pressing the corresponding tab will guide you to
specific EFC page.
EFC modules are identified by type (EFC21 in this example) and location
(front , middle , rear ) to coincide with the sample delivery or injection
device with which they are associated. Type EFC21 is used with the 1177 or
1079 PTV. The above screen is a typical EFC program for type EFC21. In this
case, a pressure program is applied to keep the column flow rate constant while
the column temperature is ramped.
Four types of Injector EFC modules exist and each type is associated with a
specific GC Injector system.
The Setup menu identifies each EFC type and its associated Injector system by
location In Table 19, on page 59 is a description of each EFC type with used
Injector.
EFC21 setup calibration (1177 and 1079 PTV Injectors) also contains a Septum
Purge Calibration button and Splitless Vent Flow.
Page: 58
User Manual 450-GC
Varian, Inc.
Septum Purge Calibration involves measuring a flow rate at a set pressure and
entering those values into the system to correctly calculate the settings for split
and column flow. The Splitless Vent Flow provides a vent purge for runs in
which the split valve remains closed for the duration of the run. It should be set
to at least 20 mL/min.
Sample Introduction
System
EFC
Module
1177
EFC21
1079 PTV
EFC21
1041 Injector
EFC23
1041 Injector
EFC24
1061 Injector
EFC23
1061 Injector
EFC24
Gas or Liquid Sampling

Valves
EFC24
Purge and Trap with

either 1177 or 1079 PTV
EFC25
Headspace with either

1177 or 1079 PTV
EFC25
1093 Injector (SPI)
EFC23
Optional Pneumatics System

Manual pneumatics - inlet flow
controller/back pressure regulator
with pressure gauge.
Manual digital flow controller with
pressure gauge
Manual pressure regulator with
gauge.
pressure gauge
gauge.
gauge.
controller/backpressure regulator
pressure gauge
Table 19: Injector EFC Modules
Varian, Inc.
User Manual 450-GC
Page: 59
Oven Screen
allows you to establish the column oven temperature,
The OVEN screen
build a temperature program, or view the column oven status.
The status field for the OVEN indicates the programmed set temperature, the
actual measured temperature and whether the column oven is ready, not ready
or in error (colored dot).
Similar to other programming tables, the initial or isothermal line will always
appear on the first line of the table. You can then build a temperature program
by adding new lines. Below is a column oven program with an initial
temperature, initial hold time, programmed ramp and final hold. The ranges of
the Column Oven temperature are dynamically depending on injectors,
detectors, columns and cryo options.
Stabilization time is the period the column oven will equilibrate for before
allowing the column oven to go READY. It will count down (visible in the Main
Operation screen) from the set value to 0.00 min when the stabilization period
is over. The Oven Power checkbox is used to turn the column oven heater and
fan ON or OFF.
The End Stabilization button is used to bypass the remainder of the stabilization
time.
Page: 60
User Manual 450-GC
Varian, Inc.
Methods Screen
By the method screen it is possible to load, save, save as, create (new) and
delete methods.
During first (after factory) startup a Default Method will be loaded, all heated
zones will be set at 50C.
The top line of the screen identifies the method that is currently active, the
current run time and the end time of the active method and whether the GC is
under local or remote control.
The * behind the method name is an indication that the present method
parameters are different then one saved (example: initial oven temperature has
been changed manually).
Saving the method under the same or other name will let the * disappear.
The * will also disappear when the loaded method parameters are in conflict
with the setup parameters. Example: the maximum column temperature in the
setup screen is changed (other column used), if a (older) method is loaded the
system will detect the difference in maximum column temperature and let the *
appear. Saving the method again will let the * disappear. The method will be
automatically adjusted to the present setup parameters.
Touching the Method name in the Title Bar will switch to the Method
screen.
Varian, Inc.
User Manual 450-GC
Page: 61
Detector Screen
screen allows you to modify the detector method

The DETECTOR
parameters and view the status of individual detectors. If more than one
detector is installed, pressing the corresponding tab will guide you to other
detector screens. If the option Analog Output is installed a tab Analog Output
on page 63 will be visible.
The above example is for an FID detector. Further details for programming
detectors can be found in the detector screen on page 279 of this manual.
Six types of detector EFC modules exist and each type is associated with a
specific GC detector system.
In Table 20, on page 63 is a description of each EFC type with the used
detector.
Page: 62
User Manual 450-GC
Varian, Inc.
Detector Type
FID
(Flame Ionization Detector)
EFC
Module
Optional Pneumatics System
Type EFC11
TSD
(Thermionic Specific
Detector)
ECD
(Electron Capture Detector)
Type EFC12
Type EFC13
Hydrogen: Valve 0-50 mL/min

Make-up: Valve 0-55 mL/min
Air: Valve 0-550 mL/min
Hydrogen:
Flow controller 0-6 mL/min
Air: Valve 0-200 mL/min
Make-up:
TCD
(Thermal Conductivity
Detector)
Type EFC14/16
PFPD
(Pulsed Flame Photometric
Detector)
Type EFC15
TCD Make-up
EFC14: 0 60 mL/min (2x)
Reference: TCD Reference
EFC16: makeup: 0 60 mL/min
Ref: 0 55 mL/min
Hydrogen:
Air 1:
Air 2:
Table 20: Detector EFC Modules
Analog Output
For detailed description of the analog outputs click here, on page 280.
Varian, Inc.
User Manual 450-GC
Page: 63
Setup/Calibration
key allows access to the instrument configuration
The Instrument SETUP
screens for the purpose of viewing or modifying the 450-GC configuration, it
also allows calibrating parts of the GC hardware.
The 450-GC has already been configured at the factory and requires only
minor input from the user.
Access to SETUP screen is only possible if:
GC in not in run state
No error(s) are present (in case of an error, goto error log on page
84 and reset error before continue.
Press the SETUP
key and select: Setup or Calibration
Calibration
The Calibration page will appear:
The next calibration possibilities can appear:

Septum Purge Calibration of the Injectors: 1177 on page 165 and
1079 on page 188.
Display touch screen calibration on page 81.
Sampler Calibrate on page 112 and Change Syringe on page 119.
Page: 64
User Manual 450-GC
Varian, Inc.
Setup
screen is normally accessed by the

At the time of installation, the SETUP
user to check/update the local time and date information, update column
parameters, or verify the instrument configuration. If the instrument
configuration is changed, such as when adding a field upgrade kit, the
involved relevant instrument SETUP screen must be updated.
More details concerning the Setup Tabs just click on the links below:
Configuration Tab on page 66, Sample Delivery Tab on page 68,
Oven Tab on page 73,
Column Tab on page 74,
Detector Tab on page 75,
Injector Tab on page 77,
Preferences Tab on page 78, System Tab on page 79
Varian, Inc.
User Manual 450-GC
Page: 65
Configuration Tab
In the Configuration Tab it is possible to set the type of injector, Injector options
and Oven in relation with each of the heated zones (their physical location) of
the 450-GC.
The Column oven always occupies 1 heated zone (zone 7). The other available
heated zones are numbered 1 through 6 and can be occupied by 1 of the
following devices: 1177 Injector, 1079 PTV Injector, 1041 Injector, 1061
Injector, 1093 Injector, SPT, FID, TCD, ECD, TSD, PFPD, large valve oven,
small valve oven, or methanizer. SPT is allowed only in zone 3. Dual TCD is
using 1 heated zone for 2 detectors.
The location typically refers to whether the device is installed in the front,
middle, or rear position on the top of the 450-GC. In the case of detectors the
location also refers to the relative positions of the detector electrometers
installed on the main electronics board. By default, zones 1, 2 and 3 are
identified as front, middle and rear and zones 4, 5 and 6 are identified as front,
middle and rear.
Zones 1, 2 and 3 are normally used for Injectors and zones 4, 5 and 6 are used
for detectors.
Page: 66
User Manual 450-GC
Varian, Inc.
External Device
If an external device is connected that needs to be ready prior GC start, the GC
state (ready, not ready) can include the state of the external device.
When the external device state is included a selection must be made if the
ready-in (pin-1 on connector J401 Analog Out on page 36 ) of the GC is
normally closed or normally open.
Enable
check box
Ready-In
check box
Normal Closed contact (N.C.)
Normal Open contact (N.O.)
Exclude ext. device
Grayed out
External device contact
Varian, Inc.
User Manual 450-GC
Page: 67
Sample Delivery Tab

This tab has Setup parameters for an AutoSampler, if installed (Page 1) and
Valving (Page 2).
Before calibration/operation of the sampler it is advised to check the
parameters on this screen.
The following AutoSampler parameters are visible:

Miscellaneous screen
Buzzer at Start of Cycle A sound will be generated to warn of impending
tower movements when this parameter is checked. The default value is
checked.
Vial Detect Checked will cause the CP-8400/8410 to halt and generate an
error if a missing vial is encountered. Unchecked will cause the AutoSampler /
AutoInjector to ignore a missing vial and continue until it finds a vial within the
specified range. The default value is unchecked.
Find Home at Start Checked will cause the CP-8400/8410 to find its home
position before starting automation or before an autoinject action. If several
people are using the 450-GC on which the AutoSampler / AutoInjector is
mounted, then it is advisable to leave this setting checked. Use the unchecked
selection for higher throughput.
Page: 68
User Manual 450-GC
Varian, Inc.
Plunger Stroke Warning Limit (1-100,000) This parameter defines the

expected number of strokes the plunger is expected to survive without
significant degradation. Once the entered value is exceeded, a message will be
displayed in the error log screen indicating the plunger counter has
exceeded the set value.
The default number of strokes is 10,000.
Setup (CP-8400)
Sampler Injection Position (Both/Front/Rear)
The CP-8400/8410 is mounted in either the front or rear position. The sampler
position determines which of the 2 Injectors are reachable by the sampler.
Sampler mounting
Injector position
Front
Front
Middle
Rear
Middle
Rear
Table 21: Sampler/Injector position
Sampler in Front position
Sampler in Rear position
Rear Injector
Middle Injector
Middle Injector
Front Injector
In case the sampler is mounted in the front position it can inject in the front and
middle Injector. In case the sampler is mounted in the rear position it can inject
in the middle and rear Injector. In the sample delivery page of Setup, the front
sampler Injection position is the first Injector (clock wise rotation of the sampler)
the sampler is able to reach. The rear sampler Injection position is the second
Injector the sampler is able to reach.
If 1 Injector is installed, make certain to specify the correct Injector. An incorrect
setting may cause the CP-8400/8410 to inject into the top cover resulting in
Varian, Inc.
User Manual 450-GC
Page: 69
damage to the syringe and the top cover. Select both setting if you have 2
Injectors that you wish to use with the sampler. Note that selecting both allows
the sampler to use 2 Injector volumes when dual/duplicate mode is used. If you
configure a single Injector, you will see a single injection volume in the
automation tables.
Syringe Size (1 L, 2L, 5 L, 10 L, 50 L, 100 L and 250 L). (Note that
this field is not visible when the AutoSampler is in the SPME mode). Enter the
syringe volume you will install and use with your CP-8400/8410. The 450-GC
will use this value to set the correct entry selections and any needed internal
settings to correctly use the indicated syringe size.
If you are simply changing a syringe with a different volume syringe you can
press OK and Exit at this point to accept the new syringe size.
Front/Rear Injection Depth (0-100 %). The Injector Needle Depth parameters
define how far into the designated Injector the needle will penetrate. 100%
causes the needle to be completely inserted to its 2-inch length. The valid
range is settable in 1% steps. The default is 90%.
Front/Rear Speed (0-100 cm/s) The Injector Injection Speed parameters define
the rate at which the needle will penetrate the Injector septum and descend to
the set Injector Needle Depth. The valid range is settable in 1 steps. The default
is 30 cm/s.
Page: 70
User Manual 450-GC
Varian, Inc.
Valving
This screen configures the 7 standard external events available on the 450-GC
that are typically used to control the 1177 and 1079 split valve with manual
pneumatics (non-EFC) or actuators for sampling or switching valves. Each
valve is identified in SETUP by a name that indicates its application. When a
name is chosen this also defines the default states (Abbreviation, - DeEnergized and + Energized) of the valve.
The Option board has 8 optional external events available and will be
numbered from 8 till 15.
Only valves that are enabled are shown in the method pages.
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User Manual 450-GC
Page: 71
In Table 22 the complete set of valve names and associated states that are
available for programming.
Valve Type
Abbreviation
Front Split Valve

Middle Split Valve
Rear Split Valve
Gas Sampling Valve
Liquid Sampling Valve
Sample
Internal Standard
Surrogate Standard
Series Bypass
Backflush to Detector
Backflush to Vent
Column Selection
Injection + Backflush to Detector
Injection + Backflush to Vent
Alternate Injection
Simultaneous Injection
Methanizer Bypass
Sample Preconcentration Trap
External Event A
External Event B
External Event C
External Event D
External Event E
External Event F
External Event G
External Event H
External Event I
External Event J
Power Fail Option Solenoid
Quick Switch Valve
FSV
MSV
RSV
GSV
LSV
S
IS
SS
SB
BD
BV
CS
IBD
IBV
AI
SI
MB
SPT
EA
EB
EC
ED
EE
EF
EG
EH
EI
EJ
PFOS
QSV
De-Energized
State (-)
ON (split)
ON (split)
ON (split)
Fill
Fill
OFF
OFF
OFF
Series
Forward
Forward
Column 1
Fill + Backflush
Fill + Backflush
Column 1
Fill
Series
SPT Desorb
OFF
OFF
OFF
OFF
OFF
OFF
OFF
OFF
OFF
OFF
OFF
OFF
Energized State (+)

OFF (s/less)
OFF (s/less)
OFF (s/less)
Inject
Inject
ON
ON
ON
Bypass
Backflush
Backflush
Column 2
Inject
Inject
Column 2
Inject
Bypass
SPT Trap
ON
ON
ON
ON
ON
ON
ON
ON
ON
ON
ON
ON
Table 22: Valve Type Names
Page: 72
User Manual 450-GC
Varian, Inc.
Oven Tab
The default temperature limit of the column oven is set at 450C (If the column
limit is set lower then 450 C the oven limit is set accordantly, the column with
the lowest column temperature limit is used as maximum temperature limit), but
can be set to a lower value.
If the 450-GC is idle for more then the Standby Timeout time, the column oven
temperature is set to the Standby Temperature and 450-GC will go into
Standby mode, see operation screen. This standby temperature will be invoked
after the timer counts to zero, provided another run is not started before the
timer has timed out.
The default Standby Temperature is 60C.
The default Standby Timeout time is 120 minutes.
A value of 0 minutes in Standby Timeout will disable the Standby Temperature.
The Coolant checkbox turns on or off the cryogenic supply for the oven, if
installed. Coolant type can be LN2 or LCO2..
Coolant time-out refers to the period of time for which the coolant will remain on
after it is turned on. For example, if the set temperature has not been reached
or the run has not started within the specified time, the coolant supply will be
turned off.
Leave always the Injector(s) / Detector(s) heating ON (enable) and at a
temperature of at least 100 C when using cryogenic column oven cooling!
Varian, Inc.
User Manual 450-GC
Page: 73
Column Tab
Column parameters such as packed column, column length, internal diameter
and choice of carrier gas are used for the flow calculations of EFC.
The column limit temperature(s) have a direct relation with the maximum oven
temperature. If set at 350 C the oven temperature limit will be also 350 C.
The column with the lowest column temperature limit is used as maximum
temperature limit.
Carrier gas is configured by carrier gas selected for the corresponding Injector.
In case of a packed column the parameters column length and internal
diameter are not used.
Page: 74
User Manual 450-GC
Varian, Inc.
Detector Tab
The detector tab identifies each Detector system and its associated EFC type
detector system by location (front , middle , rear ). In case more information
is available this will be shown on next pages. The last page (in example
Page 2) Analog output is shown.
In Table 20, on page 63 is a description of each EFC type with the related
detector.
Detector EFC involves selecting the relevant carrier/make-up/reference gas
type.
The default temperature limit of all detectors is set at 450C, but can be set to a
lower value.
The 450-GC monitors the FID background current continuously and will attempt
to light the flame (only if the checkbox Check for Flameout is checked) if the
current drops below a specified threshold and the detector temperature is still
above 100 C (for all Ignite conditions click here on page 287. Up to three
attempts to ignite the flame will be made before the 450-GC reports a flame-out
fault.
Varian, Inc.
User Manual 450-GC
Page: 75
On the second page (Page 2 or Page 3) the Detector Analog Output screen will
be visible (only if the Analog option board is present).
The Port name can be changed by the button Edit.
The Port name will be used in the Detector screen, on page 280.
If the Range setting must be changed, make sure that the Range setting
matches the mainboard jumper settings!
Page: 76
User Manual 450-GC
Varian, Inc.
Injector Tab
The Setup menu identifies each Injector system and its associated EFC type
detector system by location (front , middle , rear ).
The default temperature limit of all Injectors is set at 450C, but can be set to a
lower value.
Injector EFC involves selecting the relevant carrier gas/outlet Pressure and
more parameters.
In Table 19, on page 59 is a description of each EFC type with used Injector.
Outlet Pressure is used to distinguish between a column venting to atmosphere
or a column venting to a vacuum source such as a mass spectrometer.
A specific Gas Saver Flow and a timeout period may be set. A time entry of 0
turns the Gas Saver feature off. If a run is not started or setup activated
before the timer expires, the set Gas Saver flow rate will be started. A message
will be logged in the instrument log.
The Splitless Vent Flow is the flow used for calculating the total flow when the
method split program contains only splitless events.
Varian, Inc.
User Manual 450-GC
Page: 77
Preferences Tab
In this tab it is possible to set General parameters.
General:
Page: 78
Set Language, default English.

Pressure Display Units, default psi also kPa and bar possible.
Temperature Display Units, default C also F possible.
Date Format, default MMDDYYYY, also DDMMYYYY, DDMMYY and
MMDDYY possible.
User Manual 450-GC
Varian, Inc.
System Tab
In System tab it is possible to set General and Network parameters.
The Network Change button is un-usable when the network-switch at the Rear
panel, on page 42 is set at DHCP a (BOOTP).
General:
Date and Time, pressing the change button, it is possible to change both values.
After changing the Date and Time a reboot is required. The OK

button of the Setup screen will change to OK reboot. Rebooting is
performed automatically after pressing the OK reboot button.
a DHCP is used to obtain an IP address from Galaxie Workstation, on page 90 or a server.

Varian, Inc.
User Manual 450-GC
Page: 79
Network:
Network, pressing the edit button it is possible to change network settings.
Its possible to set a fixed IP address in the 450-GC.
Check before changing the network settings if on the Rear panel, on page 42
the dip-switch is set to the Fixed IP position. If not set switch in Fixed IP
position and restart the GC.
Fill in the IP address and Hostname, make sure the Subnet Mask and default
Gateway are compatible with the PC settings.
Page: 80
User Manual 450-GC
Varian, Inc.
Touch Screen Calibration

Description
Calibration is necessary because it is difficult to perfectly align a touch screen's
coordinates to the LCD display behind it. If a button or other "live" feature on
the display is to be properly activated, the coordinates of the area touched on
the screen must be sufficiently close to the coordinates of the feature on the
display. Otherwise, the software may not correctly act upon the soft button
presses.
The Touch-screen is factory calibrated, however re-calibration of the touchscreen can be required (possible reasons: viewing angle, temperature or
humidity changes or after vibration or shock).
Calibration
Carried out the touch-screen calibration only with the Stylus-Pen.
Do not touch the display during the calibration procedure!

This can result in an in-correct calibration.
It is possible to navigate to the touch-screen calibration procedure (on

page 83) using only the hardware keys.
Press the SETUP
Varian, Inc.
key and select: Calibration
User Manual 450-GC
Page: 81
The Calibration page will appear:
Press in the screen Display, Touch Screen the button Calibrate.

The procedure will ask to touch (using the Stylus-Pen!) a number of calibration
points (cross in Upper left and right, lower left and right corners) visible on the
display.
Press at any time the Pause button
to cancel the calibration.
Final, as verification, touch the center of the cross in the center of the screen.
If the calibration results are accepted by the software, press the Start/stop
button
Page: 82
to exit the calibration screen.
User Manual 450-GC
Varian, Inc.
If the touch screen is not accessible for screen calibration, it is possible to access via
the hard-keys.
1. Press the question mark

Information screen.
hard-key, this will bring up the Version
2. Press the following hard-keys in the correct order (not to fast!):

3. Use the correct sequence, please note that the (push/wait) timing is important.
4. Try several times if the calibration screen will not directly popup.
5. Follow the instruction on the calibration screen.
Varian, Inc.
User Manual 450-GC
Page: 83
Error/Log Handling
An Error a will be visible by a red error led.

will be visible,
Also in the right lower corner of the display a message
indicating that the Log screen has been updated with Log (Alert or Error) related
information.
In case of an Event no
Just touch the
will be visible.
to open the log screen.
a A list of all errors with error conditions, can be found in Appendix A: Error Codes on page 479
Page: 84
User Manual 450-GC
Varian, Inc.
There are 3 log-stats present:

Will give information about all none error events (like Startup date
time).
A fault that prevents correct function of the instrument (FID flameout or
Vial missing and more). There is no dangerous situation and only a
local problem in a control/module.
Actions taken by the GC:
Fault will be reported in the error-log in yellow.
The red error led will blink.
The ready led will turn off (if on).
The not ready led will turn on.
The GC ready-out contact of the GC will switch off,
The Main-Display will display Not Ready
The module/control causing the problem will be
deactivated.
If a run was already started, it will not be interrupted.
The AutoSampler will not inject, GC is in Not Ready state.
This error is potentially dangerous for user and/or instrument. The GC
will go to a safe situation for all hardware components installed. The
problem can only be solved by intervention by the service engineer.
After solving the error only power off/on can resolve the GC.
Actions taken by the GC:
Fault will be reported in the error-log in red.
The red error led will turn on.
The ready led will turn off (if on).
The not ready led will turn on.
The ready relay of the GC will switch off.
Switching off all heaters and Oven fan motor.
The Main-Display will display Error
The module/control causing the problem will be
deactivated.
All valves (external events) are set to default state identical
to when the GC is not powered.
All Detector electronics will be turn off.
All Injector/detector EFC units controlling Hydrogen gas will
be turned off (flow setting zero).
If a run was already started, it will immediately aborted.
Instrument control will be frozen
Varian, Inc.
User Manual 450-GC
Page: 85
Page: 86
User Manual 450-GC
Varian, Inc.
Loacl Automation
LOCAL AUTOMATION
Local Automation is a tool to operate multiple analysis and single method
directly via the GC. The input is done via the Display and Keyboard and is only
to a Workstation.
accessible when the GC is not connected
To access the Automation screen, touch the

local automation button in the Operation screen
The Sampler (if present) will be recognized. It is optional to disable the

Sampler.
On order to loop the sample list the repeat infinite must be checked.
button.
To start the local automation press the start
The run will start as soon as the 450-GC state is ready.
A local automation running button
will pause the local automation run
Varian, Inc.
User Manual 450-GC
will appear. Pressing the pause button

.
Page: 87
Local Automation
Page: 88
User Manual 450-GC
Varian, Inc.
Communications
COMMUNICATIONS
Introduction
The 450-GC uses Ethernet as the method of communications for instrument
control and for sending digitized data to an external data system. In addition,
the 450-GC is equipped with (optional) analog output ports which allow analog
data to be sent to external integrators or other analog data systems.
The 450-GC is equipped to handle digital and analog data simultaneously. The
Ethernet communication option allows Workstation control of the 450-GC and
transmits up to three channels of detector data to the Workstation.
The (optional) analog connection can be configured with up to three detector
analog outputs and 8 external timed events.
Various cable options are available for sending analog data to integrators and
data.
Ethernet Communications
Ethernet refers to the type of hardware connection used to transfer digital data
between the 450-GC and the data system to which it is attached.
The 450-GC has a RJ45 connector located on the rear of the GC. The Ethernet
cable connects the 450-GC to the Workstation or switch on a company network.
Figure 12: 450-GC Back-panel Ethernet Connection
Varian, Inc.
User Manual 450-GC
Page: 89
Communications
How to set IP address in Galaxie Workstation using BOOTP (DHCP)

This procedure describes how to set the IP address in Galaxie Workstation.
1. Select the network card of the computer and write down the IP-address,
SubNet mask and Gateway.
2. Example IP address network card: 10.1.128.1 or can be determine by the
customer.
3. Subnet mask and gateway can be determine by the customer, if not change
then change the subnet mask to a value that is compatible with the
instrument used.
4. Open the Galaxie configuration manager and select in Tools the BOOTP
configuration.
5. Make sure that the network interface is compatible with the GC settings.
6. Select Discover. .
7. Check if the BOOTP (DHCP) switch at the rear of the GC on page 42 is in
the upper position, switch the GC Off/On or On.
Page: 90
User Manual 450-GC
Varian, Inc.
Communications
8. When the MAC address (from the GC) appears select the address and
press Validate.
9. Fill in IP-address and the host name or description and press APPLY.
10. Select System in the organization bar to create a new system.
11. Create a new Instrument and select the Acquisition and Sequence server
and press Next.
12. Select Groups/Project and press Next.
13. Add the devices (example 450-GC and NO sampler).
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User Manual 450-GC
Page: 91
Communications
14. Only the 450-GC driver must be installed when a sampler is installed.
15. Press OK.
16. Press Yes to access the system.
17. Select communication and press the magnifying glass to see the instrument
or type in the IP-address.
18. Press activate communication.

19. The next message should appear:
a. Parameters activated.
b. Setup received from Instrument.
20. Press OK.
21. Stop and Start the instrument.
22. Instrument is ready to use with
Galaxie.
Page: 92
User Manual 450-GC
Varian, Inc.
Communications
How to set a Fixed IP address in the 450-GC

1. Check if the BOOTP (DHCP) switch at the rear of the GC on page 42 is in
the lower Fixed IP position. If no, switch the GC Off/On to On.
2. Press the SETUP
key and select: Setup on page 65.
3. Please continue at tab System on page 79.
Varian, Inc.
User Manual 450-GC
Page: 93
Communications
ANALOG CABLES
The 450-GC has a number of analog cables options, depending on the device to which
the cable is connected. All cables have a 15-pin Dsub connector on one end to attach
to J401 (analog out) on page 36 on the 450-GC and have appropriate connectors on
the other end of the cable for the devices to which they are being attached.
Partnumber
Description
Picture
392567501
Analog cable W/Sync Spade lugs.

This cable is equipped with three sets
of shielded analog signal pairs,
terminated with spade lugs and 2 sets
of sync signals, a Sync-In to the 450
and a start-pot from the 450.
392567201
Analog out cable to old ADC board.
392567301
Sample intro device cable

(Archon/Tekmar).
390793805
Analog cable to MIB 800 Box.
CBLV3800
Analog cable to PAL.
Page: 94
User Manual 450-GC
Varian, Inc.
Communications
QU040.0115
CP742629
Analog cable to QUMA.
Analog cable to QUMA/CP8400.

Table 23: Analog Cables
Varian, Inc.
User Manual 450-GC
Page: 95
Communications
Page: 96
User Manual 450-GC
Varian, Inc.
Sample Introduction
SAMPLE INTRODUCTION
Sample introduction devices refer to the hardware used to introduce the sample
into the Gas Chromatograph. These include AutoSamplers, liquid Injectors, gas
sampling valves and liquid sampling valves. This screen also covers the
pneumatic systems associated with the various sample introduction systems.
The various pneumatic systems are described with the individual sample
introduction systems.
AUTOSAMPLERS
Two Varian samplers are available for the 450-GC, the CP-8400 AutoSampler
and the CP-8410 AutoInjector, on page 103. Also a Combi PAL sampler
(Liquid, Headspace, SPME Injection System) is available for the 450-GC, more
details can be found at www.varianinc.com.
LIQUID INJECTORS
There are 5 liquid Injectors available on the 450-GC Gas Chromatograph:
1. The 1177 Split/Splitless Capillary Injector on page 153 is optimized
especially for split and splitless injections. The Injector is designed to accept a
variety of inserts allowing tailored configurations for either the Split or Splitless
injection method.
2. The 1079 PTV Injector on page 175 can be used in a variety of sampling
modes including isothermal split and splitless, temperature ramped splitless,
on-column and large volume injection. The 1079 PTV can be temperature
programmed and cooled by cryogenics.
3. The 1041 On-Column Injector on page 205 is designed for use with wide bore
capillary columns or packed columns. The standard Injector is supplied with an
adapter for wide bore capillary columns. Optional adapter kits are available for
1/8" and 1/4" packed columns.
4. The 1061 Flash Vaporization Injector on page 219 is also designed for use
with wide bore capillary or packed columns. This Injector uses a glass insert
inside the Injector body. The standard Injector is supplied with an insert for use
with wide bore capillary columns. Optional adapters are available for 1/8" and
1/4" packed columns.
5. The 1093 Septum-Equipped Programmable Injector (SPI), on page 231
gives optimum performance for non-vaporizing (cold) injection into conventional
Varian, Inc.
User Manual 450-GC
Page: 97
Sample Introduction
fused silica capillary columns. It incorporates several unique design features to

produce improved peak resolution, quantitation and versatility over other cold
on-column Injectors. The result is not only a capillary on-column injection
system ideally suited for analyses that cannot be done with conventional
split/splitless injection, but one that gives highly accurate and precise results
with a wide variety of trace to semi-trace level samples.
6. The SPT Injector, on page 251 is a concentrating system for the determination
of trace level volatile organic components in air and other gaseous matrices.
Integrated into the top of the GC, its design provides the following features:
Fast heating rates.
Page: 98
Very low cryogenic consumption using liquid carbon dioxide (LCO2) or

liquid nitrogen (LN2) cryogenic cooling.
Short and long trap length options.
Fully integrated in the GC method.
User Manual 450-GC
Varian, Inc.
Sample Introduction
SAMPLING VALVES
The 450-GC can be configured with a wide variety of gas and liquid sampling
valves. These sampling valves can be unheated or installed in a (valve) oven.
Typically a sampling valve is installed in series with a liquid Injector and thus
shares the pneumatic system of the Injector, but valves can also be installed
with their own pneumatic systems. Optional actuators are available to automate
the function on the sampling valves. In addition to sampling valves, Varian also
supplies a large number of switching valve configurations.
Load
Fill
SAMPLE OUT
SAMPLE OUT
SAMPLE IN
SAMPLE IN
LIQUID
SAMPLING
VALVE
CARRIER GAS
LIQUID
SAMPLING
VALVE
CARRIER GAS
INJECTOR
INJECTOR
SPLIT VENT
SPLIT VENT
COLUMN
COLUMN
DETECTOR
DETECTOR
Load
Fill
SAMPLE LOOP
SAMPLE OUT
SAMPLE OUT
SAMPLE IN
SAMPLE IN
SAMPLE LOOP
GAS
SAMPLING
VALVE
CARRIER GAS
GAS
SAMPLING
VALVE
CARRIER GAS
INJECTOR
SPLIT VENT
Varian, Inc.
INJECTOR
SPLIT VENT
COLUMN
COLUMN
DETECTOR
DETECTOR
User Manual 450-GC
Page: 99
Sample Introduction
The following are the typical locations for valves on the 450-GC:
Heated
Zones for
Valves
Unheated Valves located on the top panel of the instrument, beneath the
Injector cover. The area behind the Injectors can accommodate multiple (3possible) unheated valves.
Dual valve ovens which replace 1 or 2 Injectors positions on the 450-GC.

The single valve oven can accommodate 1 valve and an optional 1041 or
1061 Injector. The dual valve oven accommodates 1 or 2 valves.
A multi-position valve oven which can accommodate up to 6 standard

valves with 4 - 10 ports, or one 12 port or larger valve (including a Stream
Selector Valve) and 4 standard valves. This valve oven is mounted over the
rear Injector position and utilizes 1 heated zone.
Up to three valves can be installed on the right side of the column oven.
This is the least preferred location due to temperature cycling of the column
oven and will effect the valve live negatively.
If valves are located in a valve oven then they are configured in 450-GC as
front , middle , rear , valve ovens. The valve oven temperature is
. Note that when multiple valves are
programmed in the Oven tab
installed in one valve oven the temperature of the oven should always be set
lower than the lowest temperature rated valve. In general valves have upper
temperature ratings of 220 C or 350 C.
Page: 100
User Manual 450-GC
Varian, Inc.
Sample Introduction
External Sample Introduction Systems

In addition to liquid Injectors and sampling valves, several external sampling
systems can be used with the 450-GC. The most common are besides the
CP-8400/8410 AutoSampler a Purge and Trap System and the Heated
Headspace System. These sampling systems are supplied with individual
operators manuals.
Pneumatic Systems
Most sample introduction systems may be equipped with manual pneumatics or
Electronic Flow Control (EFC). The following table summarizes the available
pneumatics systems for liquid Injectors, sampling valves, purge and trap and
heated headspace systems.
Sample Introduction
System
EFC
Module
1177 Liquid Injector
EFC21
1079 PTV Liquid Injector
EFC21
EFC23
EFC24
EFC23
EFC24
Gas or Liquid Sampling

Valves
EFC24
Purge and Trap with

either 1177 or 1079 PTV
EFC25
Headspace with either

1177 or 1079 PTV
EFC25
1093 Liquid Injector (SPI)
EFC23
Optional Manual
Pneumatics System
pressure gauge.
gauge.
pressure gauge.
gauge.
gauge.
controller/backpressure regulator
pressure gauge.
Figure 13: Pneumatic Systems for Liquid Injectors and Sampling Valves
Varian, Inc.
User Manual 450-GC
Page: 101
Sample Introduction
Page: 102
User Manual 450-GC
Varian, Inc.
AutoSamplers
CP-8400/8410 AUTOSAMPLER
INTRODUCTION
We strongly recommend that you read this section before you start using your
CP-8400 AutoSampler or CP-8410 AutoInjector.
The CP-8400 is a 100 vial capacity AutoSampler.
The CP-8410 is an AutoInjector based on the CP-8400; it has a manually
positioned tray and can accommodate up to 10, 6 and 5 each of 2 mL, 5 mL
and 10 mL vials respectively.
Both the AutoSampler and AutoInjector can inject into 2 Injectors; the Sampler
can inject into either one of the 2 Injectors or into both (either from the same
sample vial or from adjacent vials) during the same analysis.
Varian, Inc.
User Manual 450-GC
Page: 103
AutoSamplers
Both the CP-8400 and CP-8410 are preprogrammed with several injection
modes (Standard On-Column, Standard Split/Splitless, Viscous, Volatile and
Neat) that are optimized for most common types of samples. The User Defined
mode allows access to all parameters and should be used with discretion since
injection accuracy and precision may be adversely affected by incorrect choice
of certain parameters. The SPME mode requires different hardware (optional).
If the SPME mode is selected the other injection modes will not be available.
This section will cover AutoSampler installation, software setup and calibration
to the correct sampling and injection positions, a description of the operating
parameters and some examples of how you may wish to use the CP-8400/8410
to accomplish your analyses. If, after reading this section you still have
questions or encounter a problem that is not covered, please contact your local
Varian Technical Support for further assistance.
Page: 104
User Manual 450-GC
Varian, Inc.
AutoSamplers
INSTALLING THE CP-8400/8410

If the Sampler has been installed by a service engineer, you can skip this
chapter and goto page: 122.
Before installing the Sampler, turn off the oven and any heated
zones and let them cool down. Turn off any detector gases at their
supply. Turn off the main power switch and unplug the power cord.
Use the correct (included) screws (metric) to mount the sampler.

1. Before installing the CP-8400 or CP-8410 AutoSampler, make certain your
450-GC is equipped with the appropriate Top-Cover. This cover will have a
long rectangular opening for the installation of the Injector locator plate,
markings indicating the front and rear installation positions for the
AutoSampler and a small rectangular opening to route the CP-8400/8410
power/communication cable through.
Figure 14: Top-Cover for Sampler
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User Manual 450-GC
Page: 105
AutoSamplers
There are 2 positions on the 450-GC in which the CP-8400/8410 can be

installed: front and rear.
-
The front position allows the CP-8400/8410 to use the front and middle
Injectors.
The rear position allows the CP-8400/8410 to use the middle and rear
Injectors.
2. Remove any old equipment or old autosamplers from the top of the GC.
3. Place the CP-8400/8410 near the GC, manually rotate the Injector tower so
that it does not obstruct the Sample-carrousel/tray.
4. Remove the Sample-carrousel/tray.
5. Remove the old 450-GC Top-Cover by lifting up and removing the Detector
cover. Remove the Detector cover by lifting the rear of the cover and sliding
it towards the rear of the GC and up. Remove the 4 screws holding the
Injector cover down on the top of the GC. Retain the screws and set the old
Top-Cover aside.
6. Install the sampler Top-Cover so that the guide-pins on the cover fit into the
corresponding slots on the chassis. Screw the Sampler Top-Cover in place.
Remove before installing the Sampler, the screw positioned at the

front-right of the Top-Cover. See Figure 14.
7. Route the CP-8400/8410 power/communication cable across the top of the
GC to the left side of the GC. Plug the power cable into Aux 1 (J46) or Aux
2 (J45), on page 38 and the 25-pin D-shell into the S.I.D. 2 (J4), on page 35
connector.
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User Manual 450-GC
Varian, Inc.
AutoSamplers
8. Route the CP-8400/8410 power/communication cable through the Sample

top-cover gap.
9. Install the Injector locator plate by gently pushing the

circular holes over the Injector(s). Do not use
excessive force. If the Injector(s) do not fit
conveniently, loosen the screws holding the
Injector(s) to the 450-GC chassis and adjust the
Injector(s) positions so that they conveniently fit into
the locator plate. The top cover has small access
holes to allow you to loosen the retaining screws on
the Injectors. You may need to unscrew the Injector
nut and remove the inject switch to have unimpeded
access to the Injector retaining screws; replace the
Injector nut (if removed) so that you have proper
alignment when the locator plate is installed. Once
the Injector(s) are properly aligned, screw down the
alignment plate and then screw down the Injector
retaining screws. Remove the locator plate, replace
the inject switch on each of the Injector(s) and
reinstall the locator plate.
Injector locator plate
10. The CP-8400/8410 is aligned to the Top-Cover of the

450-GC by a 2 pins protruding from the bottom of the
AutoSampler/AutoInjector base. These 2 pins will fit into holes on the TopCover.
Varian, Inc.
User Manual 450-GC
Page: 107
AutoSamplers
11. Place the CP-8400/8410 onto the Top-cover, aligning it with either the front
or rear mounting position (See Figure 14) as appropriate.
12. The base is secured to the Top-Cover via 2 (short) screws at the rear and
3 (long) screws underneath the AutoSampler/AutoInjector samplecarrousel/tray.
13. Plug the connector of the power/communication cable into the

CP-8400/8410.
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User Manual 450-GC
Varian, Inc.
AutoSamplers
14. Remove protective shipping materials from the Injector carriage and install
the syringe into the AutoSampler Injector tower by opening the clear plastic
door, carefully inserting the syringe into its holder and the needle through
its guide, then fasten the plunger screw on the top and snap the retaining
clip over the syringe.
15. Close the clear plastic
sampler door.
Plunger Retaining Nut
(unscrew to remove
syringe and tighten
when installing)
Syringe Retaining Clip

(lift up to remove
syringe)
16. Replace the left side top cover.

17. Place Waste and Solvent vial (see here for large Solvent / Wash on page
111 vial).
18. Place a capped vial into the Vial 0 location if you have a CP-8400 or the
Vial 1 location if you have a CP-8410.
19. Place the CP-8400 sample-carrousel onto the base or place the CP-8410
sample tray oriented so that Vial 1 is under the arc traced by the tower.
If you re-locate the CP-8400/8410 to the rear position, you MUST

recalibrate the Injector positions. You will not be automatically
prompted to recalibrate the Injector positions. If you fail to
re-calibrate the Injector positions, the AutoSampler may miss the
Injector, resulting in bent syringe needles.
Varian, Inc.
User Manual 450-GC
Page: 109
AutoSamplers
SAMPLER FIRST START UP

This chapter describes the GC and Sampler first time combined startup and
helps you to get the system ready for use.
1. Before GC power-up its very important to read the Warnings and Notes
below!
It is important that the CP-8400/8410 is switched on prior to power-up the
GC. A flashing green LED at the rear of the AutoSampler is indicating that
there is communication between 450-GC and the Sampler.
Do not turn off the Sampler power switch during normal operations.
Syringe moves automatically during operation of instrument. Keep your

hands and fingers out of the injection area. Failure to do so may result in
accidental needle prick/scratch.
The Injector nut and locator plate may be very hot during
instrument operation and should not be touched with
unprotected hand.
Using SPME mode sample introduction, it is mandatory to perform the
calibration process with the liquid sampling syringe provided standard
with your AutoSampler.
2. Set the Sampler switch ON.
3. Switch the GC ON.
4. The GC will start initialization the system, during this process the sampler
will start moving the CP-8400 carrousel, syringe and tower to check if all
sensors and positions are correct. If a sample-error occurs the initialization
will stop, the error will be visible in the error log. GC Power Off/On restarts
the initialization process.
5. The GC/Sampler combination must be calibrated now, proceed with the
next calibration chapter.
Page: 110
User Manual 450-GC
Varian, Inc.
AutoSamplers
LARGE SOLVENT / WASH VIAL

Large volume Liquid Injections of 50 L and more are become increasingly
important for trace analysis. Large volume injections require an extra capacity
to wash the syringe. The 5 mL wash vial does not contain sufficient solvent to
run a 100-vial tray in an automated way. With the large wash vial the capacity is
increasing by a factor of 60.
The Large Wash Vial is a 120 mL stainless steel vial and has 2 openings. Both
use a snap cap. The vial replaces the 5 mL solvent vial.
The Large solvent vial can easily be refilled. Optional a second large solvent
vial can be installed.
The vial is suitable for non-aggressive solvents. The stainless steel design
makes it unbreakable and re-usable.
The large solvent vial is available as a field installation kit only (CP741158).
Additional large solvent vials can be ordered separately (CP741161).
Varian, Inc.
User Manual 450-GC
Page: 111
AutoSamplers
CALIBRATION
Sampler calibration will align the Sampler components (Tower, Vials and
Needle) and the GC Injector ports.
Calibration procedure is important for a trouble free working GC/Sampler
combination.
Calibration must be carried out in the following cases:
First Installation of the Sampler.
Sampler has been removed from the GC and after maintenance/repair back
on the GC.
Bending Sample needles.
Other Injector positions used (back or front).
If the Injector has been removed calibration is mandatory.
Do not recalibrate the Injector positions after normal Injector maintenance such
as changing septa or inserts.
Two calibration methods are present:
- Vial calibration, on page 113.
- GC Injector calibration, on page 116.
If during Calibration a question mark appears in a yellow triangle,

this will indicate that the calibration is not correct!
Page: 112
User Manual 450-GC
Varian, Inc.
AutoSamplers
Vial calibration
The Vial Calibration procedure will allow the AutoSampler/AutoInjector to learn
the tower and carrousel/tray positions so that the syringe is positioned directly
over the middle of the first vial in the sample-carrousel (Vial 0) or the middle of
the first 2 mL vial of the AutoInjector sample tray (Vial 1).
The CP-8400 may use a number of different sample vial form factors; however,
you should use all of the same vials for each session.
Mixing different vials is strongly discouraged. If you calibrate using one vial type
and then begin using another vial type with a different height, it is strongly
recommended that you recalibrate the Vial 0 Position to avoid bent needles and
other minor problems.
In order to accurately calibrate Vial positions use the calibration
tool (P/N: CP740889). The calibration tool simulates a standard
vial. The tool is used for both the CP-8400 and CP-8410
AutoSamplers.
The calibration tool can be placed (depending of the
carrousel/tray-material) in 2 different ways in the tray.
CP-8410 (polymer tray)
calibration tool in Vial position 1
CP-8400 (metal carrousel)

calibration tool in Vial position 0
Two O-rings visible

One O-ring visible
To assure consistent operation, always approach the final Tower

and Carrousel calibration position with CW (clockwise) movements.
To help facilitate this rule, the carrousel will backup 10 steps when a
CCW (counterclockwise) action is selected but will move 1 step per
move action when a CW (clockwise) carrousel rotation is selected.
Varian, Inc.
User Manual 450-GC
Page: 113
AutoSamplers
1. Place the Calibration tool in Vial 0 or Vial 1

key and select CALIBRATION, select on the next
2. Press the SETUP
page Sampler CALIBRATE.
3. The calibration screen will be visible.
Calibrating the CP-8400 Vial 0 position involves manipulating the positions of 3

different components (Tower, Syringe and Carrousel).
Calibrating the CP-8410 Vial 1 position involves manipulating the positions of 2
different components (Tower and Syringe).
4. Press Start Calibration. The CP-8400/8410 will rotate the tower, rotate the
sample-carrousel (not for the CP-8410) and lower the syringe sled to the
approximate location of Vial 0 (or Vial 1 if CP-8410). After the
Page: 114
User Manual 450-GC
Varian, Inc.
AutoSamplers
CP-8400/8410 has found the approximate Vial 0 (or Vial 1) position, visually
check that the syringe sled is not resting on the Vial top.
If the syringe sled is resting on the vial top, press the Syringe Up button
until the syringe sled is clear of the Vial top by approximately 1 mm.
5. Start the calibration process by adjusting the tower position. Move the
Tower CCW or CW until the needle-guide is exactly cover the top of the
calibration tool.
6. For CP-8400, set the sample-carrousel position. You may have to switch
back and forth between the tower and sample-carrousel one or more times
to determine the optimum rotational positions.
7. Adjust the syringe sled height so that the needle is just barely above the
calibration tool top. You should be able to see about a papers thickness of
space between the syringe sled needle guide and the top of the calibration
tool. The penetration depth into the vial is measured from the bottom of the
needle guide, so this height will give you optimum penetration depth.
8. Press the Accept button if the calibration of Vial 0 or 1 is complete, the
calibration data will be saved.
9. Press Exit button to exit the calibration screen, without saving the
calibration data.
If the used Vial is shorter/longer then the calibration tool its
advisable to repeat only the Syringe calibration.
Varian, Inc.
User Manual 450-GC
Page: 115
AutoSamplers
GC Injector calibration
1. Press the SETUP
page Sampler CALIBRATE.
2. The calibration screen will be visible.

3. Before starting the calibration identify Injector 1 and Injector 2.
Injector 1 is the first Injector the Tower will encounter when it rotates
clockwise to reach the Injector(s). The second Injector is Injector 2. Please
notice the difference when the sampler is mounted in the Front or Rear
(next page) position.
Sampler mounted in
the Front position
Injector 2
Injector 1
Page: 116
User Manual 450-GC
Varian, Inc.
AutoSamplers
Sampler mounted in
the Rear position
Injector 2
Injector 1
Syringe moves automatically during operation of instrument. Keep

your hands and fingers out of the injection area. Failure to do so
may result in accidental needle prick/scratch.
4. On the calibration screen Injector 1 press Start Calibration button. The
Injector Tower rotates so that it is over Injector 1 position and lowers the
syringe sledge so that it is over the Injector.
Varian, Inc.
User Manual 450-GC
Page: 117
AutoSamplers
5. If the needle guide descends so that it is either resting on the inject switch
or below the needle cone on the inject switch, use the Up button move the
sled up (10 steps) until the needle guide is just above the Injector cone.
6. Using the CCW (counterclockwise) and CW (clockwise) button. Position
the tower directly over the Injector Inject Switch Locator cone.
7. Adjust the height (using the Up and Down button) of the needle guide
such that the sled is just resting on or very slightly depressing the Injector
Switch and is covering the locator cone.
8. Press the Accept button if the calibration of Injector 1 is complete, the
calibration data will be saved.
9. Calibrate Injector 2 (if present) using the above mentioned procedure.
10. Press the Exit button if calibration is finished or leaving the calibration
page without saving is needed.
The Reset Calibration button will restore the factory settings to all
calibration values.
Page: 118
User Manual 450-GC
Varian, Inc.
AutoSamplers
SYRINGE CHECK/REPLACE
For changing the syringe size continue on the next page.
If the syringe has to be replaced by the same size follow the procedure below:
1. Press the SETUP
page Sampler Change Syringe.
2. The next massage will pop-up and the Sampler Tower will go to his Syringe
Replace/Check Syringe position.
3. Check or Replace the Syringe when the above pop-up message appears.
4. After syringe replacement the syringe plunger stroke counter can be set to
zero, press OK.
5. After Syringe check (no reset of the counter necessary), press Cancel.
Varian, Inc.
User Manual 450-GC
Page: 119
AutoSamplers
SYRINGE SIZE CHANGE

For changing the syringe size the next procedure MUST be followed:
1. Change syringe size in Setup tab SampleDelivery.
2. Press OK to leave Setup.
3. Follow the Syringe Check/Replace procedure (previous page).
Follow the correct working order!
Page: 120
User Manual 450-GC
Varian, Inc.
AutoSamplers
OPERATION
PARAMETERS AND QUICK REFERENCE
The layout of the screens and the placement of the parameters followed the philosophy
of keeping those parameters that an operator may wish to change for a series of
samples (such as the injection volume, vial range, GC method) within the Automation
pages for quick access and change.
Those parameters that drive the AutoSampler actions such as clean, viscosity settings
and needle residence times are located within the AutoSampler Method.
The CP-8400/8410 AutoSampler is preprogrammed with settings and actions that are
appropriate for most common analyses. The following diagrams represent the hierarchy
of screens that follow from selecting the indicated key on the 450-GC front panel.
Varian, Inc.
User Manual 450-GC
Page: 121
AutoSamplers
SAMPLER CONFIGURATION
The AutoSampler will be delivered in one of two (Liquid or SPME)
configurations.
Default is the Liquid Sampling configuration.
The SPME operation can be thought of as fundamentally reversed from liquid
sampling in terms of the actions the plunger performs during the sampling
process. In liquid sampling, the plunger is at its home state more or less fully
descended and sampling is done by withdrawing the plunger from the syringe
barrel in order to take an aliquot for injection. In SPME however, the plunger is
at the top of its travel when it is in the home position and the SPME fiber must
be exposed by inserting the plunger into the fiber holder barrel to expose the
fiber.
The SPME Sampling mode can not be selected by the 450-GC
display/keyboard. In order to configure the system to use SPME you
must set a switch on the syringe sled to the correct position and install
the special SPME fiber holder block. This means of setting up the
system to use SPME was adopted to avoid unintentional damage to
either SPME hardware or syringes. Ones the installation is completed,
the 450-GC will recognize the sampler mode.
Page: 122
Installation of the SPME mode, on page 142.
Installation of the Liquid Sampling mode, on page 149.
User Manual 450-GC
Varian, Inc.
AutoSamplers
SAMPLE DELIVERY PARAMETERS

has parameters that represent the
The 450-GC Sample Delivery page
most frequently used parameters, however predefined modes of operation limit
the need to access all parameters.
The CP-8400 (liquid) is preprogrammed with 6 injection modes designed to

optimize your analysis for:
1.
2.
3.
4.
5.
6.
Standard On-Column on page 124 (Standard OC)

Standard Split/Splitless on page 124 (Standard Split/Splitless)
Neat samples on page 126 (Neat)
Viscous samples on page 128 (Viscous)
Volatile samples on page 129 (Volatile)
User Defined on page 131 (User Defined)
Choosing 1 of these 5 injection modes will preset critical parameters for

optimum performance and limit the parameters you need to set. If you prefer to
develop your own injection method for your CP-8400/8410, the 6th
CP-8400/8410 operation mode user defined (User Defined), allows access to
the full suite of CP-8400/8410 parameters. You should exercise care when
using the user defined mode since choices for some parameters may have
unintended consequences.
Varian, Inc.
User Manual 450-GC
Page: 123
AutoSamplers
Standard On-Column and Standard Split/Splitless Sampling Modes

Internal Standard is not permitted with Standard Sampling modes.
Standard mode parameters are set for samples dissolved in common solvents
such as iso-octane.
The Standard sampling mode for On-Column performs the following
sequence of actions:
All CleanStrokes- and Flush-Volumes are limited to 75% of the syringe

capacity.
Sampler
sequence
SyringeSize
(L)
Standard On-column - mode
10
50
- Volume (L)
0.75
1.5
3.75
7.5
- Plunger Speed Up (L/s)
0.5
2.5
187.5
20
50
50
62.5
10
25
50
25
0.75
1.5
3.75
7.5
37.5
75
187.5
0.5
2.5
10
20
50
10
25
50
25
50
62.5
Clean Strokes
(sample sample)
0.2
0.4
10
20
50
- Plunger Speed Down (L/s)
10
25
50
25
50
62.5
- Volume For Fill Strokes (L)
0.75
1.5
3.75
7.5
37.5
75
187.5
- Number Of Clean Strokes

- Viscosity Delay (s)
Page: 124
75
10
37.5
If used: Any Pre-Injection Sample Clean

Flushes
(sample waste)
- Volume (L)
250
If used: Pre-Injection Solvent Clean Flushes

(solvent waste)
100
0.0
0.0
0.0
0.0
0.0
0.0
0.0
Draw Sample
- Plunger Speed During Fill (L/s)
0.2
0.4
10
20
50
0.0
0.0
0.0
0.0
0.0
0.0
0.0
User Manual 450-GC
Varian, Inc.
AutoSamplers
Sampler
sequence
5
6
SyringeSize
(L)
Standard On-column - mode
10
50
100
250
Air Plug After sample

- Volume (L)
0.1
0.2
0.5
0.5
0.5
Inject Sample
- Plunger Speed During Injection (L/s)
0.5
2.5
10
12.5
- Pre Injection Delay (s)
0.0
0.0
0.0
0.0
0.0
0.0
0.0
- Post Injection Delay (s)
6.0
6.0
6.0
6.0
6.0
6.0
6.0
If used: Any Post Injection Solvent Clean

Flushes
(solvent waste)
- Volume (L)
0.75
1.5
3.75
7.5
37.5
75
187.5
0.5
2.5
10
20
50
10
25
50
25
50
62.5
Table 24: Injection mode parameters for On-Column
Internal Standard is not permitted with Standard Sampling modes.

Standard mode parameters are set for samples dissolved in common solvents
such as iso-octane.
The Standard sampling mode for Split/Splitless performs the following
sequence of actions:

capacity.
Sampler
sequence
Standard Split-/Splitless - mode
10
50
Varian, Inc.
100
250
- Volume (L)
0.75
1.5
3.75
7.5
9.9
9.9
9.9
9.9
37.5
75
187.5
9.9
9.9
0.5
2.5
9.9
10
20
50
50
62.5

(solvent waste)
SyringeSize
(L)
10
25
50
25

Flushes
(sample waste)
- Volume (L)
0.75
1.5
3.75
7.5
37.5
75
187.5
9.9
9.9
9.9
9.9
9.9
9.9
9.9
0.5
2.5
10
20
50
User Manual 450-GC
Page: 125
AutoSamplers
Sampler
sequence
Standard Split-/Splitless - mode
10
50
100
250
10
25
50
25
50
62.5
0.4
10
20
50
10
25
50
25
50
62.5
0.75
1.5
3.75
7.5
37.5
75
187.5
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.2
0.4
10
20
50
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.1
0.2
0.5
0.5
0.5
10
25
50
25
50
62.5
Draw Sample

- Volume (L)
Inject Sample
0.2

Clean Strokes
(sample sample)
SyringeSize
(L)
0.0
0.0
0.0
0.0
0.0
0.0
0.0
6.0
6.0
6.0
6.0
6.0
6.0
6.0

Flushes
(solvent waste)
- Volume (L)
0.75
1.5
3.75
7.5
37.5
75
187.5
0.5
2.5
10
20
50
10
25
50
25
50
62.5
Table 25: Injection mode parameters for Split-/Splitless
Neat Sampling Mode

Internal Standard is not permitted with Neat Sampling mode.
Neat mode parameters are set for samples that are normally liquids that will be
injected without dilution.
The Neat sampling mode performs the following sequence of actions:

capacity.
Page: 126
User Manual 450-GC
Varian, Inc.
AutoSamplers
Sampler
sequence
SyringeSize
(L)
Neat - mode
10
50
100
250
0.75
1.5
3.75
7.5
37.5
75
187.5
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.5
2.5
10
20
50
10
25
50
25
50
62.5
0.75
1.5
3.75
7.5
37.5
75
187.5
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.5
2.5
10
20
50
10
25
50
25
50
62.5
Coating Strokes
(same movent as Pre-Injection Sample
Clean Flushes)
- Volume (L)
0.75
1.5
3.75
7.5
37.5
75
187.5
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.5
2.5
10
20
50
10
25
50
25
50
62.5

(solvent waste)
- Volume (L)

Flushes
(sample waste)
- Volume (L)
- Number of Coating Strokes

3
Clean Strokes
(sample sample)
0.2
0.4
10
20
50
0.0
0.0
0.0
0.0
0.0
0.0
0.0
10
25
50
25
50
62.5
10
50
100
250
Draw Sample
0.2
0.4
10
20
50
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.1
0.2
0.5
0.5
0.5
10
25
50
25
50
62.5
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0

- Volume (L)
Inject Sample
Varian, Inc.
User Manual 450-GC
Page: 127
AutoSamplers
Sampler
sequence
SyringeSize
(L)
Neat - mode
10
50
100
250
- Volume (L)
0.75
1.5
3.75
7.5
0.5
2.5
37.5
75
187.5
10
20
50
10
25
50
25
50
62.5

Flushes
(solvent waste)
Table 26: Injection mode parameters for Neat
Viscous Sampling Mode

Viscous mode is designed for samples that either are viscous or are dissolved
in a viscous solvent such as cyclohexanol.
Viscous mode actions are summarized below:

capacity.
Sampler
sequence
SyringeSize
(L)
Viscous - mode
10
50
100
250
- Volume (L)
0.75
1.5
3.75
7.5
37.5
75
187.5
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.5
2.5
10
20
50
10
25
50
25
50
62.5

Flushes
(sample waste)
- Volume (L)
0.75
1.5
3.75
7.5
37.5
75
187.5
9.9
9.9
9.9
9.9
9.9
9.9
9.9
0.1
0.2
0.5
10
25
10
25
50
25
50
62.5

(solvent waste)
Page: 128
User Manual 450-GC
Varian, Inc.
AutoSamplers
Sampler
sequence
SyringeSize
(L)
Viscous - mode
1
3
0.5
2.5
10
20
50
10
25
50
25
50
62.5
0.1
0.2
0.5
0.5
0.5
2.0
4.0
0.1
0.2
0.5
10
25
9.9
9.9
9.9
9.9
9.9
9.9
9.9
0.1
0.2
0.5
0.5
0.5

- Air Gap (L) (if used)
100
250
Draw Sample

- Volume (L)
50
If used: Internal Standard

10
Inject Sample
0.5
2.5
10
20
50
0.0
0.0
0.0
0.0
0.0
0.0
0.0
12.0
12.0
12.0
12.0
12.0
12.0
12.0
- Volume (L)
0.75
1.5
3.75
7.5
37.5
75
187.5
0.5
2.5
10
20
50
10
25
50
25
50
62.5

Flushes
(solvent waste)
Table 27: Injection mode parameters for Viscous
Volatile Sampling Mode

This mode is designed for samples dissolved in highly volatile solvents such as
pentane.
Volatile mode actions are summarized below:

capacity.
Varian, Inc.
User Manual 450-GC
Page: 129
AutoSamplers
Sampler
sequence
SyringeSize
(L)
Volatile - mode
1
1
1.5
3.75
7.5
37.5
75
187.5
0.0
0.0
0.0
0.0
0.0
0.5
2.5
10
20
50
50
62.5
10
25
50
25

Flushes
(sample waste)
- Volume (L)
0.75
1.5
3.75
7.5
37.5
75
187.5
9.9
9.9
9.9
9.9
9.9
9.9
9.9
0.1
0.2
0.5
10
25
10
25
50
25
50
62.5
0.5
2.5
10
20
50
10
25
50
25
50
62.5
0.1
0.2
0.5
0.5
0.5
2.0
4.0
0.1
0.2
0.5
10
25
9.9
9.9
9.9
9.9
9.9
9.9
9.9
0.1
0.2
0.5
0.5
0.5
if used: Internal Standard
Draw Sample

- Volume (L)
250
0.0
- Air Gap (L) (if used)
100
0.0
50
0.75
10

3
- Volume (L)

(solvent waste)
Inject Sample
0.5
2.5
10
20
50
0.0
0.0
0.0
0.0
0.0
0.0
0.0
12.0
12.0
12.0
12.0
12.0
12.0
12.0
- Volume (L)
0.75
1.5
3.75
7.5
37.5
75
187.5
0.5
2.5
10
20
50
10
25
50
25
50
62.5

Flushes
(solvent waste)
Table 28: Injection mode parameters for Volatile
Page: 130
User Manual 450-GC
Varian, Inc.
AutoSamplers
User Defined Sampling Mode

Allows access to all AutoSampler parameters.
This mode of operation should be used with caution since some parameters, if not optimally set,
can produce poor area precision and anomalous results. User Defined mode has three pages of
parameters.
Page 1
Prep.Ahead
This parameter is used to select whether the AutoSampler will sample for the
next injection immediately after the current chromatographic run is completed or
to cause the AutoSampler to sample while the current run is in progress thus
improving throughput. Prep-Ahead works for either liquid or SPME sampling
modes. If you set the Prep-Ahead, the system will use the Prep-Ahead Delay
time entered into the method to determine when to begin sampling for the next
run. The Prep-Ahead timer will begin after the AutoSampler has completed all
Varian, Inc.
User Manual 450-GC
Page: 131
AutoSamplers
of its actions for the current run. For instance, if you have dual or duplicate
injections selected and the second injection is set to take place 0.5 minutes into
the run, the Prep-Ahead timer for the next sample will start once the second
injection is finished. So if you have set the Prep-Ahead timer to 10 minutes, the
system will actually start sampling at around 10.5 minutes into the run. If your
sample is either heat or light sensitive you may wish to leave the Prep-Ahead
blank. Note that the Prep-Ahead timer is independent of the run time; this
allows you to set a next sampling time while the instrument is either
equilibrating or stabilizing if the sample may be heat or light sensitive. You will
have to experiment with sample and solvent flushes along with any other preinjection settings for your AutoSampler to determine the correct Prep-Ahead
time for optimum cycle time and minimum wait before injection.
Sample Penetration Depth (0-100%)

This parameter defines how far the needle penetrates through the septum into
the sample vial. The percentage refers to the distance from the bottom of the
vial septum to the bottom of the vial interior. The valid range is settable in 1%
steps. The default is 90%.
Solvent Penetration Depth (0-100%)
This parameter defines how far into the solvent vials the needle will penetrate.
The percentage refers to the distance from the bottom of the vial septum to the
bottom of the clean vial interior. There is only one penetration depth for all three
clean/Internal Standard vials. This parameter is settable in 1% steps. The
default is 90%.
Air Plug After Sample

This parameter defines the volume of air drawn up after the sample has been
drawn into the syringe.
Page: 132
User Manual 450-GC
Varian, Inc.
AutoSamplers
Sample Air Gap

Setting this parameter will cause the syringe plunger to be withdrawn an
amount corresponding to 1 L (depending of the syringe size) prior to the
syringe sled descending and the sample being drawn up. Leaving this this
parameter blank will cause no upper air gap to be formed. The default value is
blank.
Number of Fill Strokes (0-99)
This parameter defines how many times the syringe plunger will be pumped
(withdrawn and then advanced). This parameter is required to effectively flush
the syringe with the sample to remove bubbles and prevent dilution of the
sample by residual solvent from wash processes. The syringe will use the
Plunger speed parameters as defined in the viscosity settings page. The default
value is 0.
Fill Volume for Fill Strokes
This parameter defines the volume that will be used by the fill strokes specified
above. This volume will usually be equal to or larger than the sample volume
specified in the Samplelist.
Viscosity Delay (sec)

Defines the amount of time the system will wait after the syringe plunger is
withdrawn, drawing sample into the syringe. This time is required to allow
samples with high viscosity to migrate into the syringe. The syringe remains in
its loading position with the needle at its programmed depth in the sample vial
for the duration of the Viscosity delay. The default value is 0.0.
Pre-Injection Delay (0-99.9 sec)
Specifies the length of time the needle will remain in the Injector prior to the
advancing of the syringes plunger to expel its contents into the Injector. The
default value is 0.0 sec.
Varian, Inc.
User Manual 450-GC
Page: 133
AutoSamplers
Post-Injection Delay (0-99.9 sec)

Specifies the length of time the needle will remain in the Injector after the
syringes contents have been completely expelled. The default value is 0.0 sec.
Fill Plunger Speed
Defines the speed at which the plunger will be withdrawn to draw up sample.
This parameter is required to prevent cavitation of some solvents during
extraction.
Injection Plunger Speed
Depending on the volume of the syringe installed, this parameter will be limited
to the specified ranges. The Injection rate setting has 0.1 L/sec (depending of
the syringe size) step resolution.
Page: 134
User Manual 450-GC
Varian, Inc.
AutoSamplers
Page 2
Clean Mode
Number of Pre-Injection Solvent Clean Flushes (0-99)
This parameter defines the number of times the syringe will draw up solvent,
rotate to the waste cup and expel the syringe contents before the sampling
process begins. The default value is 3.
Varian, Inc.
User Manual 450-GC
Page: 135
AutoSamplers
Number of Post-Injection Solvent Clean Flushes (0-99)

This parameter defines the number of times the syringe will draw up solvent,
rotate to the waste cup and expel the syringe contents after the injection
process has ended. The default value is 1.
Number of Pre-Injection Sample Clean Flushes (0-99)
This parameter defines the number of times the syringe will draw up sample,
rotate to the waste cup and expel the syringe contents before the sampling
process begins. The default value is 0.
Clean Solvent Source Vial (I, II, III, I&II, I&III, II&III, I&II&III)
There are three clean vials. This parameter selects which clean solvent source
or combination of clean solvent sources the AutoSampler will use for its clean
flushes. If a combination Clean Solvent Source is specified, the system will
perform the number of solvent clean flushes as set by the operator from each of
the solvent sources. Consequently, if the operator selected the Clean Solvent
Source of I&II&III and the number of pre-injection solvent clean flushes was set
to three, the system would draw up and expel solvent from Clean Solvent
Source I three times, Clean Solvent Source II three times and finally Clean
Solvent Source III three times for a total of nine syringe actions prior to
beginning the sampling process. The default value for the Clean Solvent
Source is I.
Internal Standard
Internal Standard
This parameter determines whether the system will use an Internal Standard as
part of the sampling procedure. Selecting will cause the CP-8400/8410 to draw
up the specified amount of Internal Standard from the specified vial.
The Internal Standard will always be withdrawn before the sample is withdrawn
to avoid as much as possible cross contamination of the Internal Standard with
analyses. The default value is blank.
Page: 136
User Manual 450-GC
Varian, Inc.
AutoSamplers
Internal Std Size

This parameter defines the volume of Internal Standard that will be extracted for
injection. The AutoSampler/AutoInjector will draw up the Internal Standard
(depending of the syringe size) before the sample.
Internal Std Drawup Speed
This parameter defines how fast the plunger will be drawn out of the syringe
extracting Internal Standard from the vial and into the syringe. The default value
is 5.0 L/sec.
Internal Std Vial (I, II, III)

This parameter will identify which of the three clean vials contains the Internal
Standard. The AutoSampler/AutoInjector will draw up the Internal Standard
before the sample. This order is to minimize contamination of the internal
standard by residual sample. The default internal standard vial is Clean Vial
position II.
Internal Std Pause Time (0-9.9 sec)
This parameter defines how long the syringe will remain in the vial after the
plunger has reached its set withdrawal volume. This is required to allow the
internal standard to fully migrate into the syringe. The default value is 0 sec.
Internal Std Air Gap
Selecting for this parameter will cause the AutoSampler to withdraw the plunger
a distance equal to 1 L (depending of the syringe size) after the syringe has
been withdrawn from the vial. Selecting blank will cause the syringe plunger to
remain in its position subsequent to the extraction of the Internal Standard until
some other sampling action is required. No air gap will be withdrawn. The
default value is checked.
Varian, Inc.
User Manual 450-GC
Page: 137
AutoSamplers
Page 3
Solvent Plug
This parameter determines whether the system will us a solvent plug as part of
the sampling procedure. Selecting will cause the CP-8400/8410 to draw up the
specified amount of solvent from the specified vial. The default value is blank.
Vial for Solvent Plug (I, II, III)
This parameter defines which of the vials will be used as the source for the
solvent plug. The default selection is wash vial I.
Page: 138
User Manual 450-GC
Varian, Inc.
AutoSamplers
Solvent Plug Size

This parameter defines the volume of solvent that will be used for the solvent
plug in 0.1 L steps (depending of the syringe size) for the 5 and 10 L
syringes. The default volume is 0 L.
Solvent Drawup Speed
This parameter defines how quickly the plunger will be withdrawn form the
syringe during the solvent plug extraction procedure. The default value is 5
L/sec for each of the syringe types.
Solvent Pause Time (0-9.9 sec)
This parameter defines how long the syringe needle will remain in the vial after
the plunger has been withdrawn a distance corresponding to its set volume in
the Solvent plug size parameter. The default value is 0 sec.
Solvent Air Gap
Setting this parameter will cause the syringe plunger to be withdrawn an
amount corresponding to 1 L (depending of the syringe size) prior to the
syringe sled descending and the solvent being drawn up. Setting this parameter
to blank will cause no upper air gap to be formed. The default value is blank.
Abort Clean
Use in case Automation is stopped or a serious fault is detected.
Clean Vial (I, II, III)
This parameter specifies the wash solvent vial that will be used by the Default
Cleaning procedure. The default value is 1.
Clean Volume
This parameter defines the amount of cleaning solvent that will be drawn up
and expelled to waste. The volume is selectable in 0.1 L (depending of the
syringe size). The default value is 5.0 L.
Number of Clean Strokes (0-10)
This defines the number of times the cleaning solvent will be drawn up and
expelled into the waste cup. The default value is 1.
Clean Drawup Speed
Varian, Inc.
User Manual 450-GC
Page: 139
AutoSamplers
This parameter specifies how quickly the plunger will be withdrawn from the
syringe drawing solvent into the barrel. The default value is 5 L/sec
(depending of the syringe size). This same value should be used as the plunger
speed when expelling the syringe contents into the waste cup.
SPME Sampling Mode

SPME mode is designed for using the special Solid Phase MicroExtraction fibers and fiber holder.
Do not use the clean mode actions unless you have experience with
SPME or have very dirty samples with insoluble materials that need
to be removed. Indiscriminate use of cleaning can introduce
contaminants into your analytical run and degrade your results.
SPME mode actions are summarized below:
1. The number of pre-injection solvent clean flushes specified in the method
will be performed by dipping the fiber into the solvent and waiting for each
clean stroke the time specified in the Adsorb Time for Cleaning. Once the
cleaning strokes are completed the tower will rotate over the waste station,
the fiber holder will descend and the fiber exposed for drying/desorbing
(desorbing requires a heated gas stream to be gently blown over the fiber).
2. If Prep-Ahead is used, the AutoSampler will begin the sampling process at
the set delay time after the Prep-Ahead timer has expired. This allows you
to sample for extended lengths of time without adversely affecting the
throughput of your system. The Prep-Ahead timer starts after the Auto
Sampler has finished all injections actions for the current injection.
3. If Derivatization is specified, the fiber will next be introduced into the
Derivatizing Agent vial specified in the Derivatization page. The fiber will
penetrate into the Derivatizing agent vial the depth set for the Solvent
penetration depth on the main SPME parameters page. The fiber will wait
for the specified Adsorb time and then be withdrawn.
4. The SPME fiber holder will be positioned over the sample vial and the
number of agitation strokes requested will be performed. Agitation is
accomplished by moving the fiber into and out of the fiber holder at
between 1 and 2 times per second. It is common for this action to pause a
little longer sometimes relative to others. This non-regular motion is
expected and normal. Each time the fiber descends into the sample, it will
stay in the sample for the specified Adsorb Time. Use the Sample
Penetration Depth to sample from either headspace (the vapor above the
sample) or into the liquid. The fiber holder sheath (the needle at the end of
the fiber holder) will penetrate about 6 mm into the sample vial. The fiber
will be extended varying distances based on the penetration depth setting.
Page: 140
User Manual 450-GC
Varian, Inc.
AutoSamplers
For liquid sampling you will get best results if the level of the liquid in the
vial does not contact the fiber sheath thus potentially causing carry-over.
5. The AutoSampler will next perform the SPME sample introduction into the
Injector. The SPME fiber holder will descend and penetrate the Injector
septum. The fiber will then be extended the specified Desorb time on the
main SPME parameters page.
6. Upon withdrawal from the Injector, any post injection clean actions will be
performed.
The SPME mode screens and parameters are summarized below:
Varian, Inc.
User Manual 450-GC
Page: 141
AutoSamplers
INSTALLATION OF THE SPME MODE

This section describes the installation of the SPME option on the
CP-8400 AutoSampler and the CP-8410 AutoInjector.
Never use soaps, such as Snoop. These may contaminate the
system and cause permanent damage to capillary columns. If a
liquid leak detector is desired, try a 50/50 mixture of
isopropanol/water.
Familiarize yourself with the safety regulations and the general operating
principles, including the calibration of the sampler positions.
To enable the sampler to perform SPME, 2 basic adjustments of the sampler
are required:
The syringe-holder bracket must be exchanged.

The switch on the sampler tower, mounted on the sled, must be set in the
SPME mode.
SPME syringe holder
Syringe switch
Figure 15: SPME Syringe and Holder

Page: 142
User Manual 450-GC
Figure 16: SPME/Standard Switch

Varian, Inc.
AutoSamplers
Installation of the SPME mode:

1. Turn off the main power switch and unplug the power plug.
2. Manually rotate the Sampler Tower so that it is over the GC. It is best not to
place it over an Injector since the Injector may be hot.
3. Open de tower's clear plastic door and remove the syringe.
4. Remove the syringe bracket (3 screws).
5. Push the Injectors plunger-head holder downwards.
Injector plunger
Head holder
Syringe bracket
Syringe bracket screws
6. Push the syringe sled down as far as it will go.

Once the syringe-guide foot touches the top of the gas chromatograph,
gently compress it further. Observe the white switch, which will be just
exposed once the sled has reached its maximum downward travel.
Set to SPME
(UP-position)
Push sledge down

until switch appears
Varian, Inc.
User Manual 450-GC
Page: 143
AutoSamplers
7. Set the switch to the SPME configuration (UP-Position).

8. Raise the sled until you hear a click, this fixes the sled.
9. Install the SPME syringe holder.
10. Install the SPME syringe, i.e. the fiber holder, in the block. Lock the plunger
head and fix the syringe. Position the SPME syringe in such a way that you
can see the opening in the barrel.
Mount the SPME syringe in

such a way that the opening of
the barrel is visible
Installation of the fiber into the SPME syringe, i.e. the fiber holder, is explained
in the fiber-holder manual.
11. Close the cover on the tower and turn on the power to the GC. The GC will
automatically detect the new configuration of the switch and will respond
accordingly.
12. Recalibrate the sampler, on page 112.
13. Adjust the Injector insert, on page 145 to SPME injection.
14. The instrument is now in the SPME mode.
Page: 144
User Manual 450-GC
Varian, Inc.
AutoSamplers
Injector Insert
To assure optimum results when desorbing a SPME fiber, it is important to use
the correct Injector insert. Use a straight, unpacked insert with an internal
diameter of 0.8 mm (P/N: 392611948 for the 1079 Injector). Smaller inserts do
not allow the fiber sheath to penetrate the Injector, while large inserts will
broaden early-eluting analytes.
The SPME fiber is mounted in the fiber sheath. During septum
penetration, the fiber is completely retracted into the sheath for
protection. A blunt sheath with a relatively large diameter may result in
septum leakage. If you encounter frequent septum failure, use the
optional Merlin Microseal TM.
Plunger
Barrel
Fiber Sheath
Color-coded
Screw Hub
Sealing Septum
Retaining Nut
Fiber Sheath
Fiber
Attachment Rod
(pierces septum
of sample vial
and GC injector)
SPME Fiber
Fiber
Attachment Rod
SPME Fiber
Figure 17: SPME Syringe
When performing liquid SPME, make sure that the fiber sheath does NOT
contact the liquid. This may result in carry-over.
Varian, Inc.
User Manual 450-GC
Page: 145
AutoSamplers
Injector Temperature
To accelerate the desorption process of the analytes from the SPME fiber,
elevated injection temperatures are required. The ideal temperature is
approximately 10-20C below the maximum temperature of the fiber and GC
column (usually between 200 and 280C).
Sample Vials and Septa

SPME is a concentration technique normally used in combination with a
GC/MS. To minimize pollution of the analysis by the vial septum, special Ultra
clean septa are used. These vials are included in the SPME kit. Replacement
parts see here, on page 441.
Agitation Strokes
SPME can be used in the agitation mode, which is useful when performing
liquid SPME. Agitation disrupts the depletion zone that may surround the fiber
during the extraction process. With CP-8400 and CP-8410 SPME, agitation is
achieved by moving the fiber in and out of the sample liquid, approximately
once every 2 seconds.
To use the agitation mode, fill in the number of Agitation Strokes (1 or more).
Zero will disable the Agitation mode.
Page: 146
User Manual 450-GC
Varian, Inc.
AutoSamplers
Sample Penetration Depth (%)

The penetration depth indicates the position of the fiber in the vial in the DOWN
position. The UP position is a fixed value, which is 1 cm higher than the DOWN
position. The DOWN position is set at the point at which the fiber is just fully
immersed in the sample liquid.
Typical value for the 2 mL vial (P/N: 392611549 and P/N: 392611979)
Sample volume 1 mL
Penetration depth 60%
SPME Adsorption Time

The SPME adsorption time is the period between agitation strokes. If the
number of agitation strokes is 0, the SPME adsorption time is equal to the
sampling time.
Varian, Inc.
User Manual 450-GC
Page: 147
AutoSamplers
Number of Agitation Strokes

The number of agitation strokes is the number of up and down movements of
the fiber between the sample liquid and the space above the sample in the vial.
As a guideline, use the following formula to calculate the sampling time:
Sampling time (min) = (tAdsorb + tagitation) * (nstrokes + 1)
Whereby:
tAdsorb is the adsorption time (min)
tagitation is the time per agitation stroke (approx. 0.01 min)
nstrokes is the number of agitation strokes
For example: an adsorption time of 5 minutes, in combination with 10 agitation
strokes will result in the following sampling time:
Sampling time = (5+0.01)*(10+1) is approx. 55 min
Optimum analytical yield results are obtained with an adsorption time
that is set to 0. The sampling time is determined by the number of
agitation strokes only.
Page: 148
User Manual 450-GC
Varian, Inc.
AutoSamplers
INSTALLATION OF THE LIQUID SAMPLING MODE

This section describes the installation of the Liquid Sampling option on the CP8400 AutoSampler and the CP-8410 AutoInjector.
Familiarize yourself with the safety regulations and the general operating
principles, including the calibration of the sampler positions.
To enable the sampler to perform Liquid Sampling, 2 basic adjustments of the

sampler are required:
The syringe-holder bracket must be exchanged.

The switch on the sampler tower, mounted on the sled, must be set in the
STD (Liquid Sampling) mode.
Liquid Sampling
syringe holder
Figure 18: Liquid Sampling Syringe and Holder
Varian, Inc.
User Manual 450-GC
Syringe switch
Figure 19: SPME/Standard Switch
Page: 149
AutoSamplers
Installation of the liquid sampling mode:

1. Turn off the main power switch and unplug the power plug.
2. Manually rotate the Sampler Tower so that it is over the GC. It is best not to
place it over an Injector since the Injector may be hot.
3. Open de tower's clear plastic door and remove the syringe.
4. Remove the syringe bracket (3 screws).
5. Push the Injectors plunger-head holder downwards.
Syringe bracket
Syringe bracket screws
Once the syringe-guide foot touches the top of the gas chromatograph,
gently compress it further. Observe the white switch, which will be just
exposed once the sled has reached its maximum downward travel.
Push sledge down
until switch appears
Page: 150
Set to Liquid Sample

(DOWN-position)
User Manual 450-GC
Varian, Inc.
AutoSamplers
6. Set the switch to the STD (Standard, liquid sample configuration) DOWNPosition.
7. Raise the sled until you hear a click, this fixes the sled.
8. Install the Liquid Sample syringe holder.
9. Install the Liquid Syringe, in the block. Lock the plunger head and fix the
syringe.
Fix the plunger head
Mount the liquid

syringe
Fix the syringe
10. Close the cover on the tower and turn on the power to the gas
chromatograph. The gas chromatograph will automatically detect the new
configuration of the switch and will respond accordingly.
11. Recalibrate the sampler, on page 112.
12. Adjust the Injector insert to Liquid Injection.
13. The instrument is now in the Liquid Injection mode.
Varian, Inc.
User Manual 450-GC
Page: 151
AutoSamplers
Page: 152
User Manual 450-GC
Varian, Inc.
1177 Split/Splitless Capillary Injector - Injectors
THE 1177 SPLIT/SPLITLESS CAPILLARY INJECTOR
The 1177 is a dedicated Split/Splitless Isothermal Capillary Injector which

operates in 2 modes:
Split.
Splitless.
The 1177 Injector can be used with a wide range of narrow bore to wide bore
(100 to 530 m ID) capillary columns.
The basic pneumatics design is a wide range inlet flow controller and back
pressure regulated column head pressure. This is the case whether manual
pneumatics or Electronic Flow Control (EFC) is used.
Varian, Inc.
User Manual 450-GC
Page: 153
Injectors 1177 Split/Splitless Capillary Injector
Features of the 1177 Injector
The 1177 operates isothermally from 50 to 450 C.
Changing from one injection mode to another typically involves a change of

Injector insert and a modification to the Injector and EFC program. Glass
inserts can be easily changed from the top of the Injector.
The internal Injector temperature profile keeps the septum cool while
maintaining the point of injection at the setpoint temperature.
The 1177 uses positive septum purge to minimize the adsorption of sample
onto the Injector septum and to prevent contaminants from the septum
entering the column.
The 1177 uses a unique dual split vent that allows effective sweeping of the
entire Injector body.
Automatic Start Switch

The automatic start switch is a spring loaded actuator that fits over and is
aligned with, the injection port of the 1177 Injector nut. The GC run is started
when the actuator is depressed by the syringe barrel, or manually pressed at
the moment of sample injection. The GC run can also be manually (only in local
automation) started by pressing the START
The Injector nut and automatic start switch assembly may

be very hot during instrument operation and should not be
touched with unprotected hands.
1177 Injector Inserts

Click here to see the 1177 Injector Inserts, on page 448.
Note that all 1177 Injector inserts are deactivated for maximum inertness.
Page: 154
User Manual 450-GC
Varian, Inc.
1177 Modes of Injection

The 1177 injection mode is defined by the Split Vent program and by the choice
of insert. The Split Vent is controlled differently based on the pneumatics
installed, if EFC the split valve is controlled from the Injector section, or in case
of manual pneumatics the split valve (is controlled from the valve table). The
following are brief descriptions of the various modes of injection. More detailed
information on each mode is given later in this section.
Split Mode
The split injection mode is preferred for the analysis of relatively concentrated
samples. The sample is split in the Injector with a representative portion
entering the column. The split injection mode provides the shortest sampling
time which leads to sharp chromatographic peaks. Use the 4.0 mm open insert,
or the packed 4.0 mm ID insert when operating in the split mode.
In the split injection mode, the sample volume is typically 2 L or less. Early
eluting compounds usually appear as very sharp peaks. In some cases, the
peak width is less than one second. It is important that you inject the sample as
quickly as possible. If you are using the CP-8400 AutoSampler use the
Standard Split/Splitless mode of injection. If you are using a non-Varian
AutoSampler or you are using the User Defined Mode of operation on the
CP-8400 AutoSamplers, if the sample injection time (the time between the
insertion and removal of the syringe needle from the Injector) exceeds the peak
width, peaks can broaden, tail or chromatographic performance will be
degraded. With broader, later eluting peaks, it is less important that you inject
the sample quickly. The split ratio (fraction of sample that enters the column) is
the ratio of Splitvent flow to the column flow.
Splitless Mode
The 4 mm Goose-neck insert packed with glass wool is typically used for
isothermal splitless injection. The small capillary section of the glass insert fits
around the syringe needle and restricts backflush of the sample vapor during
injection. In the splitless injection mode, the sample enters the column during a
variable sampling time at the beginning of the analysis. This period is typically
30-90 seconds during which there is no flow from the Injector to the split vent.
After the sampling time, the Injector is vented to remove any residual solvent
and sample out of the Injector.
Varian, Inc.
User Manual 450-GC
Page: 155
1177 Injector Screen

The 1177 Injector screen allows modifying the Injector parameters.
With the Enable checkbox it is possible to enable/disable the Injector
temperature control.
In the Temperature box the wanted Injector temperature can be set.
The Split State controls the flow of carrier gas through the Injector during the
analytical run. When the Split State is unchecked, most of the sample injected
is directed onto the column. When the Split State is checked, the sample is split
in the Injector with typically the smaller fraction entering the column and the
larger fraction being vented.
In the example below is a splitless injection. The Injector is held in the split state
for the initial period with split ratio of 20. When the run is started the split state
will switched Off. After 0.9 minute the split is switched on again.
Page: 156
User Manual 450-GC
Varian, Inc.
1177 Electronic Flow Control (EFC)

The EFC module used with an 1177 Injector is the EFC21 or EFC25.
The EFC21 and EFC25 type are designed specifically for the 1177 and 1079
PTV Injectors to support their various modes of operation. It duplicates the
behavior of the Split/Splitless manual pneumatics system in that there is an inlet
mass flow controller supplying carrier gas to the Injector and a pressure control
valve downstream from the Injector which sets the Injector pressure. As Injector
pressure determines the rate of carrier gas flow through the column, this
pressure is monitored close to the point of injection.
Type EFC21 allows the user to set constant Injector pressure or constant flow.
In addition the split ratio can be programmed.
Figure 20: EFC21 and 1177 in Split mode Flow Diagram
* See Pencil Filters on page 437

Varian, Inc.
User Manual 450-GC
Page: 157
Figure 21: EFC21 and 1177 in Splitless mode Flow Diagram
Page: 158
User Manual 450-GC
Varian, Inc.
The EFC25 is almost identical with the EFC21 the only exception is that the
pressure is monitored at the module itself rather than at the Injector. This allows
the EFC25 to be used with Purge and Trap devices between EFC and Injector.
Figure 22: EFC25 and 1177 Flow Diagram
Varian, Inc.
User Manual 450-GC
Page: 159
1177 Manual Pneumatics

The total flow into the system is adjusted using a 0800 mL/min manual flow
controller. The 1177 Injector uses a flow controller to supply the total flow into
the system with a back pressure regulator to control the column head pressure.
When the Injector is operated in the split mode the flow out of the split vent
relative to the flow through the column is defined as the split ratio.
In the splitless mode, gas does not flow through the split line from the Injector to
the 3-way solenoid valve (see Figure 21). Rather, gas from the flow controller
by-passes the Injector to pass through the 3-way solenoid valve. The back
pressure regulator uses this flow to control column head pressure, which in turn
controls carrier gas flow through the column.
Operation of the 1177 Injector

The following section describes how to operate the 1177Split/Splitless Capillary
Injector with the Varian 450-GC. It is separated into a series of procedures,
starting with installation of a column and basic programming of the Injector from
the keyboard, followed by detailed information on the various modes of
injection.
Column Installation
The Connect Capillary Column to Injector on page 15 procedure describes the
installation of a capillary column in a Varian 450-GC equipped with an 1177
Injector. Each step of the procedure is described in detail.
Condition the Column
For conditioning the capillary column see Column Installation and
Conditioning on page 23.
Column Installation in Detector
For connecting a capillary column into a detector, see Connect Capillary
Column to Detector on page 24.
Page: 160
User Manual 450-GC
Varian, Inc.
Setting 1177 Gas Flow Rates

The gas flow rates for the 1177 Split/Splitless Capillary Injector can be set using
manual pneumatics or Electronic Flow Control. Note that a positive flow through
the column must be set before heating the column.
Do not heat the column oven above 50 C without carrier gas flowing
through the column. The column phase can be irreversibly damaged.
EFC Pneumatics
Type EFC21 or EFC25 used with the 1177 Injector allows the user to set a
constant column head pressure, build a pressure program, or set a constant
column flow. In addition, a split ratio can be set or time programmed. A
pressure program is typically used to maintain the column flow at a constant
value while temperature programming the column oven. When Constant Flow
Programming is enabled, the pressure program needed to maintain constant
flow is derived whenever the method is loaded.
The 1177 is a pressure-controlled Injector; thus the column flow decreases with
increasing column temperature if the pressure remains constant. EFC method
parameters and status are accessible via the FLOW/PRESSURE
the 450-GC keyboard.
Varian, Inc.
User Manual 450-GC
key on
Page: 161
The Type EFC21 status field displays the actual column pressure (in the units
chosen in Setup), calculated column flow rate, calculated column linear velocity
and the split ratio. The split ratio status is either off if the split state is set to
OFF, or a whole number.
The lower part allows you to view/edit constant flow mode.
The following screen is an example of a type EFC21 method.
Constant Column Flow

Type EFC21/EFC25 with the 1177 will automatically build a pressure program
to keep the volumetric column flow rate constant during temperature
programming of the column oven when Constant Flow is selected.
The same general guidelines should be followed for all injection modes. If the
column is operated isothermally then the pressure should be kept constant. If
the column is temperature programmed then the pressure can either be held
constant or programmed. Programming the Injector pressure generally has no
significant impact on chromatography, other than a slight reduction in analysis
time. In some instances resolution may either improve or degrade depending
on the settings. A technique called Pressure Pulse is also available for use with
Constant Flow programs with Type EFC21/EFC25. Use the following guide for
setting Injector pressure and/or building a pressure program.
Page: 162
User Manual 450-GC
Varian, Inc.
Temperature programming the column oven results in an increase in carrier gas

viscosity which results in a decrease in column flow rate. This effect can be
offset by applying the appropriate column pressure program.
If Constant Flow Programming is enabled, a pressure program based on the
column parameters and the column oven temperature program will be
automatically rebuild parameter change result in an automatic rebuild of the
pressure program.
When entering a pressure program to maintain constant column flow rate, the
program is based on the column temperature program. If the column oven is
operated isothermally, then constant pressure is maintained to achieve a
desired flow rate.
Pressure Pulse
Once you have selected Constant Flow programming, a checkbox Pressure
Pulse becomes accessible.
Selecting Pressure Pulse gives you the option of enabling a pressure pulse,
setting the desired pressure and the duration for which the pressure should last.
Typically, the pressure pulse pressure is held for between 30 and 90 seconds.
The purpose of the pressure pulse is twofold. The higher pressure will prevent
the solvent vapor cloud from becoming excessively large allowing larger
injection volumes and providing more efficient passage of the sample into the
column. The higher pressure also causes higher flow rates into the column
making the transfer quicker and thus preventing excessive residence times in
the Injector with consequent decomposition of labile compounds. If you use
Pressure Pulse you need to perform a septum purge calibration using the
higher pressure pulse pressure.
Varian, Inc.
The GC will go ready based on the pressure as defined in pressure pulse.
When a run is started the column pressure as defined in pressure pulse will
remain for the Pulse Duration time. After the pulse duration time the
column pressure is calculated from the constant flow conditions.
User Manual 450-GC
Page: 163
Gas Saver
For type EFC21 and EFC25 a specific Gas Saver Flow and a timeout period
key and click on the Injector tab now choose
may be set. Press the setup
the correct Injector (Page 1 or Page 2 or Page 3).
A time entry of 0 turns the Gas Saver feature off. If a non-zero time is
entered, the Gas Saver timer will start incrementing. If a run is not started or a
new method is not loaded or download by Workstation, the set Gas Saver flow
rate will be activated (the instrument will go into stand-by). A message will be
logged in the instrument log. Stand-by is canceled by loading a method or
pressing the end stand-by key.
Page: 164
User Manual 450-GC
Varian, Inc.
Septum Purge Calibration

The 450-GC is equipped with a septum purge
for the Model 1177 split/splitless Injector and is
controlled by a manual needle valve. This is
located behind the front cover of the GC.
The manual needle valve can offer
advantages over fixed restriction types as it
can be adjusted to suit the more demanding
applications. For the accurate display of total
column flow and velocity it does require
calibration when columns of different length and diameter are installed.
With type EFC21, the septum purge calibration routine should be carried out
when the instrument is first set up or when a new column is installed or when a
significantly different pressure point is chosen.
Press the SETUP
key and click on Calibration.
The Calibration page will appear, choose Calibrate for the correct Injector (front,
middle or rear).
Enter the desired Column Head pressure. After a few seconds measure the
septum purge flow rate and adjust the septum purge valve (located behind the
column oven door) to the desired flow, enter this value (typical 3-5 mL/min) in
the Adjusted Septum Purge Flow Rate field.
Press OK.
Varian, Inc.
Typical 3-5 mL/min
User Manual 450-GC
Page: 165
Manual Pneumatics
Tools and equipment needed
Bubble or electronic flowmeter.

1. Turn the 1177 Split Flow Controller (on the GC pneumatics panel)
counterclockwise to open the split flow controller.
2. Adjust the Back Pressure Regulator (on the GC pneumatics panel) to
establish a positive column head pressure (monitored on the pressure
gauge).
Set the column head pressure based on the column installed in the GC.
For example, for a 30m x 250 m ID column, set the column head
pressure to 12-15 Psig to achieve 1 mL/min column flow rate at 50 C
oven temperature (helium).
3. Connect the flowmeter to the split vent on the left side of the GC and
measure the split vent flow rate. Turn the Split Flow Controller valve to
adjust the split vent flow rate to 50 mL/min.
4. Adjust the Septum Purge Needle valve to adjust the septum purge flow rate
to 3 - 5 mL/min. Readjust the split vent flow rate to 50 mL/min.
5. Before heating the column, purge the system with carrier gas for 10 - 15
minutes.
With manual pneumatics the split valve should be configured in the sample
delivery/valve table in set-up of the 450-GC. Split/splitless mode can be
programmed through the valve table in the sample delivery page of the GC
method.
Page: 166
User Manual 450-GC
Varian, Inc.
1177 Modes of Operation

The 1177 can be operated in several modes, depending on the nature of the
sample and requirements of the analysis. When designing an injection method the
most important parameters are:
The Injector insert used.
The Injector and column temperature when the injection is made.
The carrier gas flow profile through the Injector.
The following is a brief description of the method parameters used for each
injection mode. In all cases Electronic Flow Control (EFC) is used for carrier gas
control.
In many cases switching from one 1177 mode to another involves

changing the glass insert. A detailed stepwise procedure to carry out
this task is given in the Maintenance section of this manual, on page
171. In most injection modes the insert is installed with an O-ring.
Split Injection
The split mode is used when samples are relatively concentrated and for neat
samples. This mode of injection involves rapid vaporization of the sample
followed by sample splitting. Splitting involves directing a portion of the sample
into the column while the remainder is vented. The split ratio is defined as the
proportion of sample vented to the sample entering the column. With EFC
carrier gas control this parameter can be set automatically in the 1177 method.
Injector Insert
4 mm ID open insert packed with glass wool.
Column Installation
3.7 cm from the bottom of the column nut at the base of the Injector.
Isothermal 250 C.
Column Temperature
50 C initial for 0.1 min, ramp to 250 C at 20 C/min, hold 5 min.
Carrier Gas Control
Set the split mode to ON for the duration of the run in the 1177 method
section and set the split ratio to 100. The sample is split upon injection
and a representative portion representing 1/100th of the amount injected
enters the column. Note that the split ratio is a method specific parameter
and should be set appropriately for individual analyses. In addition the
Injector pressure or pressure ramp should be set to achieve the desired
column flow rate.
Table 29: Split Injection Typical Conditions
Varian, Inc.
User Manual 450-GC
Page: 167
Splitless Injection
The classical splitless injection technique involves vaporizing the sample in a
hot Injector and slow transfer to the column. The split state is OFF during the
sampling period; therefore, all of the injected sample should enter the column.
The initial column temperature is maintained for at least the sampling time to
trap all sample components at the head of the column. At the end of the
sampling period (typically 0.5 to 1.5 minutes) the split state is turned ON to vent
any residual sample or solvent from the Injector.
The following table describes typical method parameters for an isothermal
splitless injection.
Injector Insert
4 mm ID open insert packed with glass wool.
Column Position
Initial temperature isothermal 250 C.
Column Temperature
50 C initial for 1 min, ramp to 250 C at 20 C/min, hold 5 minutes.
Carrier gas control
Set the initial split mode to OFF and time program it to ON after 0.75
minutes. In this case the splitless sampling time is 0.75 minutes. The split
ratio during the split ON period should be set to 50. Set the appropriate
pressure or pressure ramp to achieve the desired column flow rate.
Table 30: Splitless Injection Method Parameters
Note that in all the above cases the parameters given are generic and need
optimization (including column position) for specific applications. Particular
care should be taken with the large volume mode of injection where the initial
Injector temperature and timing of the split states have to be carefully selected.
Page: 168
User Manual 450-GC
Varian, Inc.
Testing the 1177 Injector Performance

The following procedure describes how to test the performance of the 1177
Capillary Injector. This is best done with a test sample containing an
appropriate set of components for the installed detector. The following table
lists the series of test samples available for 450-GC.
Test Sample
Part Number
TCD
82-005048-01
ECD
82-005048-02
PFPD
82-005048-03
20.0 ng/L of n-dodecanethiol, tributylphosphate,

methyl parathion; 4000 ng/L of n-pentadecane in
iso-octane.
TSD
82-005048-04
2.00 ng/L of azobenzene, methyl parathion; 4.00

ng/L malathion and 4.00 g/L C17 in iso-octane.
FID
82-005048-07
Note: If the FID test sample is not available, the TCD test sample can be used if first
diluted 100:1.
Table 31: Detector Test Samples
To run one of these test samples, use the chromatographic conditions listed
previously for the injection technique you are currently using. The detector
should be operated at the most sensitive range, e.g., 12 for FID and TSD, 0.05
for TCD, 10 for PFPD and 1 for ECD. The resultant chromatogram on page 419
should approximate that shown in the detector section of this manual.
Varian, Inc.
User Manual 450-GC
Page: 169
1177 Injector Assembly

1
2
3
4
5
1.
2.
3.
4.
6
7
8
9
10
11
12
13
14
5.
Injector Nut (392597501)

Injector Nut Wrench (390842300)
Knob (392597101)
Inject Switch Assembly (390820601)
Septum, 9 mm
BTO (lowest bleed, CR298713)
Marathon (Autosampler, CR239778)
Advanced Green 3 (general purpose, CR246713)
Septum pick (7200008400)
Septum Purge Head
Pneumatic Type
Stainless Steel
UltiMetal
EFC21
392597301
392597303
EFC25 or Manual
392597302
392597304
Pneumatics
6. Purge head screw (2x 391866308)
7. O-ring, Liner
Graphite, 6.5mm for Splitless (392611930)
Viton, 6.3mm (8850103100)
8. Spacer (39258101)
1
9. Glass Insert (default 392611927 More liners)
10. Injector Body
Stainless Steel (392599401)
UltiMetal (392599411)
Manual (392599501)
11. Column Ferrule (see table below)
12. Capillary Column Nut (394955100)
13. Insulation
14. Cover
Figure 23: 1177 Injector Assembly 1
Teflon
Column ID
0.25 mm ID
0.32 mm ID
0.53 mm ID
Holes
1
1
2
1
1
2
1
Vespel
40% Graphite
60% Vespel
Max 250C
Max 350C
Max 400C
CR214103
CR212103
CR213103
CR214104
CR212104
CR213104
CR212124
CR213124
CR214105
CR212105
CR213105
CR212125
CR213125
CR214108
CR212108
CR213108
Table 32: 1177 Column Ferrules 1/16"
Graphite
SilTite
Max 450C
CR211104
CR211124
CR211105
CR211125
CR211108
Metal, GC/MS
SG073300
SG073301
SG073302
1 In combination with the PFPD detector the Siltek liner (RT210462145) must be used.
Page: 170
User Manual 450-GC
Varian, Inc.
Maintenance
Before maintaining the 1177 Injector please read the common
Injector/septum maintenance information in the section Maintenance,
on page 432.
The 1177 is a Split/Splitless capillary Injector. Typically, to change from Split
operation to Splitless involves changing the Injector insert. Also replace the
insert on routine base. This is especially important when dirty samples are
analyzed.
Tools Required
Tweezers or septum pick (P/N 72-000084-00).

Injector nut wrench (P/N 03-908423-00).
Philips screwdriver (long handle).
Clean laboratory tissue.
The Injector nut may be hot. Lower the Injector

temperature to 50C and permit the Injector nut to
cool before proceeding.
Remove the Glass Insert

Follow these steps to remove the glass insert from the 1177 Injector.
1. Use the Injector nut wrench to remove the
Injector nut. Place the nut on a clean
surface (e.g., clean tissue).
2. Remove the inject switch by unscrewing

the retaining nut.
Varian, Inc.
User Manual 450-GC
Page: 171
3. Unscrew the 2 captive screws holding the top

of the Injector to the base. Carefully move this
assembly upwards and to one side. The
Septum purge line and carrier gas supply lines
may hinder movement of the top piece
somewhat.
When using a CP-8400 AutoSampler, remove the Injector access plate

by removing the 2 retaining screws and firmly lifting the plate. It may be
hot if another Injector is also installed and powered. The plate may be a
little tight, do not force it off. Lift straight up, a slight back and forth
rocking may help remove it.
4. Use a laboratory tissue to grasp the glass
insert and remove it from the Injector body.
Replace the Glass Insert

Follow these steps to replace the glass insert in the 1177 Injector.
1. Using tweezers or clean lab tissue, carefully slide the new insert into the
Injector body. Place a new seal over the insert.
2. Carefully place the top of the Injector over the insert. Tighten the 2 captive
screws alternately for uniform sealing. Note that placing the top piece onto
the body may take some care since the gas supply line and septum purge
lines may have minor resistance to movement.
3. Install a new septa, place the Injector nut on the Injector and tighten by
hand until you feel some resistance, then tighten an extra 1/4 turn using the
Injector nut wrench.
After the Injector nut has been replaced, check the split vent and
septum purge flow rates to ensure these values have not changed.
4. Condition the insert by setting the 1177 Injector to the split mode and
purging with carrier gas for 30 min at 300C.
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User Manual 450-GC
Varian, Inc.
Injector body cleaning

To clean the Injector body, proceed as follows:
1. Set the column oven temperature to 45 C and the 1177 Injector
temperature to 50 C. Wait for the zones to reach their set temperatures
and then turn the column oven off by unchecking the checkbox Power
located in the Oven screen
2. Use the 5/16 open-end wrench to loosen the capillary column nut.
3. By hand, carefully withdraw the fused silica column and nut from the
Injector assembly. Set the column nut and column end on the floor of the
GC oven.
Use proper eye and skin protection. Methanol and acetone are toxic and
flammable chemicals. Exercise appropriate precautions when these chemicals
are used.
4. Remove the Injector nut, septum and top of Injector.
5. Remove the Insert.
6. Moisten a cotton swab and a stick with methanol and gently swab center of
the Injector body.
7. Moisten a cotton swab on a stick with iso-octane and gently swab the
center of the Injector body.
8. Replace the insert, seal, Injector top, septum and Injector nut.
9. Examine the end of the fused silica column to ensure that it has not been
damaged. Slide the end of the fused silica column into the opening of the
Injector.
Varian, Inc.
User Manual 450-GC
Page: 173
10. Gently twist the column nut in the opposite direction used to tighten the nut.
Place the column nut on the end of the Injector and tighten the nut. This
procedure minimizes twisting the column.
11. Use the 5/16 open-end wrench and tighten with 1/6-turn to secure the
column in place.
12. To check whether the Injector is leak-tight, connect a flow meter to the split
vent. Set the Relay to the split mode. If the flow meter indicates a flow less
than previously measured, the Injector has a leak.
Turn the column oven back on by checking the checkbox Power in the oven
screen
Page: 174
User Manual 450-GC
Varian, Inc.
1079 PTV Injector - Injectors
THE 1079 PTV INJECTOR
The 1079 is optimized as Programmable Temperature Vaporizing (PTV) Injector and is

also used for large volume injections (LVI).
The 1079 PTV represents the latest evolution in Varian's Injector technology - extending
the benefits of Varian's patented 1093 Septum-equipped Programmable Injector (SPI),
to include split and splitless injection.
The 1079 PTV delivers improved chromatographic performance and increased GC uptime, is compatible with the full range of open tubular columns and is capable of
isothermal or temperature programmed operation.
Advanced Performance
Five modes of operation: split, splitless, temperature-ramped splitless, Large Volume
Injection (LVI) and cold on-column; allow maximum Injector flexibility.
Varian, Inc.
Temperature-programmable on-column mode optimizes the recovery of polar

and thermolabile compounds.
Large-volume injections in temperature-ramped splitless mode means less
sample preparation and increased sensitivity.
Manual or electronic control of gas flow guarantees optimum retention time
reproducibility.
An insert sealing design enables easy insert removal and replacement.
A unique inlet design for unparalleled system inertness allows analysis of even
the most thermolabile compounds.
User Manual 450-GC
Page: 175
Injectors 1079 PTV Injector
Features of the 1079 PTV Injector
The 1079 PTV can be operated isothermally or temperature programmed. The

temperature range of the Injector is from -99 to 450 C. Sub-ambient
temperatures are achieved using cryogenic cooling.
Changing from one injection mode to another typically involves a change of

Injector insert and a modification to the Injector program. Glass inserts can be
easily changed from the top of the Injector.
Temperature programming in the splitless mode gives better recovery of labile

analytes and is useful for wide boiling point mixtures.
The Injector temperature profile keeps the septum cool while maintaining the
point of injection closer to the setpoint temperature.
The 1079 PTV Injector design facilitates large volume injection (5 - 250 L).
The 1079 PTV uses positive septum purge to minimize the adsorption of
sample onto the Injector septum and to prevent contaminants from the septum
entering the column.
The 1079 PTV combined with the ChromatoProbe on page 198 is an effective
tool for chromatographic analysis of dirty samples (liquids, solids and slurries,
blood, urine or milk), without cleanup or extraction. The ChromatoProbe is
based on intra-Injector thermal extraction of the semi volatile compounds in a
sample microvial, while non-volatile residue is retained in the microvial, which is
disposed of after the analysis.

aligned with, the injection port of the 1079 PTV Injector nut. The GC run is
started when the actuator is depressed by the syringe barrel, or manually
pressed at the moment of sample injection. The GC run can also be manually
(only in local automation) started by pressing the START

be very hot during instrument operation and should NOT
be touched with unprotected hands.
1079 PTV Injector Inserts

Click here to see the 1079 PTV Injector Inserts, on page 451.
Note that all 1079 PTV Injector inserts are deactivated for maximum inertness.
Page: 176
User Manual 450-GC
Varian, Inc.
1079 PTV Injector Assembly

1
2
1.
4
2.
3.
5
6
4.
5.
6.
7.

Injector Nut Wrench, (390842300)
Automatic Start Switch (390820601)
Septum, 11.5 mm
Septum pick, 7200008400
Septum Support (391867600)
Insert Ferrule (392534201)
Glass Insert, default 392611945 More liners
Injector Body
Pneumatic Type
Stainless Steel
UltiMetal
EFC
392544001
392544011
Manual Pneumatics
392559601
392559611
8.
9.
Column Ferrule, see table below

Bottom Nut (394955100)
8
9
Figure 24: 1079 PTV Injector Assembly
Teflon
Column ID
0.25 mm ID
0.32 mm ID
0.53 mm ID
Varian, Inc.
Holes
1
1
2
1
1
2
1
Vespel
40% Graphite
60% Vespel
Max 250C
Max 350C
Max 400C
CR214103
CR212103
CR213103
CR214104
CR212104
CR213104
CR212124
CR213124
CR214105
CR212105
CR213105
CR212125
CR213125
CR214108
CR212108
CR213108
Table 33: 1079 Column Ferrules 1/16"
User Manual 450-GC
Graphite
SilTite
Max 450C
CR211104
CR211124
CR211105
CR211125
CR211108
Metal, GC/MS
SG073300
SG073301
SG073302
Page: 177
1079 PTV Modes of Injection

The 1079 PTV injection mode is defined by the Split Vent program and by
choice of insert. The Split Vent is controller differently based on the pneumatics
installed, with EFC the split valve is controlled from the Injector section, with
manual pneumatics the external events control the split valve. The following are
brief descriptions of the various modes of injection; more detailed information
on each mode is given later in this section. The 1079 PTV is optimized for PTV
and LVI, but it is possible that he Injector can work in other modes.
Temperature Ramp Splitless Mode
The splitless temperature ramp mode is preferred for compounds that are
altered by higher temperatures (thermolabile). Also, the splitless temperature
ramp mode is used with wide boiling range mixtures (e.g., hydrocarbon
mixtures). 2 glass inserts are recommended when operating in the splitless
temperature ramp mode: 1) The 2 mm ID glass wool packed insert is used for
non-polar compounds at levels >1 ng; and 2) the 0.5 mm ID open insert is used
for thermolabile and/or polar compounds at trace levels (pg level).
In the splitless temperature ramp mode, the Injector is held at a temperature
that is equal to or slightly below the boiling point of the injection solvent. The
sample is deposited on the surface of the insert. After injection, the temperature
of the Injector is increased rapidly (ramped). As the temperature of the Injector
increases, the sample then vaporizes and is swept onto the column.
Large Volume
In the large volume mode of injection typically > 5 L of sample is deposited
into the Injector slowly, the solvent is vented and then the components of
interest are transferred to the column. This is done using a special split vent
program and an Injector temperature ramp. The CP-8400/8410 AutoSampler
allows automated injection of up to 250 L of sample.
Page: 178
User Manual 450-GC
Varian, Inc.
Split Mode
The split injection mode is preferred for the analysis of relatively concentrated
samples. The sample is split in the Injector with a representative portion
entering the column. The split injection mode provides the shortest sampling
time which leads to sharp chromatographic peaks. Use the 3.4 mm open insert,
the 3.4 mm ID fritted insert, or the packed 3.4 mm ID insert when operating in
the split mode.
In the split injection mode, the sample volume is typically 1 L or less. Early
eluting compounds usually appear as very sharp peaks. In some cases, the
peak width is less than one second. Thus, it is important that you inject the
sample as quickly as possible. If the sample injection time, (time between the
insertion and removal of the syringe needle from the Injector) exceeds the peak
width, peaks can broaden, tail or chromatographic performance will be
degraded. With broader, later eluting peaks, it is less important that you inject
the sample quickly. The split ratio (fraction of sample that enters the column) is
the ratio of the flow of carrier gas out the split vent to the flow through the
column. The 1177 Split/Splitless Injector on page 153 is optimized for Split
application.
Isothermal Splitless Mode

The 3.4 mm insert packed with glass wool is typically used for isothermal
splitless injection. The small capillary section of the glass insert fits snugly
around the syringe needle and restricts backflush of the sample vapor during
injection. In the splitless injection mode, the sample enters the column during a
variable sampling time at the beginning of the analysis. This period is typically
30 - 90 seconds during which there is no flow from the Injector to the split vent.
After the sampling time, the Injector is vented to clean any residual sample out
of the Injector. The 1177 Split/Splitless Injector on page 153 is optimized for
Splitless application.
On-Column Modes
In the on-column modes the column is sealed to the glass insert (0.18 - 0.53
mm columns). This ensures that there is maximum transfer of sample to the
column. In the on-column modes the sample is normally injected at or below
the solvent boiling point and then the Injector is ramped to transfer the sample
onto the column. The 1093 OC Injector, on page 231 is optimized for OnColumn applications. Especially for applications operating at an oven
temperature range that require short wire-bore columns.
Varian, Inc.
User Manual 450-GC
Page: 179
1079 Injector Screen

The 1079 Injector screen allows modifying the Injector parameters.
With the Enable checkbox it is possible to enable/disable the Injector
temperature control.
In the Temperature box the wanted Injector temperature can be set.
The Split State controls the flow of carrier gas through the Injector during the
analytical run. When the Split State is unchecked, most of the sample injected
is directed onto the column. When the Split State is checked, the sample is split
in the Injector with typically the smaller fraction entering the column and the
larger fraction being vented.
In the example below is a splitless injection. The Injector is held in the split state
for the initial period with split ratio of 20. When the run is started the split state
will switched Off. After 0.9 minute the split is switched on again.
The Coolant checkbox turns on or off the cryogenic supply to the Injector, if
installed. In the example below the cooling will start when the Injector
temperature reaches the 250 C. In the
setup screen of the Injector tab 1079 some
rarely changed coolant parameters can be
changed, like coolant type (LN2, LCO2 or Air)
and coolant timeout.
Coolant time-out refers to the period of time
for which the coolant will remain on after it is turned on. For example, if the set
temperature has not been reached or the run has not started within the
specified time, the coolant supply will be turned off.
Page: 180
User Manual 450-GC
Varian, Inc.
1079 PTV Electronic Flow Control (EFC)

The Electronic Flow Control module used on a 1079 PTV Injector is identified
as a type EFC21 or EFC25. In simple terms it duplicates the behavior of the
1079 PTV manual pneumatics system in that there is an inlet mass flow
controller supplying carrier gas to the Injector and a pressure control valve
downstream from the Injector which sets the Injector pressure. As Injector
pressure determines the rate of carrier gas flow through the column, this
pressure is monitored close to the point of injection. The type EFC21 flow
diagram shown below is an indication of the control mechanism of this type of
EFC module.
Figure 25: EFC21 and 1079 in Split mode Flow Diagram
*Pencil Filters on page 437

Type EFC21 allows the user set constant Injector pressure or constant flow. In
addition the split ratio can be programmed.
Varian, Inc.
User Manual 450-GC
Page: 181
The EFC25 is almost identical as the EFC21 the only exception is that the
pressure is monitored at the module itself rather than at the Injector. This allows
the EFC25 to be used with Purge and Trap devices upstream from the Injector.
Page: 182
User Manual 450-GC
Varian, Inc.
1079 PTV Manual Pneumatics

The total flow into the system is adjusted using a 0800 mL/min manual flow
controller. The 1079 PTV Injector uses a flow controller to supply the total flow
into the system with a back pressure regulator to control the column head
pressure. When the Injector is operated in the split mode the flow out the spilt
vent relative to the flow through the column is defined as the split ratio.
In the splitless mode, gas does not flow through the split line from the Injector to
the 3-way solenoid valve. Rather, gas from the flow controller by-passes the
Injector to pass through the 3-way solenoid valve. The back pressure regulator
uses this flow to control column head pressure, which in turn controls carrier
gas flow through the column.
Operation of the 1079 PTV Injector

The following section describes how to operate the 1079 PTV Injector with the
Varian 450-GC. It is separated into a series of procedures, starting with
installation of a column and basic programming of the Injector from the
keyboard, followed by detailed information on the various modes of injection.
Column Installation
installation of a capillary column in a Varian 450-GC equipped with a 1079 PTV
Injector. Each step of the procedure is described in detail.
For conditioning the capillary column see Column Installation and Conditioning
on page 23.
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User Manual 450-GC
Page: 183
Setting 1079 PTV Gas Flow Rates

The gas flow rates for the 1079 PTV Injector can be set using manual
pneumatics or Electronic Flow Control. Note that a positive flow through the
column must be set before heating the column.
Do not heat the column oven above 50 C without carrier gas flowing through
the column. The column phase can be irreversibly damaged by exposure to
oxygen at elevated temperatures. Allow 10 15 minutes to purge the column
before heating.
EFC Pneumatics
Type EFC21 used with the 1079 PTV Injector allows the user to set a constant
column head pressure, build a pressure program, or set a constant column
flow. In addition, a split ratio can be set or time programmed. A pressure
program is typically used to maintain the column flow at a constant value while
temperature programming the column oven. When Constant Flow Programming
is enabled, the pressure program needed to maintain constant flow is derived
whenever the method is loaded.
The 1079 PTV is a pressure-controlled Injector; thus the column flow decreases
with increasing column temperature if the pressure remains constant. EFC
method parameters and status are accessed via the FLOW/PRESSURE
key on the 450-GC keyboard.
Page: 184
User Manual 450-GC
Varian, Inc.
The Type EFC21 status field displays the actual column head pressure (in the
units chosen in Setup), calculated column flow rate, calculated column linear
velocity and the split ratio. The split ratio status is either off if the split state is
set to OFF, or a whole number.
The lower part allows you to view/edit constant flow mode.
The following screen is an example of a type EFC21 method.
Constant Column Flow

Type EFC21 with the 1079 PTV builds automatically a pressure program to
keep the column flow rate constant during temperature programming of the
column oven when Constant Flow is selected.
The same general guidelines should be followed for all injection modes. If the
column is operated isothermally then the pressure should be kept constant. If
the column is temperature programmed then the pressure can either be held
constant or programmed. Programming the Injector pressure generally has no
significant impact on chromatography, other than a slight reduction in analysis
time.
In some instances resolution may either improve or degrade depending on the
settings. For larger volume hot splitless injections, a technique called Pressure
Pulse is also available for use with Constant Flow programs with Type EFC21.
Use the following guide for setting Injector pressure and/or building a pressure
program.
Varian, Inc.
User Manual 450-GC
Page: 185
Temperature programming the column oven results in an increase in carrier gas

viscosity which results in a decrease in column flow rate. This effect can be
offset by applying the appropriate column pressure program.
If Constant Flow Programming is enabled, a pressure program based on the
column parameters and the column oven temperature program will be
automatically built. Any parameter change result in an automatic recalculation
of the pressure program.
When entering a pressure program to maintain constant column flow rate, the
program is based on the column temperature program. If the column oven is
operated isothermally, then constant pressure is maintained to achieve a
desired flow rate.
Pressure Pulse
Once you have selected Constant Flow programming, a checkbox Pressure
Pulse becomes accessible.
Selecting Pressure Pulse gives you the option of enabling a pressure pulse,
setting the desired pressure and the duration for which the pressure should last.
Typically, the pressure pulse pressure is held for between 30 and 90 seconds.
The purpose of the pressure pulse is two fold. The higher pressure will prevent
the solvent vapor cloud from becoming excessively large allowing larger
injection volumes and providing more efficient passage of the sample into the
column. The higher pressure also causes higher flow rates into the column
making the transfer quicker and thus preventing excessive residence times in
the Injector with consequent decomposition of labile compounds. If you use
Pressure Pulse you will need to perform septum purge calibration using
the higher pressure pulse pressure.
Page: 186
The GC will go ready based on the pressure as defined in pressure pulse.
When a run is started the column pressure as defined in pressure pulse will
remain for the Pulse Duration time. After the pulse duration time the
column pressure is calculated from the constant flow conditions.
User Manual 450-GC
Varian, Inc.
Gas Saver
For type EFC21 a specific Gas Saver Flow and a timeout period may be set.
key and click on the Injector tab, choose the correct

Press the setup
Injector (Page 1 or Page 2 or Page 3).
A time entry of 0 turns the Gas Saver feature off. If a non-zero time is
entered, the Gas Saver timer will start incrementing. If a run is not started or a
new method is not loaded or download by Workstation, the set Gas Saver flow
rate will be activated (the instrument will go into stand-by). A message will be
logged in the instrument log. Stand-by is canceled by loading a method or
pressing the end stand-by key.
Varian, Inc.
User Manual 450-GC
Page: 187

for the Model 1079 PTV Injector and is
controlled by a manual needle valve. This is
located behind the front cover of the GC.
calibration when columns of different length
and diameter are installed.
With type EFC21, the septum purge calibration routine should be carried out
when the instrument is first set up or a new column is installed or when a
significantly different pressure point is chosen. Press the SETUP
click on Calibration.
key and
middle or rear).
Press OK.
Page: 188
Typical 3-5 mL/min

User Manual 450-GC
Varian, Inc.
Manual Pneumatics
Tools and equipment needed
Bubble or electronic flowmeter, e.g., Varian Intelligent Digital Flowmeter, 01900115-00.

1. Turn the 1079 PTV Split Flow Controller (on the GC pneumatics panel)
counterclockwise to open the split flow controller.
2. Adjust the Back Pressure Regulator (on the GC pneumatics panel) to
establish a positive column head pressure (monitored on the pressure
gauge).
Set the column head pressure based on the column installed in the GC.
For example, for a 30m x 250 m ID column, set the column head
pressure to 12-15 psig to achieve 1 mL/min column flow rate at 50 C
oven temperature (helium).
3. Connect the flowmeter to the split vent on the left side of the GC and
measure the split vent flow rate. Turn the Split Flow Controller valve to
adjust the split vent flow rate to 50 mL/min.
4. Adjust the Septum Purge Needle valve to adjust the septum purge flow rate
to 3-5 mL/min. Readjust the split vent flow rate to 50 mL/min.
5. Before heating the column, purge the system with carrier gas for 10 - 15
minutes.
Varian, Inc.
User Manual 450-GC
Page: 189
1079 PTV Modes of Operation

The 1079 PTV can be operated in several modes, depending on the nature of
the sample and requirements of the analysis. When designing an injection
method the most important parameters are:
The Injector insert used and the position of the column within the insert.
The Injector and column temperature when the injection is made.
The carrier gas flow profile through the Injector.
The following is a brief description of the method parameters used for each
injection mode. In all cases Electronic Flow Control is used for carrier gas
control.
In many cases switching from one 1079 PTV mode to another involves
changing the glass insert. A detailed stepwise procedure to carry out
this task is given in the Maintenance section of this manual, on page
195. In most injection modes the insert is installed with a graphite
ferrule. Use the special fixture supplied with the 1079 PTV accessory kit
to install the ferrule correctly on the insert.
Isothermal Split Injection
The split mode is used when samples are relatively concentrated and for neat
samples. This mode of injection involves rapid vaporization of the sample
followed by sample splitting. Splitting involves directing a portion of the sample
into the column while the remainder is vented. The split ratio is defined as the
proportion of sample vented to the sample entering the column. With EFC
carrier gas control this parameter can be set automatically in the 1079 PTV
method.
Injector Insert
Install the fritted split insert (03-926119-46) or unpacked split insert (03926119-45). See instructions in the Maintenance section on page 195 for
changing the 1079 PTV insert.
Column Installation
7.5 cm from the bottom of the column nut at the base of the Injector
Isothermal 250 C.
Column Temperature
Carrier Gas Control
Set the split mode to ON for the duration of the run in the 1079 PTV method
section and set the split ratio to 100. The sample will be split upon injection
and a representative portion representing 1/100th of the amount injected will
enter the column. Note that the split ratio is a method specific parameter and
should be set appropriately for individual analyses. In addition the Injector
pressure or pressure ramp should be set to achieve the desired column flow
rate.
Table 34: Split Injection Typical Conditions
Page: 190
User Manual 450-GC
Varian, Inc.
Isothermal Splitless Injection

The classical splitless injection technique involves vaporizing the sample in a
hot Injector and slow transfer to the column. The split state is OFF during the
sampling period; therefore, all of the injected sample should enter the column.
The initial column temperature is maintained for at least the sampling time to
trap all sample components at the head of the column. At the end of the
sampling period (typically 0.5 to 1.5 minutes) the split state is turned ON to vent
any residual sample or solvent from the Injector.
The following table describes typical method parameters for an isothermal
splitless injection.
Injector Insert
Install the standard 3.4 mm ID splitless insert (P/N 03-926119-45).
Column Position
Initial temperature isothermal 250 C.
Column Temperature
Carrier gas control
ratio during the split ON period should be set to 50. Set the appropriate
pressure or pressure ramp to achieve the desired column flow rate.
Table 35: Isothermal Splitless Injection Method Parameters
Temperature Ramped Splitless Injection

This is a similar technique to isothermal splitless except the sample is
vaporized slowly, utilizing temperature programming. This controlled mode of
vaporization reduces the risk of mass discrimination and thermal breakdown of
sample components during the sampling period. The sample is deposited in the
Injector as a liquid, therefore the initial Injector temperature must be close to the
solvent boiling point and there must be a nearby surface for the sample to be
retained on. For this mode of injection either a narrow bore (0.5 mm) insert or a
glass wool packed insert is used. This facilitates efficient transfer of the sample
to a surface from which it is then vaporized.
Note that the glass wool packet insert is not recommended for low levels of
polar analytes.
The following are typical method parameters for a temperature ramped splitless
injection. In this example hexane is used as the solvent which has a boiling
point of 68 C. Note that the sampling time and initial column hold time are 2
minutes to allow the Injector get to maximum temperature.
Varian, Inc.
User Manual 450-GC
Page: 191
Injector Insert
Column Position
Column Temperature
Carrier gas control
Install either the narrow bore 0.5 mm ID insert (03-926119-49) or the

glass wool packed 2 mm ID insert (03-926119-53) or the open 3.4 mm ID
splitless insert (03-926119-45).
Initial temperature 65 C, hold for 0.1 minute, ramp to 250 C at
150 C/minute, hold 10 minutes.
ratio during the ON period should be set to 50. Set the appropriate
pressure or pressure ramp to achieve the desired column flow.
Table 36: Temperature Ramped Splitless Injection
On-column Injection
The wide-bore on-column mode uses a wider bore insert with a taper to allow
insertion of a 0.53 mm ID capillary column inside the insert. A standard gauge
GC syringe (26s) is used to deposit sample inside the column.
In case narrow bore columns are required, a retention gap is used as noncoated 0.53 mm ID pre-column.
This enables true on-column injection in a narrow bore column while using
standard syringes.
The Injector is temperature ramped to minimize sample decomposition due to
thermal effects or active sites.
The on-column technique involves some special setup of the 1079 PTV
Injector.
In the on-column mode the column has to be sealed within the insert. The
Injector nut, septum, septum support and insert are removed from the Injector.
The column is pushed up through the Injector until it protrudes past the top of
the Injector. The tapered on-column insert is then pushed onto the column to
make a seal between the polyimide coating on the column and the glass
surface. The insert is then lowered into the Injector and the septum support
installed without a graphite ferrule. The septum support must not be screwed
all the way down or the septum will not seal.
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User Manual 450-GC
Varian, Inc.
The following are typical conditions for carrying out an on-column injection. The
Injector should be maintained at 10 - 20 C below the solvent boiling point at
injection. In this example the solvent is hexane which has a boiling point of
68 C.
Injector Insert
Install the on-column insert (P/N 01-900109-07) for wide bore (0.53 mm
ID) columns.
Seal/Position Column
Seal the column within the tapered insert.
Initial temperature 50 C, hold for 0.1 minute, ramp to 250 C

at 150 C/minute, hold 10 minutes.
Column Temperature
Carrier gas control
Split does not apply in on-column mode. The Splitless vent flow must be
set to 20 mL/min or greater in Setup. Delete any splitter program and
set initial state to off in the Injector screen.
Table 37: On-Column Injection
Large Volume Injection

The large volume injection technique is used where the absolute lowest level of
detection is required. Up to 250 L of sample may be introduced into the 1079
PTV Injector. The sample is injected at a very slow rate while the Injector
temperature is set a few degrees below the solvent boiling point. In the example
below hexane is used as the solvent which has a boiling point of 68 C.
Using the large volume injection technique the Injector is maintained in the split
ON state at the beginning of the run to vent most of the solvent. The sample
components are trapped in the Injector insert so the same type of insert is used
as for temperature ramped splitless injection. The split state is then
programmed to OFF and the Injector temperature ramped to transfer the
sample components to the head of the column. The following are typical
conditions for a large volume injection.
Varian, Inc.
User Manual 450-GC
Page: 193
Injector Insert
Install either the narrow bore 0.5 mm ID insert (03-926119-49) or the

glass wool packed 2 mm ID insert (03-926119-53).
Column Position
Initial temperature 66 C, hold for 1 minute, ramp to 250 C at

150 C/minute, hold 10 minutes.
Column Temperature
Carrier gas control
Set the initial split mode to ON, time program it to OFF after 1.00 minutes
and then back to ON after 3.00 minutes. The split ratio should be set to 50
during the split ON periods.
Table 38: Large Volume Injection
Note that in all the above cases the parameters given are generic and will have
to be optimized for specific applications. Particular care should be taken with
the large volume mode of injection where the initial Injector temperature and
timing of the split states have to be carefully selected.
Testing the 1079 PTV Injector Performance

PTV Injector. This is best done with a test sample containing an appropriate set
of components for the installed detector. The following table lists the series of
test samples available for Varian GC.
Test Sample
Part Number
TCD
82-005048-01
3.00 g/l of C14, C15 and C16 in iso-octane.
ECD
82-005048-02
33.0 pg/l of lindane and aldrin in iso-octane.
PFPD
82-005048-03
20.0 ng/l of n-dodecanethiol, tributylphosphate,

methyl parathion; 4000 ng/l of n-pentadecane in isooctane.
TSD
82-005048-04
2.00 ng/l of azobenzene, methyl parathion; 4.00

ng/l malathion and 4.00 g/l C17 in iso-octane.
FID
82-005048-07
30 ng/l of C14, C15 and C16 in iso-octane.
diluted 100:1.
Table 39: 1079 PTV Test Samples
To run one of these test samples, use the chromatographic conditions listed previously
for the injection technique you are currently using. The detector should be operated at
the most sensitive range, e.g., 12 for FID and TSD, 0.05 for TCD, 10 for PFPD and 1 for
ECD. The resultant chromatogram should approximate that shown in the detector
section of this manual. Some chromatographic interpretation information is given in the
troubleshooting section of this manual.
Page: 194
User Manual 450-GC
Varian, Inc.
Maintenance
The 1079 PTV Injector that can be operated in several modes. These modes
include split, splitless, on-column and large volume injection. Typically, to
change from one mode of operation to another involves changing the Injector
insert. The insert should be replaced on a routine basis. This is especially
important when dirty samples are analyzed.
After prolonged use, the 1079 PTV Injector glass insert may need to be
replaced with a new insert.
Tools Required
Tweezers or septum pick (P/N 72-000084-00)

Injector nut wrench (P/N 03-908423-00)
Flat-blade screwdriver (short handle)
Clean laboratory tissue
Graphite ferrules (P/N 03-925342-01)
Insert/ferrule positioning tool (P/N 03-925385-00)
1. Use the Injector nut wrench to

remove the Injector nut. Place
the nut on a clean surface (e.g.,
clean tissue).
THE INJECTOR NUT MAY BE HOT. LOWER THE
INJECTOR TEMPERATURE TO 50C AND PERMIT THE
INJECTOR NUT TO COOL BEFORE PROCEEDING.
2. Unscrew the 2 T-20 Torx screws holding

the top of the Injector to the base. Carefully
move this assembly to one side. The
Septum purge line and carrier gas supply
lines may hinder movement of the top
piece somewhat.
Varian, Inc.
User Manual 450-GC
Page: 195
CP-8400 AutoSampler, remove the Injector access plate by removing

the 2 retaining screws and firmly lifting the plate. It may be hot if
another Injector is also installed and powered. The plate may be a little
tight, do not force it off. Lift straight up, a slight back and forth rocking
may help remove it.
3. With tweezers or septum pick, remove the septum.
Replace the Injector septum each time the glass insert is replaced.
4. Use a clean flat-blade screwdriver to

unscrew the septum support nut until it is
loose.
5. Remove the septum support with the
tweezers or septum pick.
Typically, when the septum support is removed, the insert and ferrule
remain in the septum support. If the ferrule and insert are in the
Injector body after the septum support nut is removed, use the
tweezers to grasp the top of the insert and lift it from the Injector body.
6. Use a laboratory tissue to grasp the glass

insert and remove it from the septum support
nut.
7. To remove the graphite ferrule from the glass
insert, use clean lab tissues to hold the graphite ferrule and the glass insert.
Gently turn the glass insert while you pull off the graphite ferrule.
Page: 196
User Manual 450-GC
Varian, Inc.

1. Use the insert/ferrule positioning tool supplied in the 1079 PTV accessory
kit to set the 5 mm graphite ferrule on the insert and in the septum support.
See the pictures for an exploded view of the tool with septum support,
insert ferrule, glass insert and tool as well as the correct position of the tool
when setting the ferrule. The objective is to have the ferrule set with the
bottom of the insert, flush with the bottom of the tool.
Septum Support
Insert Ferrule
Glass Insert
Insert/ferrule
positioning tool (392538500)
2. Position the tool as shown on a flat, clean surface. Use clean laboratory
tissue on the surface. Tighten the septum support finger-tight. Holding the
tool with a 5/8" wrench, give the septum support an extra 1/3 to 1/2 turn
past finger-tight. Now unscrew the septum support which now has the
ferrule and insert seated in it. If there is any graphite extruded past bottom
of the septum support, cut it off with a blade or sharp knife. Carefully wipe
off any graphite flakes which may adhere to the insert or septum support.
Gripping the septum support unit with a piece of laboratory tissue, carefully
put this unit in the 1079 PTV Injector and tighten the septum support 1/6turn past finger-tight.
3. Use tweezers to place a new septum over the septum support.
If the septum has a Teflon face, place the Teflon face toward (down) the
column.
4. Place the Injector nut on the Injector and tighten by hand until you feel
some resistance, then tighten an extra 1/4 turn using the Injector nut
wrench.
5. Condition the insert by setting the 1079 PTV Injector to the split mode and
purging with carrier gas for 30 min at 300 C.
Varian, Inc.
User Manual 450-GC
Page: 197
ChromatoProbe
How to Assemble the ChromatoProbe
Refer to the exploded view on the next page.
The ChromatoProbe assembly consists of the adapter, guide, ChromatoProbe,
ChromatoProbe cap and the small and large O-rings. One small O-ring is
placed on the ChromatoProbe shaft; the other is placed on the ChromatoProbe
cap shaft. The large O-ring is placed in the groove in the bottom of the adapter
which connects to the 1079 Injector body.
The storage stand may be used to hold and protect the ChromatoProbe or
ChromatoProbe cap. The user may find the small holes in the top of the storage
stand useful for holding microvials during filling or just prior to running an
analysis.
How to Install the ChromatoProbe

The ChromatoProbe is designed to be installed into the 1079 Injector body.
Several parts of the Injector must be removed and
replaced with the appropriate parts from the
ChromatoProbe kit before the ChromatoProbe can be
connected. Remove the Injector nut, septum, septum
support (gold piece) and the Injector insert. The Injector
nut, septum support and the Injector insert should be set
aside for use when you use the Injector in the normal
manner. Install the glass insert included in the
ChromatoProbe kit into the Injector (3.4 mm split insert).
This insert must be installed with the small orifice at the
bottom, as shown in the picture. This position will allow the
ChromatoProbe to slip into the insert during operation.
Use the following procedure to set the insert, ferrule and
the guide.
1. Place the 1/4 inch graphite ferrule over the open end of the insert so that
the tapered end of the ferrule is up.
2. Place the insert and the ferrule into the guide so that the ferrule can fit
snugly inside the guide.
3. Using the ferrule positioning tool (P/N 03-925385-00) included with the
1079 Injector, place the insert and guide into the tool and screw the guide
clockwise with the key provided to tighten the ferrule around the insert. The
insert is positioned correctly if the bottom of the insert is aligned with the
bottom of the ferrule positioning tool. Refer to the maintenance section of
the 1079 for removal of the glass insert on page 195.
Page: 198
User Manual 450-GC
Varian, Inc.
Once the ferrule is positioned and tightened, the guide and insert can be placed
into the 1079 Injector body. Screw the guide into the Injector body with the key
and tighten snugly.
At this point the ChromatoProbe is ready to be attached onto the Injector. The
adapter is attached to the Injector such that the portion containing the large Oring is screwed onto the Injector. Tighten this fingertight to prevent any leaks.
DO NOT use a tool to tighten this connection. Insert the ChromatoProbe cap
into the top of the adapter and hand tighten to cap off the Injector when not
using the ChromatoProbe.
1
2
3
4
ChromatoProbe Kit (03-925677-91)
5
6
8
10
11
9
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
ChromatoProbe Cap (03-925592-01)

Small O-ring, 0.239 (ID 03-930109-11)
Adapter (03-925589-01)
Large O-ring, 0.426 ID (03-930109-12)
Key (03-925690-01)
Guide (03-925582-01)
ChromatoProbe (03-925591-01)
Microvials (100/bottle) (03-925671-11)
Stand (03-925694-01)
Glass insert 03-918464-00
Graphite ferrule (5 mm) (2/pack)
03-925342-02
- Passivation Lacquer (03-925699-01)

- Tweezers (29-899510-00)
- Ferrule (0.4 mm) (10/pack) (28-694580-01)
- Ferrule, 2-hole (0.4 mm) (28-694559-01)
- Column nut (03-949551-00)
Figure 27: ChromatoProbe Assembly
Varian, Inc.
User Manual 450-GC
Page: 199
NOTE: If it appears that there is an alignment problem while inserting the

ChromatoProbe, follow this alternative method for installing the adapter:
1. Connect adapter to the Injector without tightening it.
2. Insert the ChromatoProbe through the adapter with a loose fit and then
tighten the adapter to the Injector while the ChromatoProbe is inserted.
3. Finger tighten to prevent any leaks. DO NOT use a tool to tighten this
connection.
A 2m x 0.10 mm fused silica column with 0.1 m methyl silicone coating is
provided for use with the ChromatoProbe. For a gas chromatograph containing
2 Injectors, it is possible to have the ChromatoProbe and a traditional column
connected simultaneously. In this case, please refer to here on page 202. If
only one Injector exists or the ChromatoProbe is installed alone, please
continue as follows:
1. Remove any column that you have installed in the GC/MS and replace it
with this 2 meter column.
2. Use the 0.4 mm single hole ferrule and the column nut provided in the kit.
3. The column should be inserted a distance of 7.5 cm into the Injector
(standard for 1079 Injectors). The mass spectrometer side is set so that the
column end is 1 mm past the end of the transfer line.
4. Set the head pressure to 10 psi and measure a flow out of the split vent of
50 mL/min. This will provide a flow rate of about 1 mL/min into the mass
spectrometer and a split ratio of about 50:1.
5. Condition the Injector and the column at 300C for 30 minutes. If an EFC is
included, provide 1 mL/min column flow rate with split vent of 50 mL/min.
Using the ChromatoProbe

How to Perform Analysis with the ChromatoProbe
Liquids, solids and slurries, or even samples such as blood, urine, or milk can
be analyzed using the ChromatoProbe.
Place the sample into a microvial provided with the kit. Solid or powder samples
are easier to introduce to the microvial as a liquid solution with a standard
syringe. This way is also cleaner and has smaller memory effects.
Alternatively, powders can be introduced into the microvial with the help of a
Pasteur pipette. The microvial containing the sample is placed into the microvial
holder position at the bottom of the ChromatoProbe shaft. Refer to the exploded
view if this is unclear.
Remove the ChromatoProbe cap from the adapter which should be installed on
top of the Injector and position the ChromatoProbe through the adapter, into the
Injector.
Finger tighten the ChromatoProbe to seal the Injector. The sample is volatilized
by raising the Injector port temperature.
Page: 200
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Varian, Inc.
The column can be hot and isothermal or temperature programmed to match

the Injector. Since most analyses of solid samples do not require high
sensitivity, the split vent should be opened during the entire analysis to only
allow low nanogram amounts into the mass spectrometer.
Adjust the split flow to achieve a fast response, reduce thermal decomposition
and to prevent the mass spectrometer from being overloaded and
contaminated. A good starting value is about 50:1. If the split ratio is too high for
a particular sample, rerun a fresh sample with a lower split ratio to get the
desired sensitivity. In order to prevent overloading of the system, either load the
smallest amount of solid possible or preferably dissolve the solid and load 1 L
of about 0.1% solution. Note Injector comment below.
Samples can be analyzed in any of the mass spectrometer modes of operation
(EI, CI, MS/MS, CI-MS/MS). In general, use AGC target values of 5,000-10,000
to ensure a high spectral quality. A suggested temperature program for the
1079 PTV Injector and column oven is as follows.
INJECTOR:
120C (or 20C above the boiling point of the solvent if

a solution is introduced) for 1 minute, then heat at
40C/min to 300C and hold for 4.5 min.
COLUMN OVEN:
140C for 1 minute, then heat at 40C/min to 300C

and hold for 5 min.
If liquids are to be analyzed, the user must empirically determine certain

parameters to prevent sample from being inadvertently expelled out of the
microvial during analysis, caused by sudden boiling (bumping) or spraying.
These parameters include maximum fill level in the microvials; maximum initial
temperature and heating rates of the Injector.
Analysis of Thermally Labile Samples
Thermally labile samples may decompose in the injection port. The hot metal
surface of the ChromatoProbe can contribute to thermal decomposition
resulting in improper spectra.
In order to eliminate this, Varian has introduced Silcosteel coated
ChromatoProbes.
Varian, Inc.
User Manual 450-GC
Page: 201
Using the ChromatoProbe Along with Traditional GC/MS

For gas chromatographs containing 2 Injectors it is possible to have both the
ChromatoProbe column and a traditional column connected simultaneously.
This can be accomplished by employing a 2-hole ferrule and connecting both
columns into the mass spectrometer. When the ChromatoProbe is not in use,
replace the probe with the ChromatoProbe cap.
Heat the ChromatoProbe Injector to about 300C with the split vent open to
remove any contamination from previous samples. Now, reduce the
ChromatoProbe Injector head pressure to 3-5 psi to minimize the helium flow
into the mass spectrometer. The total flow of helium should remain between 1
and 1.5 mL/min to insure the best sensitivity and spectral quality. Other options
include a Y connector for the 2 columns going into a single transfer line into
the mass spectrometer. Be aware of the possible problems of surface activity
when using this type of connection.
Using the ChromatoProbe as a Dirty Sample Inlet
The ChromatoProbe can be used as an effective tool for chromatographic
analysis of dirty samples, without cleanup or extraction. This use of the
ChromatoProbe is based on intra-Injector thermal extraction of the semivolatile
compounds in the sample microvial, while non-volatile residue is retained in the
microvial, which is disposed of after the analysis. For effective use of the
ChromatoProbe with dirty samples, the following advice should be considered:
1. The sample microvial should be handled with tweezers only. Similarly, the
microvial holder should not be touched with the hands to avoid fingerprints
and dirt being included in the analysis.
2. Introduce into the microvial the smallest sample size that is easy to
quantitatively transfer with a syringe. This is typically 1-3 microliter liquid
samples.
3. Solid samples might be blended or dissolved for a more quantitative
transfer, as well as for more efficient thermal extraction from the microvial.
4. The sample should be introduced at an Injector temperature about 20C
above the solvent boiling temperature, to enable fast but gentle solvent
vaporization without sample splashing from the microvial. This temperature
can be 120C for water (urine) or 90C for acetone blended fruit and
vegetables.
5. The initial column temperature should be low enough to trap the extracted
semivolatile compounds. For example, 50-80C initial column temperature
is desirable for pesticide analyses.
Page: 202
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Varian, Inc.
6. Solvent vaporization takes about one minute for each 3-4 microliter sample.
The split vent can be opened during that time, with a split flow rate above
20 mL/min to speed up the solvent vaporization.
7. After approximately one minute solvent vaporization time, the Injector
temperature should be fast programmed to 250C (for pesticides) or the
appropriate temperature required for the thermal extraction of the
semivolatile compounds. The final temperature chosen is a compromise
between higher temperature for more effective and faster thermal extraction
and a lower temperature value that might be required to prevent thermal
degradation of delicate compounds.
8. During the Injector heatup and thermal desorption time, the split valve must
be closed and the carrier gas flow rate must be at least 4-5 mL/min for
effective thermal extraction. At lower carrier gas flow rates a higher Injector
temperature will be required.
9. The thermal desorption stage takes between 0.5-2 minutes. After that time,
the Injector is cooled down, the carrier gas flow rate is programmed to the
chromatographic optimal value and the GC oven program can begin in the
usual way. Note that the final GC oven upper temperature and time can be
significantly reduced since the less volatile compounds are retained in the
microvial.
10. At the end of the analysis, dispose of the sample microvial. Do not re-use
microvials. The microvial holder should only be removed from the adapter
after both the GC oven and Injector are cool and a helium purge flow from
the ChromatoProbe protects the column.
11. In addition to passivation of the microvial holder, analysis of thermally labile
sample compounds is facilitated with a shorter microvial (up to 6 mm long).
The standard 15 mm long microvials can be cut (like a column) to the
desirable length. Handle the microvial carefully while cutting to avoid
contamination.
12. The microvial volume is 30 microliters. Up to 20 microliters can be loaded
and the solvent evaporated outside the GC prior to sample introduction.
13. Test your method for thermal vaporization efficiency, reproducibility and
long term stability before beginning routine analysis.
Varian, Inc.
User Manual 450-GC
Page: 203
Cleaning
Should the ChromatoProbe become contaminated with time, it can be cleaned
by placing it in a solvent such as acetone and placed in a sonic bath. If it is
severely contaminated a mild abrasive can be used to clean it.
Recommended Reading
1. Aviv Amirav and Shai Dagan, A Direct Sample Introduction Device for Mass
Spectrometry Studies and GC/MS Analysis. European Mass Spectrometry,
3, 105-111 (1997).
2. Hongwu Jing and Aviv Amirav, Pesticide Analysis with the Pulsed Flame
Photometric Detector and a direct sample Introduction Device. Analytical
Chemistry, 69, 1426-1435 (1997).
3. Samuel B. Wainhaus, Shai Dagan, Mark L. Miller and Aviv Amirav, Fast
Drug Analysis in a Single Hair. Submitted for publication.
Page: 204
User Manual 450-GC
Varian, Inc.
1041 On-Column Injector - Injectors
THE 1041 ON-COLUMN INJECTOR
The 1041 On-Column Injector is designed for on-column sample injection onto 530
micron I.D. fused silica columns, 1/4 inch and 1/8 inch O.D. packed columns (glass or
metal).
On-column injection provides complete sample transfer from Injector to column results
in good quantitation.
The fused silica column or glass column extends all the way from the Injector septum to
the detector, providing a clean inert system without cross-overs.
Quick and easy to switch from megabore to packed column or vise versa by changing
an adaptor. The 1041 is supplied with capillary mounting hardware as standard. If you
wish to operate the Injector in the packed column mode then a packed column adapter
kit must be ordered (03-925588-91). This kit contains Injector and detector hardware to
facilitate use of the Injector with 1/8" metal packed columns. In addition, adapter kits are
available for 1/4" columns. Full instructions on converting the 1041 to packed column
use are included with the packed column kit.
The 1041 On-Column Injector is available in manual pneumatics and electronic flow
control (EFC) for different laboratory requirement.
Choose from EFC23 (constant flow control) and EFC24 (constant pressure control and
constant total flow control) for different application requirement.
Varian, Inc.
User Manual 450-GC
Page: 205
Injectors 1041 On-Column Injector

aligned with the injection port of the 1041 universal Injector nut. The GC run is
started when the actuator is depressed by the syringe barrel, or manually
pressed at the moment of sample injection. The GC run can also be manually
(only in local automation) started by pressing START

1041 Injector Insert

Click here to see the 1041 Injector Insert, on page 453.
Note that all 1041 Injector inserts are deactivated for maximum inertness.
Page: 206
User Manual 450-GC
Varian, Inc.
Injector Assembly and Insert

A cross-sectional view of the 1041 On-Column Injector with insert and 530m
ID fused silica capillary column is shown below.
1
3
1.
2.
3.
4
4.
5
6
5.
6.
7.
8.
9.

Septum, 9.5 mm
Injector Body
EFC23 type (392548201)
Injector Body Ferrule
40% Graphite/60% Vespel (up to 400C) (CR213400)
Graphite (up to 450 C) (CR211400)
Injector Body Nut (Stainless Steel, SWSS4021)
Injector Insert (Stainless Steel, 392543101)
Capillary Nut (394955100)
8
9
Figure 28: 1041 On-Column Injector with Insert
Teflon
Vespel
Column ID
Max 250C
0.53 mm ID
CR214108
Max 350C
CR212108
40% Graphite
60% Vespel
Max 400C
CR213108
Graphite
Max
450C
CR211108
SilTite
Metal, GC/MS
SG073302
Table 40: 1041 Column Ferrules 1/16" x 0.8 mm
Varian, Inc.
User Manual 450-GC
Page: 207

The Electronic Flow Control module used on a 1041 Injector can be type
EFC23 or EFC24.
The EFC23 is used to control the 1041 Injector under flow control to program
the column flow. EFC23 sets a required carrier flow into the Injector/Column
system. A leak in the system would be indicated to the user by a drop in inlet
pressure.
The EFC24 is used to control the 1041 Injector in combination with Headspace
sampler and other devices that have a long carrier gas line.
Both EFC types are designed specifically for the 1041 Injector to support its
various modes of operation. In simple terms it duplicates the behavior of the
1041 manual pneumatics system in that there is an inlet mass flow controller
supplying carrier gas to the Injector and a pressure control valve downstream
from the Injector which sets the Injector pressure. As Injector pressure
determines the rate of carrier gas flow through the column, this pressure is
monitored close to the point of injection.
The type EFC23 flow diagram on the next page shown is an indication of the
control mechanism of this type of EFC module.
Page: 208
User Manual 450-GC
Varian, Inc.
*See Pencil Filters on page 437
Varian, Inc.
User Manual 450-GC
Page: 209
The type EFC24 flow diagram shown below is an indication of the control
mechanism of this type of EFC module.
Page: 210
User Manual 450-GC
Varian, Inc.
Column Installation
installation (or reinstallation) of a capillary column in a Varian 450-GC equipped
with a 1041 Injector. Each step of the procedure is described in detail.
on page 23.

The gas flow rates for the 1041 On-Column Injector can be set using manual
pneumatics or Electronic Flow Control (EFC). Note that a positive flow through
the column. The column phase can be irreversibly damaged by exposure to
oxygen at elevated temperatures. Allow 10 15 minutes to purge the column
before heating.
EFC Pneumatics
Type EFC24 used with the 1041 or 1061 Injectors allows the user to set a
column flow. With EFC23 equipped Injectors a flow range of 0 100 mL/min
may be set from the 450-GC keyboard. A pressure program is typically used to
maintain the column flow at a constant value while temperature programming
the column oven. When Constant Flow Programming is enabled, the pressure
program needed to maintain constant flow is derived whenever the method is
loaded. The only user settable parameter with the 1041 type of EFC is the
desired flow rate.
parameters and status are accessed via the FLOW/PRESSURE
key on
The next screen is an example if a type EFC24 is used.

Varian, Inc.
User Manual 450-GC
Page: 211
Flow Rates for Operation

Recommended flow rates differ, depending on the operating mode used. Refer
to the appropriate paragraph for your operational mode.
Capillary Mode
When operating the Injector in the capillary mode, the following carrier gas flow
rates are recommended:
Carrier Gas
Column Flow Rate

(Optimum)
Column Flow Rate

(Typical)
Nitrogen
1.5 mL/min
3 - 15 mL/min
Helium
2.4-4.0 mL/min
4 - 15 mL/min
4.0-8.0 mL/min
8 - 20 mL/min
Hydrogen
Table 41: Carrier Gas Flow Rates for 1041
Packed Mode
When operating in the packed column mode, adjust the carrier gas flow to
applicable packed column flow rates (20 to 50 mL/min), depending on carrier
gas type.
Page: 212
User Manual 450-GC
Varian, Inc.
1041 Operation
This screen contains the specific operating information and procedures required
for optimum performance of the 1041 on-column Injector. All installations for
both the instrument and the Injector must be completed before continuing
further.
1041 Injector Method

The 1041 Injector method component on the 450-GC keyboard contains one
screen for setting the required Injector temperature and viewing the status
information. The 1041 is an isothermal Injector and cannot be temperature
programmed.
Varian, Inc.
User Manual 450-GC
Page: 213
Testing the 1041 Injector

The most effective method of testing Injector performance is by running a test
sample. The following procedure describes how to test the performance of the
1041 on-column Injector. This is best done with a test sample containing an
appropriate set of components for the installed detector. The Table 61, on page
419 lists the series of test samples available for Varian GC detectors.
below. The detector should be operated at its most sensitive range.
Example chromatograms can be found in the detector section on page 419 of
this manual.
Injector temperature
250 C
Column temperature
50 C initial, ramp to 250 C at

20 C / minute and hold for 5
minutes
Injection Volume
1 L
Table 42: 1041 Injector Chromatographic testing conditions
Observe the eluting peaks for symmetry, separation and elution time.
Abnormally wide or skewed peaks, excessive elution times, abnormally small
peaks and noisy or drifting baselines indicate faulty performance.
Page: 214
User Manual 450-GC
Varian, Inc.
Maintenance
Hardware Replacement and Cleaning Procedures
Routine cleaning and maintenance of the 1041 On-Column Injector system
includes septum replacement and column conditioning. Pressure testing and
leak checking procedures are included to assure proper functioning of the
system.
Septum Replacement
Septum replacement represents the major part of routine chromatographic
maintenance. Septum damage from the needle penetrations can be avoided by
injecting into the same hole and not using syringes with needles having burrs or
bends at the tip which cut the septum.
The Injector nut and automatic start switch assembly may be

very hot during instrument operation and should not be
touched with unprotected hands. Allow sufficient time for the
Injector nut and surrounding assemblies to cool before
continuing with this procedure.
Handling a septum with bare fingers may result in column
contamination. Use tweezers, finger cots, or gloves when installing a
new septum.
1. Be sure the Injector nut is cool. Unscrew the Injector nut (use the Injector
Nut wrench) and place on a clean, uncontaminated surface.
2. Using tweezers, remove the septum, taking care not to scratch the internal
surfaces of the Injector.
3. Using tweezers, place a new high temperature septum in the Injector. If the
septum is TFE or FEP coated put that side down.
4. Replace the Injector nut and tighten until resistance is felt, then tighten an
extra 1/2 to full turn.
Varian, Inc.
User Manual 450-GC
Page: 215
Needle/ Syringe Cleaning

For normal use, rinse the needle/syringe by slowly drawing up and quickly
expelling solvent or the next sample to be used. Repeat the process several
times.
When rinsing with the next sample, DO NOT expel sample back into the
sample container
Leak Checking
Leak checking methods used with the 1041 On-Column Injector are presented
in order of overall sensitivity and performance. When leak checking the Injector
only, be sure to use the appropriate procedure.
1. Remove the test column and plug the Injector outlet with a 1/16" no-hole
ferrule (P/N 28-694590-01). Remove the Injector nut, install a new septum,
then replace Injector nut and turn nut clockwise until it comes to a stop.
2. Pressurize the Injector to 400 kPa (60 psig) with carrier gas. Turn off the
carrier gas flow at the supply.
3. A pressure drop less than or equal to 3 kPa (0.5 psig) in 15 minutes is
acceptable. Locate leaks with an appropriate leak detector.
Any changes in temperature while performing this test may result in
false readings due to expansion/contraction of the gas with
temperature.
Commercial soap type leak detection fluids should not be used at any
point in a capillary system, since, if a leak is present, the fluid will
penetrate and contaminate the system. Column performance will be
degraded and a substantial period of time may be required to achieve a
clean system.
4. An alternate way to leak check the Injector only is to have the column
installed in the Injector end and the opposite column end sealed with a
flame or appropriate fitting.
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Syringe Leak Checking

In some instances, non-reproducible chromatographic responses can be
attributed to a worn and/or leaky syringe. The syringe must be leak tight. To
check the syringe, insert the needle in an Injector operating at 150-200 kPa (20
to 30 psig) with a no-hole ferrule. Place a drop of solvent at suspect leak
locations and look for bubbles.
clean system.
Varian, Inc.
User Manual 450-GC
Page: 217
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Varian, Inc.
1061 Flash Vaporization Injector - Injectors
THE 1061 FLASH VAPORIZATION INJECTOR
The 1061 flash vaporization Injector is designed for use with wide-bore columns
of 0.53 mm ID.
Used with packed glass liner with vaporization volume for dirty samples.
Glass liner is removable from the top. No need to disconnect the column.
The 1061 Injector can operate in 2 modes: the capillary column mode or the packed
column mode.
Switching from one mode to another involves changing the Injector and detector column
mounting hardware.
The 1061 is supplied with capillary mounting hardware as standard.
If you wish to operate the Injector in the packed column mode then a packed column
adapter kit must be ordered (03-925588-92). This kit contains Injector and detector
hardware to facilitate use of the Injector with 1/8 metal packed columns.
Complete instructions are provided in this kit for installing and operating the Injector in
the packed column mode.
Varian, Inc.
User Manual 450-GC
Page: 219
Injectors 1061 Flash Vaporization Injector

aligned with the injection port of the 1061 Injector nut. The GC run is started
automation) started by pressing START

Page: 220
User Manual 450-GC
Varian, Inc.

The 1061 Flash Injector with insert and 530m ID capillary column
1
1
2
3
4
5
6
7
8
9
10

Septum, 9.5 mm
BTO (lowest bleed, CR298705 )
Glass Insert, default 392611943 More liners
Injector Body, EFC23 (392548301)
Column Guide (392558301)
Ferrule,
40% Graphite/60% Vespel (up to 400C) (CR213400)
Graphite (up to 450 C) (CR211400)
Injector body Nut (SWSS4021)
Bottom Nut (394955100)
6
7
8
9
10
Figure 31: 1061 Flash Vaporization Injector with Insert
Teflon
Vespel
Max 250C
Max 350C
Column ID
0.53 mm ID
CR214108
CR212108
40% Graphite
60% Vespel
Max 400C
CR213108
Graphite
Max
450C
CR211108
SilTite
Metal, GC/MS
SG073302
Table 43: 1061 Column Ferrules 1/16" x 0.8 mm
Varian, Inc.
User Manual 450-GC
Page: 221

The Electronic Flow Control module used on a 1061 Flash Injector can be type
EFC23 or EFC24. The EFC23 is used to control the 1061 Injector under flow
control to program the column flow. A leak in the system would be indicated to
the user by a drop in inlet pressure. The EFC24 is used to control the 1061
Injector in combination with Headspace Sampler or other devices that have a
large carrier gas line.
monitored close to the point of injection. The type EFC23 flow diagram shown
below is an indication of the control mechanism of this type of EFC module.

Page: 222
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Varian, Inc.
Varian, Inc.
User Manual 450-GC
Page: 223
1061 Injector Insert

Click here to see the 1061 Injector Insert, on page 453.
All 1061 Injector inserts are deactivated for maximum inertness.
The 1061 Injector contains a glass insert with a tapered section on the bottom.
This allows a wide bore capillary column seal with the insert. The sample is
vaporized in the insert and then swept onto the column. The use of glass wool
in the insert allows the analysis of samples containing non-volatile components.
The non-volatile material is trapped on the glass wool while the volatile
components vaporize onto the column. The packed column kit for the 1061 also
contains a glass insert, in this case the packed column buts up against the
bottom of the insert.
Column Installation
The following instructions apply to installing a 0.53 mm ID capillary column in
the 1061 Injector. Note that the thin polymeric coating on fused silica columns
will give some protection against breakage; however, fused silica columns are
somewhat fragile and must be handled with care. Alternative is to use UltiMetal
0.53 mm wide-bore columns.
Column Installation
installation of a capillary column in a Varian 450-GC equipped with a 1061
Flash Injector. Each step of the procedure is described in detail.
on page 23.
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The gas flow rates for the 1061 Flash Injector can be set using manual
pneumatics or Electronic Flow Control (EFC). Note that a positive flow through
the column. The column (stationary) phase can be irreversibly damaged by
exposure to oxygen at elevated temperatures. Allow 10 15 minutes to purge
the column before heating.
EFC Pneumatics
Type EFC24 used with the 1061 Injector allows the user to set a constant
column head pressure, build a pressure program, or emulate a constant column
flow when the column is temperature programmed. With EFC23 equipped
Injectors a flow range of 0 100 mL/min may be set from the 450-GC
keyboard. A pressure program is typically used to maintain the column flow at a
constant value while temperature programming the column oven. When
Constant Flow Programming is enabled, the pressure program needed to
maintain constant flow is derived whenever the method is loaded.
parameters and status are accessed via the FLOW/PRESSURE
key on
The next screen is an example if a type EFC24 method.
Varian, Inc.
User Manual 450-GC
Page: 225
Flow Rates for Operation

Recommended flow rates differ, depending on the operating mode used. Refer
to the appropriate paragraph for your operational mode.
Capillary Mode
When operating the Injector in the capillary mode, the following carrier gas flow
rates are recommended:
Carrier Gas
Column Flow Rate

(Optimum)
Column Flow Rate

(Typical)
Nitrogen
1.5 mL/min
3 - 15 mL/min
Helium
2.4-4.0 mL/min
4 - 15 mL/min
4.0-8.0 mL/min
8 - 20 mL/min
Hydrogen
Table 44: Carrier Gas Flow Rates for 1061 Flash Injector
Adjust the make-up gas flow to give a total of 30 mL/min.

Packed Mode
When operating in the packed column mode, adjust the carrier gas flow to
applicable packed column flow rates (20 to 50 mL/min).
Page: 226
User Manual 450-GC
Varian, Inc.
1061 Flash Injector Operation

This section contains the specific operating information and procedures
required for optimum performance of the 1061 flash Injector. All installations for
both the instrument and the Injector must be completed before continuing
further.
1061 Flash Injector Method

screen for setting the required temperature for the Injector and viewing the
status information. The 1061 Flash Injector is an isothermal Injector. The
temperature of the 1061 Flash Injector must be optimized in order to have good
sample evaporation in the liner.
Varian, Inc.
User Manual 450-GC
Page: 227
Testing the 1061 Flash Injector

The most effective method of testing Injector performance is by running a test
sample. The following procedure describes how to test the performance of the
1061 flash vaporization Injector. This is best done with a test sample containing
an appropriate set of components for the installed detector. The Table 61, on
page 419 lists the series of test samples available for Varian GC detectors.
below. The detector should be operated at its most sensitive range.
Example chromatograms can be found in the detector section on page 419 of
this manual.
250 C
Column temperature
50 C initial, ramp to 250 C at

20 C/minute and hold for 5 minutes.
Injection Volume
1 L
Table 45: 1061 Flash Injector Chromatographic Testing Conditions
Observe the eluting peaks for symmetry, separation and elution time.
Abnormally wide or skewed peaks, excessive elution times, abnormally small
Page: 228
User Manual 450-GC
Varian, Inc.
MAINTENANCE
The 1061 is mechanically similar to the 1041 except that it uses a glass insert
for flash vaporization injection. Follow the same maintenance procedures for
the 1061 that are outlined above for the 1041, except in the case of changing or
cleaning glass inserts.
Replacing the 1061 Glass Insert

After prolonged use, the 1061 glass insert may need to be removed for
replaced with a new insert. Note that there are 2 different glass inserts, one for
use with wide bore (0.53 mm ID) capillary columns and one for use with packed
columns. These inserts are not interchangeable.
Wide bore glass insert, Part Number: 03-926119-43.
Packed column glass insert, Part Number: 03-926119-44.
See also #Injector_Parts_1061 on page 453.

Follow these steps to remove the glass insert from the 1061 Injector.
1. Use the Injector nut wrench to remove the
Injector nut. Place the nut on a clean surface
(e.g., clean tissue).
The Injector nut may be hot. Lower the Injector temperature

to 50 C and permit the Injector nut to cool before
proceeding.
Varian, Inc.
User Manual 450-GC
Page: 229
CP-8400 AutoSampler, remove the Injector access plate by removing

the 2 retaining screws and firmly lifting the plate. It may be hot if
another Injector is also installed and powered. The plate may be a little
tight, do not force it off. Lift straight up, a slight back and forth rocking
may help remove it.
2. With tweezers or a septum pick, lift the edge of
the septum. Remove the septum.
Replace the Injector septum each time the

glass insert is replace.
3. Use tweezers or a septum pick to grasp the
glass insert and remove it from the Injector.

Follow these steps to replace the glass insert in the 1061 Injector.
1. Pick up the new insert with tweezers and place it in the Injector carefully.
2. Use tweezers to place a new septum in the Injector.
If the septum has a Teflon face, place the Teflon face toward (down) the
column.
3. Place the Injector nut on the Injector and tighten by hand until you feel
some resistance, then tighten an extra 1/2 to full turn using the Injector nut
wrench.
After the Injector nut has been replaced check the head pressure (EFC
status on display or manual pressure gauge on pneumatics panel)
increases to its normal value. If this does not happen there is an
indication of a leak.
4. Condition the insert by setting the 1061 Injector temperature to 300C and
allowing the system to condition for 30 minutes.
Page: 230
User Manual 450-GC
Varian, Inc.
1093 Septum-Equipped Programmable Injector (SPI) - Injectors
1093 SEPTUM-EQUIPPED PROGRAMMABLE INJECTOR (SPI)
The Varian 1093 Injector gives optimum performance for non-vaporizing (cold)
injection into conventional fused silica capillary columns (0.32-0.53 mm ID
columns).
It incorporates several unique design features to produce improved peak
resolution, quantitation and versatility over other cold on-column Injectors.
The result is not only a capillary on-column injection system ideally suited for
analyses that cannot be done with conventional split/splitless injection, but one
that gives highly accurate and precise results with a wide variety of trace to
semi-trace level samples.
The 1093 Injector can replace manually operated vaporizing capillary Injectors
in many cases and may provide improved quantitation of labile and high
molecular weight samples.
Temperature-programmed, cold injection: The Injector is held at a temperature
20 C to 30 C below the solvent boiling point during injection and then is
rapidly temperature programmed up to the final column temperature.
The oven is started at the same temperature as the Injector. Conventional
temperature programmed analysis is carried out in the GC column.
Varian, Inc.
User Manual 450-GC
Page: 231
Injectors 1093 Septum-Equipped Programmable Injector (SPI)
Frequently, good results may be obtained and the run time may be reduced by
injecting into a cold Injector but with the column at 5C above the solvent boiling
point. In this case, the column is held at the initial temperature until the Injector
is at its final temperature.
Cold injection reduces or eliminates many of the problems of conventional
vaporizing split/splitless injection, such as molecular weight discrimination (loss
of high and low boiling substances), thermal decomposition of the sample and
sample adsorption onto hot, active Injector surfaces. These problems are
largely eliminated in cold injection because the sample is directly introduced
into the column as a liquid. In the split/splitless Injector, the sample is first
vaporized and then allowed to pass into the column, where it may be
condensed back into its liquid state.
The 1093 Injector may also be used as an isothermal, vaporizing Injector.
However, best performance is achieved using the temperature-programmed
mode. The system consists of three major components: a glass insert, the
heated Injector body and a standard syringe. Maximum syringe needle
diameter is 0.019" (0.49 mm) or 26 gauge.
All heated parts and all parts in direct contact with the carrier gas stream are
constructed of stainless steel, borosilicate glass, fused silica, silicone rubber
(septum) and Inconel X750.
The Injector body is mounted on an insulated enclosure. The Injector heating
rate is adjustable to allow optimization for thermally sensitive samples. A purge
exit is provided for bake-out and septum purge. The internal dead volume of the
Injector body has been minimized.
In operation, the fused silica column is inserted up into the Injector body from
the column oven and seated in the glass insert. The column is sealed to the
Injector with conventional polyimide/graphite or graphite ferrules. The syringe
needle enters the glass insert from the top. After the syringe is withdrawn, the
entire injection zone is rapidly heated, driving the sample into the column where
the peaks are sharpened by the solvent effect and cold trapping. Significant
peak broadening occurs (up to 2X) in Injectors without this rapid heating step,
especially when larger samples and high-boiling samples are used.
Of the 2 internal parts in the Injector body, the septum support and glass insert
require periodic removal for cleaning. A biweekly check is recommended during
regular use. The need for cleaning will vary with different samples and the glass
insert is easily replaced in case of non-removable deposits or breakage.
The 1093 Septum-Equipped Programmable Injector (SPI) is factory-installed or
available as a field upgrade (must be installed by trained personnel).
Page: 232
User Manual 450-GC
Varian, Inc.

aligned with the injection port of the 1061 Injector nut. The GC run is started
automation) started by pressing START
The Injector nut and automatic start switch assembly

may be very hot during instrument operation and
should not be touched with unprotected hands.
Varian, Inc.
User Manual 450-GC
Page: 233

The 1093 Septum-Equipped Programmable Injector (SPI).
1
3
4
5
6
7
8
1. Injector Nut, (3949666601)

Injector Nut Wrench, (390842300)
2. Automatic Start Switch (390820601)
3. Septum, 7/16
BTO CenterGuide, (CR298717 )
Advanced Green 3 CenterGuide , CR246225)
4. Septum Support, (391821100)
5. Glass Insert, default SG092034 More liners
High performance (190010906)
On-Column (190010907)
Packed (392611950)
6. Wave spring washer 2x, (1492000501)
7. Coolant exit, Frit Restrictor (3600004601)
Plug, 1/8 tube (2824707101)
8. Screws 3x, (391866306)
9. Injector Body
10. Ferrule,
40% Graphite/60% Vespel (up to 400C), CR213400
Graphite (up to 450 C), CR211400
11. Bottom Nut brass (394955100)
Stainless Steel (CP743117)
12. Heater/probe 120 Vac, (391833400)
230 Vac, (391833401)
10
11
12
Figure 34: 1093 Injector Assembly
1093 Injector Parts

Click here to see the 1093 Injector parts on page 454.
Page: 234
User Manual 450-GC
Varian, Inc.

EFC23 or EFC24. The EFC23 is used to control the 1093 Injector under flow
control to program the column flow. A leak in the system would be indicated to
the user by a drop in inlet pressure. The EFC24 is used to control the 1093
Injector in combination with Headspace Sampler or other devices that have a
large carrier gas line.
monitored close to the point of injection. The type EFC23 flow diagram shown
below is an indication of the control mechanism of this type of EFC module.

Varian, Inc.
User Manual 450-GC
Page: 235
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User Manual 450-GC
Varian, Inc.
Glass Insert
Different glass inserts are available for use in the 1093 Injector.
Click here to see all inserts of the 1093 Injector parts on page 454
The standard insert is the high performance (P/N 190010906).
The high-performance insert (P/N: 190010906) is used when the presence of

glass wool is unacceptable. The small internal diameter of this insert provides
efficient transfer of the liquid sample from the syringe. If inserts with larger
internal diameters are used without any packing, then sample transfer from the
syringe may not be quantitative.
The on-column insert (P/N: 190010907) is used for on-column injection into
large bore (0.53 mm ID) columns.
The glass wool packed insert (P/N: 392611950) provides efficient transfer of the
liquid sample from the syringe and traps any contaminants present in the
sample.
Syringe
The required syringe needle length is 2.00" (excluding the hub) for both manual
injections and used in the CP-8400 and 8410 AutoSamplers.
Varian, Inc.
User Manual 450-GC
Page: 237
Mounting the Column

During operation, the fused silica capillary column hangs on the capillary
column holder in the column oven.
Hang the coiled column on the capillary column holder, then prepare the
column end and complete column connections to both the Injector and detector
fittings, as detailed in the following paragraphs.
Column Installation
installation (or reinstallation) of a capillary column in a Varian 450-GC equipped
with a Varian 1093 Injector. Each step of the procedure is described in detail.

on page 23.

Connecting CO2 to the 1093 Injector

The recommended tank for use with the 1093 Injector is a size 1A cylinder
containing approximately 60 pounds of bone dry liquid CO2. The tank should
be equipped with a liquid eductor tube. Special fittings provided in the Start-Up
Kit (P/N 03-918335-90) for the Injector are required for connection to the CO2
tank. Refer to figure below.
To CO2 tank
Teflon
washer
CGA320
Fitting
In-Line Filter
Hex Head
Reducer
Swagelok
Fitting
To CO2 Solenoid
Valve
Figure 37: Connection CO2 tank to GC
Page: 238
User Manual 450-GC
Varian, Inc.
Approximately 100 chromatographic runs can be made per tank of CO2 when
the Injector is cooled to -50C for each run. Cooling to higher temperatures will
consume less coolant per run. The rate of use of CO2 is dependent on the
operational conditions, thus your actual use may vary from this estimate.
1. Use 1/8" copper or stainless steel tubing for the connection between the
CO2 solenoid valve and the CO2 tank. NOTE: If stainless steel tubing is
used, change all fittings to stainless steel.
2. Connect one end of the 1/8" Swagelok fitting to the GC and the other end of
the tubing to the in-line filter and CGA 320 adapter. All hardware is supplied
in the Start-Up Kit.
3. The CGA 320 fitting will be connected to the CO2 tank. A Teflon washer is
fitted in the nut that will connect to the tank and it must be inspected. Check
that the washer is in good condition. If it is not, replace that washer and
then connect the CGA 320 fitting to the tank. NOTE: Do not over tighten
the CGA 320 fitting. A high torque is not required, as the Teflon
washer is the seal.
Connecting LN2 to the 1093 Injector

When connecting LN2 to the 1093 Injector, Neoprene insulation tubing (P/N 24000467-00) must be installed over the entire length of tubing from the solenoid
valve to the tank, to prevent ice build up and condensation. Consumption of LN2
is approximately 0.5 to 1.0 pounds per run when the Injector is cooled to -50C
for each run. Cooling to higher temperatures will consume less coolant per run.
The rate of use of LN2 is dependent on the operational conditions, thus your
actual use may vary from this estimate.
Full tank pressure is directed to the GC and the tank regulator should
be less than 50 psi for stable operation.
LN2 tanks that are designed for pressures higher than 50 psi must not
be used with in-line regulators, shut-offs, or restrictors due to high
pressure build-up. In all cases, never limit the tank's built-in venting
system.
Compressed air at 40 psig may be used to cool the Injector using the
LN2 option; however, it is not recommended due to the low efficiency of
cooling with air. If operation above 50C is acceptable, then air may give
satisfactory cooling rates.
Varian, Inc.
User Manual 450-GC
Page: 239

The gas flow rates for the 1093 Injector can be set using manual pneumatics or
Electronic Flow Control. Note that a positive flow through the column must be
set before heating the column.
Do not heat the column oven above 50 C without carrier gas flowing
through the column. The column phase can be irreversibly damaged.
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Varian, Inc.
EFC Pneumatics
EFC23 or EFC24.
The EFC23 is used to control the 1093 Injector under flow control to program
the column flow. EFC23 sets a required carrier flow into the Injector/Column
system. A leak in the system would be indicated to the user by a drop in inlet
pressure.
The EFC24 is used to control the 1093 Injector in combination with Headspace
sampler and other devices that have a long carrier gas line.
monitored close to the point of injection.
Type EFC23 or EFC24 used with the 1093 Injector allows the user to set a
column flow. A pressure program is typically used to maintain the column flow
at a constant value while temperature programming the column oven. When
Constant Flow Programming is enabled, the pressure program needed to
maintain constant flow is derived whenever the method is loaded.
parameters and status are accessible via the FLOW/PRESSURE
key on
The next screen is an example if a type EFC24 used.
Varian, Inc.
User Manual 450-GC
Page: 241
1093 Injector Operation

This screen contains the specific operating information and procedures required
for optimum performance of the 1093 Injector. All installations for both the
instrument and the Injector must be completed before continuing further.
screen for setting the required temperature, Injection rate and hold time can be
time programmed for the Injector.
Page: 242
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Varian, Inc.
Testing the 1093 Injector Performance

Injector. This is best done with a test sample containing an appropriate set of
components for the installed detector. The following table lists the series of test
samples available for 450-GC.
Test Sample
Part Number
TCD
82-005048-01
ECD
82-005048-02
PFPD
82-005048-03
20.0 ng/L of n-dodecanethiol, tributylphosphate,

methyl parathion; 4000 ng/L of n-pentadecane in
iso-octane.
TSD
82-005048-04
2.00 ng/L of azobenzene, methyl parathion; 4.00

ng/L malathion and 4.00 g/L C17 in iso-octane.
FID
82-005048-07
diluted 100:1.
previously for the injection technique you are currently using. The detector
should be operated at the most sensitive range, e.g., 12 for FID and TSD, 0.05
for TCD, 10 for PFPD and 1 for ECD. The resultant chromatogram on page 419
should approximate that shown in the detector section of this manual.
Observe the eluting peaks for symmetry, separation and retention time.
Abnormally wide or skewed peaks, excessive retention times, abnormally small
When the instrument is installed a definitive indication of instrument
performance can be obtained by running a test chromatogram for the
detector(s) that will be used with the Injector. This initial test chromatogram
should be retained as a standard of comparison for later checking the
instrument if change in detector sensitivity is suspected.
Varian, Inc.
User Manual 450-GC
Page: 243

for the Model 1093 Injector and is controlled
by a manual needle valve. This is located
behind the front cover of the GC.
calibration when columns of different length
and diameter are installed.
With type EFC23/24, the septum purge calibration routine should be carried out
when the instrument is first set up or a new column is installed or when a
significantly different pressure point is chosen. Press the SETUP
click on Calibration.
key and
middle or rear).
Typical 3-5 mL/min

Press OK.
Page: 244
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Varian, Inc.
Maintenance
Before maintaining the 1093 Injector please read the common
Injector/septum maintenance information in the section Maintenance,
on page 432.
Septum Replacement
Septum replacement represents the major part of routine chromatographic
maintenance. Septum damage from the needle penetrations can be avoided by
injecting into the same hole and not using syringes with needles having burrs or
bends at the tip which cut the septum.
Handling a septum with bare fingers may result in column
contamination. Use tweezers when installing a new septum.
Follow steps 1 through 7 below for replacing the septum in the Injector. Be sure
to cool all heated zones to less than 80C before opening the septum nut and
decrease the column head pressure to less than 2 psig. If pressure is too high,
the septum support and glass insert may pop up, rather than remain in their
correct positions.
Removal of Glass Insert
Use care when removing or replacing the glass inserts for the 1093 Injector.
The Injector nut may be hot. Lower the Injector temperature
to 50 C and permit the Injector nut to cool before
proceeding.
Removal
To avoid contaminating the capillary system, ALWAYS use
tweezers or the extraction tool to handle the Injector
internal parts.
1. Use the Injector nut wrench to remove the Injector
nut and place on a clean, uncontaminated surface,
such as a fresh cleaning tissue.
Varian, Inc.
User Manual 450-GC
Page: 245
2. Remove the Injector

switch and the 2 wave
spring washers.
3. Using tweezers or the
extraction tool (P/N:
7200008400) supplied in the Accessory Kit, remove
the septum, septum support and glass insert. Place
these parts on a clean, uncontaminated surface.
4. If the glass insert does not pop up when the
septum support is removed, it may be
necessary to push up on the column from the
column oven. The polyimide on polymer-coated
fused silica columns often forms a very tight
seal to the glass insert. This seal must be
broken before the insert can be removed.
Re-assemble
Install a new glass insert by following steps 5 through 8.
To avoid contaminating the capillary system, ALWAYS use tweezers or
the extraction tool to handle the Injector internal parts.
5. Place the insert into the Injector body.
6. Install the septum support over the insert. The
line on the septum support must not be visible!
7. Using tweezers, place a new high temperature
septum over the septum support. If a Tefloncoated septum is used, the Teflon side must
face down.
8. Place the Injector switch and the 2 wave spring washers and nut on the
Injector and tighten until resistance is felt, then tighten an extra 1/4-turn.
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Varian, Inc.
Leak Checking
Leak checking methods used to leak check the 1093 Injector are
presented in order of overall sensitivity and preference.
Leak Checking the Injector Only
1. Remove the (test) column and plug the Injector outlet with a 1/16" no-hole
ferrule (P/N: 28-649503-00). Turn Injector nut clockwise until it comes to a
stop. Turn off the septum purge.
2. Pressurize the Injector to 30 psig with carrier gas. Turn off the carrier gas
flow at the ON-OFF valve.
3. The pressure should hold for 30 minutes, as shown on the status screen. A
pressure drop less than or equal to 1 psig per minute at 30 psig is
acceptable. Locate leaks with an appropriate leak detector.
clean system.
4.
An alternate way to leak check the Injector only is to have the column
installed in the Injector end and the opposite column end sealed.
Gas Leak Checking

A convenient and non-contaminating way to leak test fittings and connections
after installation or hardware replacement procedures is to direct a small jet of
gas (butane from a disposable lighter is recommended) at the point to be
tested, then use the detector, at maximum sensitivity, to detect leakage of gas
into the system. Use normal column flow, a cool oven and an operational
detector. If a peak is detected in excess of the magnitude given in table below,
repair the leak.
Butane
Attenuation,
Range
16 x10-12
Maximum
Peak Size
30%
Dichloromethane
2x1
50%
Detector
Gas
FID
ECD
PFPD, Sulfur Mode
TSD
Natural gas containing Methanethiol

Dichloromethane
2 x 10
-10
50%
2 x 10
-12
2%
Table 47: Detectable Gas Leak Checking
Varian, Inc.
User Manual 450-GC
Page: 247
Visual Leak Checking

The least preferred method of leak checking is to place a drop of pure solvent
(isopropyl alcohol is recommended) on the suspected fitting or connection and
look for bubbles.
clean system.
Syringe Leak Checking
In some instances, non-reproducible chromatographic responses can be
attributed to a worn and/or leaky syringe. The syringe must be leak tight. To
check the syringe, insert the needle in an Injector operating at 20 to 30 psi
(150-200 kPa) with a no-hole ferrule. Place a drop of solvent at suspect leak
locations and look for bubbles while moving the syringe plunger up and down.
Injector and Column Conditioning

Initial bake out of a factory-installed Injector or test column is not necessary. If
bake out becomes necessary due to contamination from handling, etc., follow
the procedures or recommendations in the following paragraphs.
Baking Out the Injector
It may be necessary to bake out the Injector if it has become contaminated
during the re-assembly process, i.e. if the internal parts were placed on dirty
surfaces or touched with bare hands. Then, both the Injector and column
should be conditioned.
To prevent contamination and overheating of the fused silica column, the
column must NOT be connected to the Injector during the Injector bakeout procedure.
1. Disconnect column from Injector.
2. Fully open the septum purge.
3. Install a no-hole ferrule in the capillary column nut. Thread the nut up onto
the assembly and tighten.
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Varian, Inc.
4. Set flow between 100 and 200 mL/min. Measure flow at the purge line exit,
then remove the no-hole ferrule from the column nut.
5. Set the Injector temperature to 450C.
6. Bake out the Injector for not less than 4 hours, to a maximum of 16 hours at
a time.
7. Cool the Injector to 50C and then install the capillary column, on page 15.
8. Replace the septum.
9. Readjust the septum purge to the desired flow rate.
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User Manual 450-GC
Page: 249
Page: 250
User Manual 450-GC
Varian, Inc.
Sample PreConcentration Trap (SPT) - Injectors
SAMPLE PRECONCENTRATION TRAP (SPT)
Description
The SPT is a concentrating system for the determination of trace level volatile
organic components in air and gaseous matrices. Integrated into the top of the
GC, its design provides the following features:
Fast heating rates.

Very low cryogenic consumption.
Short and long trap length options.
Liquid carbon dioxide (LCO2), liquid nitrogen (LN2) cryogenic cooling.
Trap heating rates of up to 40 C/sec provide fast injection from the trap to the
capillary column. This helps to ensure good chromatographic performance
without the need of an isolation valve, even for low boiling analytes.
Fast injection also allows higher initial column oven temperatures, thereby
reducing or eliminating the need for column oven cryogenics. Cryogenic usage
for trap cooling is minimized because of the compact design of the SPT and the
specially designed algorithm that controls the cooldown and temperature of the
SPT.
Varian, Inc.
User Manual 450-GC
Page: 251
Injectors Sample PreConcentration Trap (SPT)
SPT temperature zone

The SPT temperature zone is independently controlled by a heated zone of the
450-GC for setting the trapping temperature and up to 2 desorption programs.
Because of the traps fast heating rates, there is no rate parameter setting for
the desorption programs.
.
Each SPT option includes a SPT valve oven, installed either for operation with
2 gas switching valves or with one valve and one Injector. The SPT valve oven
is controlled by the 450-GC heated zone and provides a constant temperature
environment for the trap ends and tubing connecting them to an SPT valve.
The SPT is assigned to heated zone 3 only.
The multi-valve oven may be installed on the 450-GC for SPT systems which
require more than 2 valves.
See building an SPT method on page 263 for more details.
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User Manual 450-GC
Varian, Inc.
Two trap sizes available

Two trap sizes and various packing materials are available:
The short trap is generally used for cryogenic trapping on glass beads
using LN2 or for highly adsorbing trap materials.
The long trap length is suitable for trapping with adsorbents such as
Tenax or charcoal-based materials at ambient or near ambient trapping
temperatures where LCO2 cryogen may be used.
The following are nominal measurements for the 2 trap sizes:

Trap Size
Short
Long
Active Bed Length

6.8 cm
29.2 cm
Total Length
17.02 cm
39.47 cm
Using the SPT

Trapping Methodology
There are fundamentally 2 methods of preconcentrating volatile organics:
cryogenic trapping and adsorbent trapping. Cryogenic trapping takes place on
an inert material, such as glass beads, at a very low temperature. For example,
hazardous air pollutants with boiling points down to -30C can be
preconcentrated on glass beads at -160C using LN2.
The other trapping method uses adsorbents, such as Tenax, charcoal or other
carbon-based materials, porous polymers, or coated column packings, alone or
in various combinations at near ambient trapping temperatures. For example,
the same pollutants mentioned above can be trapped on a Tenax/Charcoal,
Carbopack B, or Vocarb 4000 (Supelco) packed trap at ambient temperatures.
Trapping Media
Several trapping media were mentioned above. In general, the least active
medium that will still provide adequate capacity (retention volume) for the
components should be used. This will keep the desorption temperature at a
minimum and allow faster release of the analytes from the trap to the column.
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User Manual 450-GC
Page: 253
Trap Dimensions
Once the trapping material is chosen, the trap size (long or short) should be
selected based on the volume of the sample to be passed through it and the
trapping temperature (all SPT traps are made from 1/8 o.d., type 316 stainless
steel tubing). Most traps should be able to accommodate samples of
approximately 400 milliliters at flow rates of about 40 mL/min in order to obtain
the detection levels required.
Trap Temperature
The temperatures required for cryogenic trapping on glass beads are easy to
determine. As noted above, a trap temperature of -160C has been used for air
toxics. When preconcentrating even lower boiling analytes, such as the
C2-hydrocarbons, trap temperatures as low as -180C are necessary. When
using adsorbents, the trapping temperature is determined by the breakthrough
volume of the sample. Lower activity adsorbents require lower temperatures.
Trapping and Desorption
The flow rate during trapping is generally from 10 to 40 mL/min. Trapping is
always more efficient at lower flow rates. Flow rate during desorption depends
on the analytical system to which the analytes are passed. Desorption flow
rates of 5 mL/min or greater are compatible with 0.53 mm i.d. columns and
usually produce narrow peaks for early eluting components. When the capillary
column i.d. does not allow this high flow, fast desorption flow rates in
combination with inlet splitters may be used.
To improve peak shape and quantitation in cases where narrow bore column
systems are in use but detectivity requirements prohibit the use of split inlet
systems, column oven cryogenics will be required. This allows refocussing of
early eluting components.
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Varian, Inc.
Electrical System
The SPT option provides independent temperature control of 2 parts of the trap
assembly:
1. Heating and cooling of the trap.
2. Heating of the trap ends.
Trap temperature programming is accomplished in 450-GC heated zone 3,
controlling heating and cryogen cooling of the trap. The SPT trap is mounted on
the SPT valve oven, which maintains the SPT trap ends at a constant
temperature. The oven is powered by one of the other remaining heated zones.
Extremely fast heating of the trap is made possible by utilizing the wall of the
trap tubing as an electrical heating element. This eliminates the extraneous
thermal mass associated with conventional heater cartridges. To match the
electrical resistance characteristics of the trap tubing, a specific electrical
voltage and current are provided by the SPT transformer (mounted in the rear
of the GC). To provide the required voltages, the SPT trap harness connectors
for the short and long trap are different. Although low voltages (less than 8 volts
AC) are used to heat the trap, the SPT transformer is designed to deliver very
high currents.
The trap ends carry dangerous currents. Do not put any conducting
material, such as wrenches, screwdrivers, or metal tubing, across the trap
ends. Do not wear metallic jewelry while working near the trap.
Variations in line voltage supplied to the GC will have an effect on the
heating rate while the trap is desorbing.
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User Manual 450-GC
Page: 255
Circuit breaker
The circuit breaker reset button is located above the SPT transformer on the
rear panel of the GC. This pop-out button protects the SPT from abnormal
power usage by interrupting the electrical connection to the trap. Wait at least 5
minutes after the circuit breaker is tripped before resetting it.
Figure 38: SPT Electrical Diagram
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User Manual 450-GC
Varian, Inc.
LCO2 Option
System Description
The SPT-LCO2 option allows trapping temperatures as low as -60C. This
system is very efficient and consumes a minimum amount of LCO2.
Because of low coolant consumption, conditions that affect thermal efficiency of
the coolant transfer system are very important to consider.
Figure 39: LCO2 Coolant Flow Diagram
Varian, Inc.
User Manual 450-GC
Page: 257
Theory of Operation
As LCO2 expands into the gas phase in the SPT cryo Enclosure, the latent heat
of vaporization provides cooling power. The coolant flow rate is regulated by
varying the pulse rate of the cryo solenoid valve.
The latent heat of vaporization drops rapidly as the temperature increases to
the CO2 critical point of 31C. In order for the SPT to have adequate cooling
power, LCO2 should be delivered to the cryo valve at 27C or cooler.
Characteristics of LCO2 as a Coolant
The coolant for this option is liquid phase carbon dioxide (LCO2) supplied from
a pressurized cylinder a. At pressure, this cylinder contains both liquid and gas
phases coexisting at equilibrium. The cylinder pressure is then equal to the
saturation pressure and is dependent on the supply temperature. As the
cylinder temperature rises, the cylinder pressure rises. Thus if a constant
temperature is provided a constant pressure is maintained. This is true until the
liquid phase CO2 is depleted. For this reason it is advisable to keep the cylinder
at a fairly full condition. Do not let it drop more than 60% of its weight.
Inadequate Cooling
To insure reliable cooling power and trapping temperature stability, the CO2
must be delivered as liquid phase CO2. When cooling power is lost, the CO2 is
often being delivered as gas phase. This may be caused by 2 different
conditions.
1. CO2 supply is too low. There is insufficient CO2 remaining in the cylinder to
build supply pressure to the saturation pressure.
2. The CO2 has vaporized in the transfer line because the temperature of the
transfer line is higher then that of the supply. The supply temperature must
be equal to or warmer than the transfer line.
Locating the LCO2 supply cylinder near the GC in a temperature controlled
room is ideal.
a The critical point of CO is 31 C

2
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Varian, Inc.
Transfer Line
The SPT option comes with a 3 meter long, small diameter, low volume transfer
line. The supply cylinder must be located then, less than 3 meter from the GC.
The low volume feature of the transfer line helps this option tolerate situations
where the GC and transfer line are slightly warmer than the supply cylinder.
Keep the transfer line cool and stable by insulating it with foam insulation
provided in the Accessory Kit.
Recommended Supply Conditions
Supply
High pressure cylinder with siphon tube.
Supply Conditions
Temperature 15C to 27C (740 psia to 975 psia)
Outlet Filter
Transfer Line (from LCO2
cylinder to the GC)
Varian, Inc.
15 micron particulate filter (accessory kit) installed at

the cylinder connection.
A 3 meter long, 1/16 dia. Stainless steel tube is
included with this option. Install as a dedicated line
from supply to SPT. Insulate with foam pipe insulation.
User Manual 450-GC
Page: 259
LN2 Option
Description
The SPT - LN2 option allows trapping temperatures as low as -190C. For best
utilization of the high performance features of the SPT, it is recommended that
the transfer line from the LN2 source to the GC be very efficient. The LN2
transfer line should have the following characteristics:
Minimal length.
Should not have excessive restriction to flow.
Low thermal mass.
Well insulated.
In addition, the transfer line should not be routed near heat sources that could
reduce the cooling efficiency, such as the column oven exhaust fan.
If the SPT system is at ambient temperature (e.g., 23C) the time required
for initial cooling of the SPT from 50 to -190C might be longer
(approximately 5-10 minutes) than subsequent cooling cycles.
Figure 40: LN2 Coolant Flow Diagram
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User Manual 450-GC
Varian, Inc.
Recommended Supply Conditions

Due to high pressure build-up, LN2 tanks that are designed for pressures
higher than 50 psi must not be used with in-line regulators, shut-offs, or
restrictors. In all cases, never limit the tanks built-in venting system.
Supply
LN2 tank configured for liquid delivery.
Supply Pressure
19 to 25 psig
Transfer Line (from LN2 tank to GC).
1 to 3 meters length of (0.190 i.d.) o.d.

copper tubing, insulated with foam insulation
tubing.
Recommended temperature ranges
Parameter
450-GC Range
Recommended
Trapping Temperature
-60 to 450 C
-185 to 450
LCO2 - 60 to 50 C
LN2
- 185 to 40 C
Desorption Temperature
Program 1
Desorption Temperature
Program 2
SPT Temperature Limit
SPT Valve Oven
-185 or -60 to 450 a C
50 to 420C
-185 or -60 to 450 b C
50 to 420 C
-60 to 450 C
-185 to 450 C
--
-150 to 250 C
Table 48: SPT recommended operating ranges
No cryogen is used for trap temperature settings 50 C; no heat is

applied to the trap at trapping temperatures < 0 C.
It is advisable to purge adsorbent-containing traps by using an inert gas

(N2 or He). This procedure prevents inadvertent oxidation of the
adsorbent by accidental heating of the trap.
a Trapping temperature range is determined by coolant type.

b Trapping temperature range is determined by coolant type.
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User Manual 450-GC
Page: 261
Configuring the SPT

The SPT is typically factory installed and should be already configured when
the 450-GC is delivered. To check the SPT configuration press the setup
button. The SPT must be installed in zone 3.
Press on the Injector tab.

Press Page X button to view the SPT Injector setup, verify that the coolant
choice of LCO2 or LN2 matches the 450-GC hardware.
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User Manual 450-GC
Varian, Inc.
Building an SPT method

Follow the steps to set the SPT parameters:
1. Press the Injector button and press the SPT tab.
2. Verify that the SPT Enable checkbox is checked.

3. Verify that the Coolant checkbox is checked.
4. The Start Coolant at parameter is the temperature at which the coolant
valve turns on.
When the cooling starts the Remaining Coolant Time will count down.
If the cooling reaches the set temperature and the 450-GC does not go
into run, the cryo-valve will be turned off it the coolant time-out is
reached, and no further coolant will be applied. An event error will then
be generated.
5. The SPT temperature program can now be entered, see above for a typical
SPT program.
Varian, Inc.
User Manual 450-GC
Page: 263
Replacing the Trap Assembly

The trap can suddenly become extremely hot. Both the
trap and the SPT valve oven can remain hot for an
extended period of time, although the SPT cover, cryo
enclosure, and SPT valve oven cover might become cool.
Always turn power off to the GC and disconnect the SPT
trap harness connector from the SPT transformer prior to
removing the SPT cover or working on the SPT trap.
Tools required
3/16 back-up wrench (supplied in kit)

7/16 open-end wrench
Needle nose pliers
#2 Phillips screwdriver
Large flat blade screwdriver (LN2 Option only)
1/4 open-end wrench (2)
Varians ultra-clean reducing ferrules (supplied in kit) are

required for connecting the 1/16 stainless steel oven/trap lines
to the trap ends. These ferrules provide leak-tight seals, while
electrically isolating the trap end fittings from the tubing, and
have been specially treated to ensure that they are free of
contamination.
To maintain the ultra-clean condition of the reducing ferrules, the use of

clean cotton gloves or clean forceps is recommended.
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User Manual 450-GC
Varian, Inc.
SPT System Components

The replacement trap assembly is provided as a single unit. It should not
be disassembled. The following description of its basic components is for
reference only during installation of a replacement trap assembly.
VTAT traps cannot be used in the SPT.
Figure 41: SPT Components (Short Trap Assembly, LCO2 Option Shown
Varian, Inc.
User Manual 450-GC
Page: 265
Remove the SPT Cover

Follow these steps to remove the SPT cover and valve oven.
1. Turn the 450-GC power off (using the powerswitch) and unplug power cord.
2. Shut of coolant supply.
3. Remove GC top cover.
4. Unplug SPT trap harness connector from
SPT transformer harness (on page 256).
5. Remove SPT cover, by loosen the 2 screws.
6. Disconnect the LCO2 delivery line (part of LCO2

end plate assembly) from the union that
connects it to the restriction tube or Disconnect
LN2 delivery line (part of LN2 end plate
assembly) from the LN2 solenoid valve by
loosening and disengaging the Swagelok nut from
the fitting on the LN2 solenoid valve. The valve
mounting bracket might need to be loosened
slightly so fitting can be moved towards the rear.
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Varian, Inc.
7. Disconnect oven/trap lines from trap end fittings.

Use the 3/16 backup wrench to prevent rotation of
the trap end fittings (the flats on trap end fittings
should remain vertical). With the 7/16 open-end
wrench, loosen the two Swagelok nuts to release
any strain on the reducing ferrules.
8. Locate the screw holding the trap clamping bar.

Notice the Belleville washer under the screw head.
Unscrew and remove the bar.
9. Lift the trap/end plate assemblies to disengage trap
ends from slots in trap mounting block.
10. Remove the trap/end plate assemblies (if
necessary, lift up the SPT valve oven cover).
Detach Trap Assembly

1. Unhook the four SPT extension springs from the slots
along the edge of the LCO2 or LN2 end plate. The springs
should remain attached to the blank end plate assembly.
Use needle nose pliers to gently grip the open hook end of
the extension springs. Do not overextend the springs.
Overextending them might result in their permanent
distortion.
Figure 42: Removing Springs from Trap assembly

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User Manual 450-GC
Page: 267
Remove Cryo Nozzle Assembly

Follow the next steps to remove Cryo Nozzle Assembly form LN2 end plate
assembly.
Figure 43: Cryo Nozzle Assembly
1. Unscrew the cryo nozzle insert using a large flat bladed screwdriver.
Do not remove the cryo nozzle insert from within the cryo nozzle
assembly.
2. Remove entire cryo nozzle assembly: hold both cryo nozzle and
cryo nozzle insert together while removing them from within the trap coil.
This prevents loss of the three belleville washers that are stacked inside
the cryo nozzle assembly.
If the used trap assembly is still functional, its ends should be capped off to
isolate it from atmospheric contamination during storage.
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User Manual 450-GC
Varian, Inc.
Installing the Trap Assembly

Follow the steps below to prepare the replacement trap:
1. Confirm the part number of the intended replacement trap assembly.
Check that the size of the trap is correct (the long trap has three coils).
2. Uncap the replacement trap.
3. Hold the trap assembly with the trap ends pointed towards you, and the
word TOP on the cryo enclosure facing upwards.
In the following procedures, the terms right and left refer to this
orientation.
4. Preassemble the LN2 cryo nozzle components (Figure 43, on page 268):
a. Using a narrow pointed tool (such as a small screwdriver), align the
stack of three belleville washers in alternating orientations,
placing the first washer with its convex side facing the pointed tool.
b. Holding the pointed tool pointing up so the washer stack doesnt fall
off, lower the cryo nozzle over the washer stack so that the
washers are inserted fully into the large cavity of the cryo nozzle.
c.
Tip the cryo nozzle so that its large cavity is facing upwards, then
remove the pointed tool so as to not disturb the orientation of the
washer stack.
d. Insert the cryo nozzle insert (slotted end facing out) into the cryo
nozzle cavity.
e. Keep the cryo nozzle insert closely engaged within the cryo
nozzle.
5. Align the LN2 end plate assembly with the right open end of the cryo
enclosure and engage the cryo nozzle assembly (Figure 43, on page 268):
a. Orient the LN2 end plate assembly so that its delivery tube is
pointing away from you. Vent barb and vent tube should be at the
bottom with vent tube exiting to the rear.
b. The LN2 end pilot assembly, which is attached to the inside of the
LN2 end plate assembly, should fit into the right open end of the
cryo enclosure. Take care not to catch the edge of the gasket
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User Manual 450-GC
Page: 269
against the rim of the cryo enclosure; the rim should bear evenly
against the gasket facing in the area surrounding the end pilot.
c.
From the left side of the trap coil, engage the cryo nozzle
assembly through the coil. Screw the cryo nozzle insert onto the
threaded stud of the LN2 end pilot assembly using a large flat
blade screwdriver. Take care not to cross-thread the cryo nozzle
insert. Tighten gently, then back off approximately 1/12th of a turn.
6. To align the LCO2 end plate assembly, with the right open end of the cryo
enclosure:
a. Orient the LCO2 end plate assembly so that its delivery tube is
near the bottom of the right face and pointing away from you. The
Vent barb and vent hose should exiting to the rear.
b. The LCO2 end pilot assembly, which is attached to the inside of
the CO2 end plate assembly, should fit into the right open end of
the cryo enclosure. Take care not to catch the edge of the gasket
against the rim of the cryo enclosure; the rim should bear evenly
against the gasket facing.
7. Align the blank end plate assembly (see Figure 42, on page 267) with the
left open end of the cryo enclosure. The four SPT extension springs
attached to this assembly will have to be held out of the way of the
enclosure. The blank end pilot should engage into the left rim of the cryo
enclosure. Take care not to catch the edge of the gasket against the rim of
the enclosure; the rim should bear evenly against the gasket facing.
8. Use needle nose pliers to gently grip the open hook end of the extension
springs, and extend the springs to engage their respective slots that
should be aligned on the right end of the cryo enclosure in the LCO2 or
LN2 end plate assembly. Do not overextend the springs. Overextending
them might result in their permanent distortion.
9. If both end plate assemblies are properly engaged into the cryo
enclosure, they should be parallel to each other and perpendicular to the
sides of the cryo enclosure. The SPT extension springs should firmly hold
the end plate assemblies against the rims of the cryo enclosure. The
SPT extension springs should not touch the trap ends.
10. The oven/trap lines that connect to the trap end fittings should be
preformed for proper alignment with the trap end fittings. The nut and the
reducing ferrules should be preplaced onto the line ends so that when the
trap is installed, there is minimal bending of the lines.
To maintain the ultra-clean condition of the reducing ferrules during
installation, the use of clean cotton gloves or clean forceps is
recommended.
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11. Confirm that the trap assembly with the trap ends pointing towards the
front of the GC, with the word TOP on the cryo enclosure facing
upwards.
12. Engage the oven/trap lines into trap ends.
13. Align both trap ends with the slots in the trap mounting block. Lower trap
ends to engage into the slots.
14. Place the trap clamping bar over the trap ends.
15. Make sure the belleville washer on the trap clamping bar screw has its
concave side facing the trap clamping bar. Tighten trap clamping bar
screw to anchor the trap assembly into the SPT valve oven. Do not
overtighten.
16. Reconnect the valve oven/trap lines to trap end fittings. The packing type
number is stamped on the inlet trap end fitting (see Figure 41 on page
265). Carefully engage each nut onto its respective fitting to prevent crossthreading. Using the faces of the hexagonal nut as a guide, tighten each nut
fingertight, then tighten an additional:
a. Using new ferrules, 4/6 - 5/6 of a turn.
b. Reusing ferrules, 2/6 of a turn.
17. Do not over tighten. Use 3/16 backup wrench to prevent rotation of the
trap end fittings (the flats on fittings should remain vertical).
To avoid the possibility shorting the SPT electrical circuit, do not insert
the valve oven/trap lines more than 8 mm into the trap ends. Inserting the
lines too far into the trap ends will cause them to come in contact with
the trap.
Do not plumb the valve in such a way that metal tubing shorts across
trap tube ends.
18. Connect the LCO2 delivery line:

a. Connect the LCO2 delivery line (part of LCO2 end plate
assembly) to the union that connects to the restriction tube.
b. Check that vent barb and vent hose are exiting to the rear. Feed
the vent hose through the back panel of the GC.
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User Manual 450-GC
Page: 271
19. Connect the LN2 delivery line (part of LN2 end plate assembly) to the
LN2 solenoid valve by engaging the Swagelok nut to the connector on the
valve (see on page 266). Do not over tighten Swagelok fitting. The Valve
mounting bracket might need to be anchored to the GC. Do not induce
strain onto the delivery line: carefully align the LN2 solenoid valve and its
bracket during tightening of the valve mounting bracket.
20. Check that the drip pan is located under the LN2 solenoid valve. The drip
pan should not excessively block vent holes in the column oven top.
21. Tighten down the SPT valve oven cover.
22. Install the SPT cover.
23. Connect the SPT trap harness connector to the SPT transformer harness.
24. Replace GC top cover.
25. Turn on coolant supply.
26. Power up GC.
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Trap Conditioning
With carrier or auxiliary gas passing through the trap, condition the trap
according to the following table:
Packing Type
Mesh Size
Conditioning Procedure
Silanized Glass Bead
60-80
1 to 16 hours @ 250 to 400 C
Tenax/GR Charcoal
60-80
4 to 16 hours @ 250 C
HayeSep D
60-80
4 to 16 hours @ 250 C
Carbopack B, Carbopack C, Carboxen

1000, Carboxen 10001
60-80
4 to 16 hours @ 270 C
5% OV-101 on Chromosorb G/HP

Haysep D
60-80
4 to 16 hours @ 270 C
Tenax Gr, Carbopack B, Carbosieve

S-111
60-80
4 hours @ 225 C
Tenax TA,
60-80
4 hours @ 225 C
Tenax TA, Charcoal
60-80
4 hours @ 200 C
Carbopack C, Carbosieve S-111
60-80
4 hours @ 200 C
Carbopack C, Carbopack B
60-80
4 hours @ 270 C
Carbopack B, Carbosieve S-111
60-80
4 hours @ 200 C
Tenax GR
60-80
4 hours @ 200 C
Table 49: SPT Trap conditioning
Varian, Inc.
User Manual 450-GC
Page: 273
Replacement SPT traps

The table below is a partial list of available trap assemblies. Consult your local
sales representative or Parts and Supplies Marketing for additional versions.
Trap Description
Partnumber
Short Traps
Short Trap Assembly Kit (8 cm), silanized glass beads
03-925713-92
Short Trap Assembly Kit (8 cm), blank
03-925713-91
Blank Trap
03-925713-01
Packed, Glass Beads
03-925713-02
Long Traps
Long Trap Assembly Kit (30 cm), blank
03-925714-91
Blank Trap
03-925714-01
Tenax GR/Charcoal
03-925714-02
Tenax GR
03-925714-03
Carbopack B, Carbosieve S-III
03-925714-04
5% OV-101 on Chromosorb G/HP, HayeSep D
03-925714-05
Carbopack C, Carbopack B, Carboxen 1000, Carboxen 1001
03-925714-06
Carbopack C, Carbosieve S-III
03-925714-07
HayeSep D
03-925714-08
Tenax TA, Charcoal
03-925714-09
Tenax TA
03-925714-10
Tenax GR, Carbopack B, Carbosieve S-III
03-925714-11
Kit, Blank Trap
03-925714-91
Kit, Tenax GR/Charcoal
03-925714-92
Kit, Tenax GR
03-925714-93
Kit, Carbopack B, Carbosieve S-III
03-925714-94
Kit, 5% OV-101 on Chromosorb G/HP, HayeSep D
03-925714-95
Kit, Carbopack C, Carbopack B, Carboxen 1000, Carboxen 1001
03-925714-96
Kit, Carbopack C, Carbosieve S-III
03-925714-97
Kit, HayeSep D
03-925714-98
Kit, Tenax TA, Charcoal
03-925714-99
Kit, Tenax TA
03-925714-80
Kit, Tenax GR, Carbopack B, Carbosieve S-III
03-925714-81
Table 50: SPT replacement traps

Page: 274
User Manual 450-GC
Varian, Inc.
SPT replacement parts

Partnumber
Part Description
Cryo Valve:
LCO2
LN2
03-925555-01
03-925557-01
Ferrule for Restriction Tube (LCO2)
28-694502-00
Nuts for Restriction Tube (LCO2)
28-694501-00
Insulation Tubing (LN2)
24-000467-00
Outlet Filter (LCO2)
27-590826-00
Reducing Ferrule (Ultra-clean, for Trap Assembly)
03-918850-00
Restriction Tube, 22 Long (LCO2)
03-918853-01
SPT PCB
03-918758-00
SPT Transformer
03-918788-00
Transfer Line from LN2 Supply to GC

(1/4 Copper, 10 Length)
37-000146-01
Trap Clamping Bar
03-918765-00
Trap Mounting Block
03-918764-00
Union (LCO2)
28-211457-00
Transfer Line from LCO2 supply to GC

(1/16 stainless steel, 10)
03-918852-00
Ferrules for stainless steel Transfer Line (Front)
28-693996-00
Ferrules for stainless steel Transfer Line (Back)
28-693997-00
Nuts for stainless steel Transfer Line
28-693998-00
Ferrules for stainless steel Transfer Line (1/8) (Front)
28-694027-00
Ferrules for stainless steel Transfer Line (1/8) (Back)
28-694028-00
Nuts for stainless steel Transfer Line (1/8)
28-694029-00
Ferrules, Vespel, Reducing 1/8 To 1/16
03-918850-00
Installation Kit, LCO2
03-918801-01
Installation Kit, LN2
03-918801-02
Table 51: SPT Replacement Parts
Varian, Inc.
User Manual 450-GC
Page: 275
Troubleshooting
This section provides troubleshooting information to aid the operator in locating
and correcting apparent problems when working with an SPT system. The
following table is geared specifically to SPT troubleshooting. If you have
questions about any of the corrective actions described below, contact your
Varian Customer Support Representative.
Symptom
Possible Cause
Remedy
SPT overheating.
Faulty SPT RTD sensor.
Replace trap assembly.

Check and reconnect
harness.
SPT heating too slowly.
SPT RTD harness not properly

connected to SPT electronic board.
Short in electrical system:
Oven/trap line making contact with
trap.
Adjust oven/trap line and

trap end fitting.
Replace mounting block.
Insulating surface (gray) of the SPT

trap mounting block damaged.
Bushings not isolating trap from the
cryo enclosure.
Replace cryo valve.
SPT not heating.
Cryo valve stuck open.

SPT transformer circuit breaker
tripped.
Correct problem; reset.

Reconnect harness.
SPT trap harness not properly

connected to the SPT transformer.
SPT RTD harness open or shorted.
SPT trapping temperature set to <0
C.
Page: 276
User Manual 450-GC

Set temperature to equal or
greater than 0C.
Varian, Inc.
Symptom
Possible Cause
Remedy
No coolant flow.
SPT performing desorption

temperature program.
Perform trapping
Coolant supply exhausted or low.
Replace coolant supply.
Coolant restriction tube plugged

(LCO2).
Clean or replace restriction

tube. Replace in-line filter.
Coolant supply not connected.
Connect and turn on coolant

supply.
SPT overcooling.
SPT undercooling or
cooling too slowly.
Coolant has timed out (status light

blinking).
Press [RESET]; Enter new

value for Coolant Timeout, if
desired.
Coolant is not enabled in GC

Configure table.
Enable coolant.
Cryo valve is not connected to

Temperature Control electronic
board.
Connect cryo valve.
Cryo valve stuck closed.

Cryo valve stuck open.
Replace cryo valve.

Replace cryo valve.
Supply cylinder too warm or to cold.
Relocate coolant supply to a

location within
recommended temperature
limits.
Make sure that GC and
transfer line are cooler than
cryo supply cylinder.
Coolant supply has been depleted of

liquid phase CO2.
Trapping temperature is
oscillating out of ready.
Supply too warm (27C)
GC and transfer line are too warm

relative to the supply.
Varian, Inc.
User Manual 450-GC
Replace supply with a full

dewar or cylinder.
Relocate coolant supply to a
location within
recommended temperature
limits.
Make sure that GC and
transfer line are cooler than
cryo supply cylinder.
Provide a cooler
environment for the GC
(should be cooler than cryo
supply).
Page: 277
Symptom
Page: 278
Possible Cause
Remedy
Transfer line is too long.
Shorten transfer line.

Insulate transfer line.
User Manual 450-GC
Varian, Inc.
Detectors
DETECTORS
INTRODUCTION
The 450-GC can accommodate up to three installed detectors and have all
three running simultaneously.
The standard detectors available on the 450-GC are:
The Flame Ionization Detector (FID), on page 283.
The Pulsed Discharge Helium Ionization Detector (PDHID), on page 295.
Thermionic Specific Detector (TSD), on page 305.
Thermal Conductivity Detector (TCD), on page 319.
Electron Capture Detector (ECD), on page 329.
Pulsed Flame Photometric Detector (PFPD), on page 343.
Except for the TCD and PFPD any combination of three detectors can be
installed.
In case of the PFPD, only two may be installed but any one additional detector
may also be installed including a TCD.
In the case of the standard TCD, only two can be installed and then no
additional detectors can be installed.
However, a dual TCD option is available as a custom solution which allows
installation of an additional ionization detector.
The dual TCD consists of 2 detector cells in one housing but using only one
heating zone.
Detectors are mounted on the top of the 450-GC, above the left side of the
column oven.
The position of the detector, however, is determined by the location of the
detectors electrometer in the electronics cabinet. Detector electrometers are
installed on the left side of the GC accessed by removing the left side panel.
All cables connecting the electrometers to the detectors are accessible by
removing the 2 covers on the top left of the 450-GC, i.e. the detector top cover
and the cover over the keyboard/display.
For connecting a capillary column to a detector, see Connect Capillary Column
to Detector on page 24.
Varian, Inc.
User Manual 450-GC
Page: 279
Detectors
ANALOG OUTPUT
The 450-GC can be equipped with an option board.
The analog output signals are located at connector J401, on page 36 on the top
of the GC, accessed by removing the top left cover.
This connector contains all 3 analog channels plus status signals for Ready-In
to the GC and Start Out from the GC.
page by the detector tab on the second page (Page 2 or
In the SETUP
page 3) the Detector Analog Output screen will be visible, only if the Analog
option board is present.
The Analog Output Port name can be changed by the button Edit.
If the Range setting must be changed, make sure that the Range setting
matches the mainboard jumper settings!
Page: 280
User Manual 450-GC
Varian, Inc.
Detectors
The analog output ports are programmed in the 450-GC method by pressing
key on the keyboard, select Analog Output.
the DETECTOR
This brings up a menu screen from which you choose one of the three ports to
program; Page 1, Page 2 or Page 3. The following screen appears when
Page 1 is chosen.
The Analog Output Port name is in this example is A, but can be changed in the
Setup screen. The individual analog ports can be assigned to any installed
detector on the 450-GC. The ports are identified as A, B and C with the default
assignment being front, middle and rear detector respectively. Default Analog
output voltage is 0-1 Volt (0-10 Volt is possible by selectable jumpers on the
mainboard (contact your local Varian office).
The right-side of the screen is used to time program the signal source of the
analog output. By default analog output A is assigned to the front detector. In
the example above, the analog port is programmed to transmit the Front
detector signal for the first 10 minutes of the run and then switch to the Middle
detector after 20 minutes the switch will be made to the rear detector for the
remainder of the run. This mode of operation is known as detector switching.
Note that the attenuation should normally be set to 0. However for optimum
resolution (less electronic noise) the best results are achieved by increasing the
attenuation if small peaks are detected. For overloaded peaks decrease
attenuation.
Varian, Inc.
User Manual 450-GC
Page: 281
Detectors
The 450-GC has a number of analog cable options on page 94, depending on
the device to which the cable is connected. All cables have a 15 pin D-shell
connector on one end to attach to J401 on the 450-GC and have the
appropriate connectors on the other end of the cable for the devices to which
they are being attached.
Page: 282
User Manual 450-GC
Varian, Inc.
Flame Ionization Detector (FID) - Detectors
FLAME IONIZATION DETECTOR (FID)
The flame ionization detector (FID) is the most sensitive gas chromatographic
detector for hydrocarbons such as butane or hexane. With a linear range for 6
or 7 orders of magnitude (106 to 107) and limits of detection in the low picogram
or femtogram range, the FID is the gas chromatographic detector for volatile
hydrocarbons and many carbon containing compounds.
The FID detector employs hydrogen as the combustion gas which is mixed with
Air and the column eluent (helium, nitrogen or other appropriate gas) and burn
at a small jet situated inside a cylindrical electrode. A potential of a few hundred
volts is applied between the jet and the electrode and when a carbon containing
solute is burn in the jet, the electron/ion pairs that are formed are collected at
the jet and cylindrical electrode.
The following instructions refer to the operation of a 450-GC Flame Ionization
Detector (FID). The FID is installed on a detector base, directly above the
column oven. The FID electrometer is installed in the electronics cabinet on the
left of the instrument. The electronics of the FID are controlled from the 450-GC
Display/Keyboard, the gas flows are set and controlled either from the 450-GC
Display/Keyboard (if detector EFC is installed) or at the pneumatics panel.
Varian, Inc.
User Manual 450-GC
Page: 283
Detectors Flame Ionization Detector (FID)
Initial Set-Up
To set-up the FID, proceed as follows. Note that when the 450-GC is first
powered up all heated zones with the exception of the column oven are
powered off and all detector electronics are turned off.
1. Refer to the Pre-Installation Instructions for additional information on gas
supply requirements.
key on the 450-GC Display/Keyboard to display
2. Press the DETECTOR
the DETECTOR screen. The FID should be listed in position Front ( ),
Middle ( ) or Rear ( ). If your GC is equipped with detector EFC verify the
makeup gas you will be using with your FID.
3. Install a chromatographic column in the GC, on page 13. If the analytical
column is not pre-conditioned, use a no-hole ferrule in the detector column
nut while conditioning the column and leave the detector end of the column
loose in the oven. If the analytical column is pre-conditioned, follow the
usual procedure for column installation.
Page: 284
User Manual 450-GC
Varian, Inc.
4. If detector EFC is present, set the following flow rates in the adjustments
section of the FID method:
Make-up flow to 25 mL/min.

The hydrogen flow to 30 mL/min.
Air flow to 300 mL/min.
Note: For optimum performance the combined column + make-up flow

should be 30 mL/min, so some adjustment of the make-up flow may be
necessary.
5. If manual pneumatics is installed, attach a bubble or digital flowmeter
(AL5700) to the top of the FID tower using the adapters supplied in the FID
accessory kit (Note that the most reliable measure of flow is directly from
the flame tip. This prevents wrong-adjustment due to leaks in the overall
tower assembly). Check the following flow rates and set them if necessary:
combined carrier gas + make-up flow to 30 mL/min, the hydrogen flow to 30
mL/min and the air flow to 300 mL/min.
key on the 450-GC Display/Keyboard, select
the FID by its location and turn on the FID oven power. Set the oven
temperature to 300 C. Verify that the FID electronics is turned OFF.
Operation
1. Check the detector temperature status on the DETECTOR/FID screen.
Check the FID range setting and set to range 12, if necessary.
Generally, to prevent water condensation in the detector assembly, the
detector should be operated at a temperature above the column
temperature and not below 150 C. If the detector is operated at a lower
temperature, condensation can lead to excessive noise.
2. After the FID oven has reached its setpoint temperature, turn on the FID
electronics. Note that the FID will ignite automatically when auto-ignite
conditions are fulfilled (for detailed information about auto-ignite conditions
see here, on page 287). The 450-GC monitors the FID background current
continuously and will attempt to ignite the flame (only if in Setup/Detector
the checkbox on page 75 check for flame out is checked) if the current
drops below a specified threshold. Up to three attempts to ignite the flame
will be made before the 450-GC reports a flame-out fault. If a flame-out fault
is reported, correct the cause of the flame-out and then clear the fault in
Instruments Log.
The FID will automatically ignite after the fault is cleared.
Varian, Inc.
User Manual 450-GC
Page: 285
DO NOT look directly into the detector tower

when attempting to ignite the flame.
You can verify that the flame is lit by monitoring the FID signal in the
status region of the FID display.
Uncheck the box AutoZ. and press Clear AutoZ.
Initially the signal will read a very high value but should then stabilize.
Typically the signal will be > 50 mV at range 12 when the flame is first
lit but should drop to < 10 mV within 30 minutes.
To avoid a possible fire or explosion, always turn

off the flow of hydrogen when the column is
removed or when the detector is not being used.
This prevents the accumulation of hydrogen.
3. Set the Time Constant to Fast. The default setting for the time
constant is Fast.
Fast time constant:
- Used with capillary columns.

- Reduce high frequency noise.
- Used for narrow peaks.
Slow Time Constant:
- Used with packed columns.

- Used for broad peaks.
4. The Ignite button applies power to the FID igniter filament for 5
seconds.
5. The Autozero button applies an immediate zeroing of the detector
signal.
Page: 286
User Manual 450-GC
Varian, Inc.
FID auto-Ignite flow diagram
1
Figure 44: FID auto-Ignite flow diagram
a In an automated sequence the 60 seconds delay helps to recover from FID flame faults and avoids
having the fault again in the next run. It also prevents a workstation starting a run while FID ignition is still
going on.
Varian, Inc.
User Manual 450-GC
Page: 287
Installation/Disassembly
At times, it is necessary to remove the detector components to inspect, to
clean, to replace parts, or to install another detector. Follow the
disassemble/reassemble instructions on the next pages for both the FID and
the detector oven.
Exploded View
6
1
8
9
4
10
1
2
3
4
5
6
7
8
9
10
11
11
12
13
14
15
16
-----
11
Signal Cable (200187700)
Signal Probe (200187300)
12
Ignitor Cable (392548701)
Ignitor Probe (200187200)
13
Screws, 8-32 x (1214200804)
Collector Tube (394958700)
Tower Screws, 8-32 x 3 (391866301)
14
Ceramic Insulator (2100003200)
Tower Top Plate (3400073100)
Detector Tower Body (100099300)
Flame Tip, 0.01 in. Capillary Tip (200187500)
15
Flame Tip, 0.02 in. Standard Tip (200193800)
Ferrule: Vespel (100%) max. 350C (CR212200)
16
Graphite/Vespel 40/60 max. 400C (CR213200)
Graphite (100%) max. 450C (CR211200)
Aluminum Seal Washer (1500334701)
Figure 45: FID Exploded View
Detector Base (392547501)
Column Ferrule
Column Nut (394955100)
Flow Tube (200187600)
Large Stopper (394958600)
Page: 288
User Manual 450-GC
Varian, Inc.
Disassemble the FID

To disassemble the FID, proceed as follows:
1. Set the FID to 50 C and wait for it to cool before disassembly. Turn the
detector electronics and detector oven OFF in the active method. Remove
the GC Top-Covers.
2. Turn off the main GC gas supplies to the detector at the pneumatics panel.
These are the make-up, hydrogen and air supplies.
3. Disconnect the signal and igniter cables from their probes on the detector
tower.
4. Remove the signal and igniter probes from the detector tower. DO NOT
rotate the probes as you disconnect them from the electrical contacts in the
tower. Place the probes on a clean surface such as a lint-free laboratory
tissue.
5. Remove the 2 tower mounting screws from the top of detector tower.
6. Remove the tower assembly from the detector oven, lifting straight up until
clear of the flame tip. Remove the collector tube and insulator from the
detector tower. Avoid contamination of the ceramic insulator and probes. If
the detector is not completely cool, use a metal tool (such as tweezers or a
hooked wire) to remove parts from the tower assembly. Place parts on a
clean Kimwipe. Never place them on a counter or painted surface.
7. Remove the flame-tip assembly from the detector base. Take care not to
break the ceramic flame tip tube or the Vespel/graphite or graphite ferrule.
8. Remove and discard the aluminum seal washer from the detector base.
Always use a new aluminum seal washer each time you reassemble the
detector. Note that the aluminum seal washer may remain in the detector
tower when the tower is removed from the base.
Varian, Inc.
User Manual 450-GC
Page: 289
Reassemble the FID

Refer to Figure 45 on page 288 to reassemble the FID detector. To reassemble
the FID, proceed as follows:
1. Re-assembly is the reverse of removal.
2. Install the flame tip in the detector base. The FID and TSD flame tips are
identical.
If you are installing the flame tip with a new Vespel/graphite ferrule,
tighten the assembly finger-tight plus an extra 1/6-turn.
If you are installing the flame tip assembly with a used graphite
ferrule, tighten about 1/3-turn past finger tight.
3. The Vespel/graphite ferrule supplied with the GC has a maximum
temperature limit of 400 C. If it is necessary to operate the detector above
400 C, you may need to replace the Vespel/graphite ferrule with a graphite
ferrule (450 C).
4. Install a new aluminum seal washer onto the shoulder of the detector base.
To ensure a reliable tower seal, use a NEW aluminum washer each time
you install the detector.
5. Place the detector tower on the detector base and secure it with the 2 tower
mounting screws. Alternately tighten these screws a -turn as the tower
tightens into place.
Handle the ceramic insulator and probes with tweezers to avoid

contamination.
6. Carefully insert the igniter probe into the lower arm of the detector tower.
Align the probe key with the tower arm slot. Check the orientation of the
igniter elements by looking down through the top of the detector tower. The
spring clip should slip around the flame tip and make good contact (see
Figure 46 on page 291). The igniter coil must not touch the flame tip
assembly nor be positioned directly above it. Tighten the knurled nut to
secure the probe.
7. Make sure the notch in the detector tower arm does not cut the O-ring seal.
8. Insert the insulator into the detector tower, then insert the collector tube into
the tower. The collector tube must not touch the igniter coil.
Page: 290
User Manual 450-GC
Varian, Inc.
9. Insert the signal probe into the upper arm of the detector tower. The probe
clip should fit around the tapered section on the collector tube tightly
enough to exert a downward force (see Figure 47). Secure the signal probe
by tightening the knurled nut. Make sure the notch in the detector tower arm
does not cut the O-ring seal.
10. Connect the igniter cable to the igniter probe and the signal cable to the
signal probe.
Detector Tower
TOP VIEW
Ignitor Coil
Spring Clip
Flame Tip
Figure 46: Orientation of Igniter Probe Elements in FID Tower
Collector Tube
(03-949587-00)
Signal Probe
Insulator
Ignitor Coil
Notch
Spring Clip
Flame Tip
Assembly
Ignitor Probe
Figure 47: FID Cross-sectional View
Varian, Inc.
User Manual 450-GC
Page: 291
MAINTENANCE
When the performance of the FID has degraded you may want to replace the
flame tip ferrule, or clean the deposits from the internal parts, including the
flame tip.
Clean the Flame Tip and Internal Parts

If the FID noise increases with frequent spikes, the internal parts may be
contaminated and need to be cleaned.
To clean the flame tip and the internal parts of the FID, proceed as follows:
Always handle detector components with tweezers to avoid
contamination.
Use proper eye and skin protection. Methanol and acetone

are toxic and flammable chemicals. Exercise appropriate
care when you use and dispose of these substances.
1. Remove the detector and internal parts (see disassemble the FID, on page
289).
2. Scrape the deposits from the bore of the collector tube, the insulator and
the metal part of the flame tip with emery cloth (e.g., SiO2).
3. If the flame tip is plugged, insert a wire through the flame tip orifice to clear
it.
4. If you have access to an ultrasonic cleaner, clean the collector, insulator
and flame tip with distilled water.
5. Rinse the cleaned components with methanol or acetone and air dry.
6. Wipe the detector tower with acetone.
7. Clean the probe arms with methanol and air dry or dry in an air oven
(maximum drying temperature of 150 C).
8. Reassemble the FID, see Reassemble the FID, on page 290.
Page: 292
User Manual 450-GC
Varian, Inc.
Replace the Flame-Tip Ferrule

After a period of prolonged use, the flame-tip ferrule may deteriorate and crack.
As a consequence, a leak may develop around the base of the flame tip
assembly that causes unstable baseline noise and reduced sensitivity. In this
situation, or when the detector is to be operated at temperatures above 400 C,
you must replace the ferrule. Be sure to select the proper ferrule for the
application. The Vespel/graphite ferrule has a maximum temperature limit of
400 C see Figure 45on page 288.
Varian recommends to NOT using other ferrules then those listed. Due to small
dimensional variations common in these ferrules leaks on higher temperatures
are possible.
FID Test Chromatogram

For an FID test chromatogram see section Detector Test Chromatograms, on
page 420.
Varian, Inc.
User Manual 450-GC
Page: 293
Page: 294
User Manual 450-GC
Varian, Inc.
Pulsed Discharge Helium Ionization Detector (PDHID) - Detectors
PULSED DISCHARGE HELIUM IONIZATION DETECTOR (PDHID)
The PDHID is a non-radioactive pulsed discharge ionization detector (PDHID)

which is optimized for the Varian 450-GC. A schematic representation of the
detector is shown in Figure 48.
The detector utilizes a stable, low power, pulsed DC discharge in helium as the
ionization source. Elutants from the column, flowing counter to the flow of
helium from the discharge zone, are ionized by photons from the helium
discharge above. Resulting electrons are focused toward the collector electrode
by the 2 bias electrodes.
The principal mode of ionization is photoionization by radiation arising from the
transition of diatomic helium He2 (A1+u) to the dissociative 2He(1S1)ground
state. This is the well-known Hopfield emission. The photon energy from the
He2 continuum is in the range of 13.5 to 17.7 eV.
The detector is essentially non-destructive (0.01 - 0.1% ionization) and highly
sensitive. The response to organic compounds is linear over five orders of
magnitude with minimum detectable quantities (MDQs) in the low picogram
range. The response to fixed gases is positive (the standing current increases),
with MDQs in the low ppb range.
Detector response is universal except for neon, which has an ionization
potential of 21.56 eV. Since this potential is close to the energy of the He*
metastable (19.8 eV) but greater than the photon energy from the He2
continuum, neon exhibits a low ionization efficiency and low detector response.
When a dopant is added to the discharge gas, the detector also functions as a
selective photoionization detector. (Suitable dopants include Ar for organic
compounds, Kr for unsaturated compounds, or Xe for polynuclear aromatics).
Varian, Inc.
User Manual 450-GC
Page: 295
Detectors Pulsed Discharge Helium Ionization Detector (PDHID)
Figure 48: Schematic of the PDHID Detector
HELIUM IONIZATION (PDHID)

The PDHID is essentially non-destructive (0.01 - 0.1% ionization) and highly
sensitive. The response to organic compounds is linear over five orders of
magnitude with minimum detectable quantities (MDQs) in the low or sub
picogram range. The response to fixed gases is positive (the standing current
increases), with MDQs in the low ppb range.
The PDHID response is universal except for neon, which has ionization
potential of 21.56 eV. Since this potential is close to the energy of the He*
metastable (19.8 eV) but greater than the photon energy from the He2
continuum, neon exhibits a low ionization efficiency and low detector response.
Page: 296
User Manual 450-GC
Varian, Inc.
During normal operation, the detector produces ultraviolet energy (UVA,

UVB), some of which may be emitted. Do not watch the arc without eye
protection!
Cable overview
Figure 49: PDHID Cable Overview
Varian, Inc.
User Manual 450-GC
Page: 297
Exploded View
1.
Ground electrode (CP740764)

Nut for ground electrode (CP914060)
Spanner tool (CP740760)
2.
Detector cell (CP740765)
3.
High voltage cable (CP740763)
4.
Bias Cable assy (CP740761)
5.
Electrometer cable assy (CP740773)
3
5
Figure 50: PDHID Exploded View
Page: 298
User Manual 450-GC
Varian, Inc.
Gas Connections
Figure 51: PDHID Gas Connections Overview
Installation
The installation of the PDHID detector is normally done at the factory, field
installations are not advised.
Varian, Inc.
User Manual 450-GC
Page: 299
General Precautions
Do not use plastic/polymer or copper tubes for gas handling and

interconnections. Use only stainless steel tubing with Valco gold-plated ferrules.
Do not turn the unit on until helium discharge gas is flowing through the
detector.
Do not shut off or disconnect the discharge gas when the detector is hot, even if
the unit is turned off. Turn off the discharge power switch and allow the detector
to cool down naturally before disconnecting or shutting off the discharge gas.
Do not cover the unit with anything which could restrict air circulation.
Position the controller unit where the mains switch on the rear panel can be
reached easily.
Never use leak detecting fluids on any part of the system.
Installing and Purging the Helium Purifier

1. If the pressure regulator has a 1/8" male cone-type outlet port, install the
Valco 1/8" external to 1/16" internal reducer (EZR21); if it has a 1/4" male
cone-type outlet port, install the Valco 1/4" external to 1/16" internal reducer
(EZR41). For other regulator outlet fittings, a wide variety of Valco adapters
is available.
2. Remove the cap from the inlet tube of the Valco helium purifier and insert
the tube fitting into the 1/16" reducer port. (Keep the outlet tube capped.)
Use a 1/4" wrench to turn the nut one-quarter turn past the point where the
ferrule first starts to grab the tubing. Do not remove the fitting. When made
up properly, it should be leak-tight.
3. Turn the output pressure regulating knob clockwise until the gauge
registers 345 kPa (50 psi).
4. Allow 5 minutes for equilibration, then turn the regulating knob all the way
counterclockwise.
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5. Observe the needle of the output pressure gauge for 15 minutes. There will
be a slight initial drop, but if it doesnt move after that, consider that all the
connections are tight.
6. If necessary, use an electronic leak detector to locate any leaks. If a leak
detector is not available, tighten all the fittings (including the output
pressure gauge) and repressurize the system for another test.
7. Uncap the outlet tube of the purifier and purge the system for 15 to 30
minutes at 60 - 80 mL/min to eliminate air from the purifier getter material.
Connecting the Discharge Gas to the Detector

1. If you are supplying the GC from the helium purifier, use the Valco ZX1
cross. (The cross supplies an extra port for a blank helium run.) Otherwise,
use one of the Valco 1/16" unions (ZU1) to connect the outlet tube of the
purifier to the inlet of the supplied discharge gas.
2. Restrictor (TGA-R-35F80P).
3. Connect the outlet end of the restrictor to a flow measuring device. Adjust
the helium pressure to 80 psi to obtain a continuous flow of ~35 mL/min.
4. After setting the flow rate, connect the outlet of the restrictor to the
discharge gas inlet tube (labeled INLET) which comes out the side of the
detector.
Capillary Column Connection

If the capillary column adapter is installed in the column inlet:
1. Make a mark on the column 11.4 cm from the end.
2. Remove the knurled nut and plug from the capillary column
adapter in the column inlet at the bottom of the detector. Slide
the nut over the end of the column, followed by the appropriate
column ferrule (FS.4 or FS.5, or ZF.5V for megabore).
3. Seat the ferrule in the detail of the column adapter and begin
sliding the column through the capillary column adapter and
into the column inlet.
4. Get the nut started on the threads and tighten it until you feel it
contact the ferrule, then back off half a turn. Slide the column
into the column inlet until the mark is flush with the surface of
the knurled nut and secure the column in the adapter by
tightening the knurled nut finger tight only.
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User Manual 450-GC
Page: 301
If the capillary column adapter has been removed, reinstall it:

1. Unscrew the liner as far as it will go, then screw the fitting body into the
column inlet fingertight.
2. While using a 1/8" wrench to prevent rotation of the liner (the part with the
seat for the column ferrule), use a 1/4" wrench to tighten the body of the
adapter until the ferrule has sealed. The liner will deform if it rotates.
3. Proceed to Step 1 above.
Packed Column Connection

To prevent detector contamination, we strongly recommend
disconnecting the column from the detector during column bakeout
procedures.
The PDHID is optimized for packed columns. The column tubing must be
thoroughly cleaned and baked before the column is packed. Even when the
best care is taken in column tubing cleaning and in the support and stationary
phase selection, a new column will often bleed compounds, resulting in a
considerable increase in the detector baseline. This initial bleed will usually be
reduced to acceptable levels after the column is conditioned with clean carrier
gas flow for several hours at the recommended bakeout temperature.
1. Loosen and remove the knurled nut and plug of the capillary
column adapter, (or remove the column ferrule and the column if
one has been installed).
2. Use a 1/8" wrench to hold the liner that part of the adapter in
which the column ferrule sits. While the 1/8" wrench keeps the
liner from rotating, use a 1/4" wrench on the fitting body to
loosen the adapter 1/2 turn.
3. Set aside the 1/8" wrench and completely remove the adapter
from the column inlet.
4. Screw the packed column adapter into the column inlet by hand.
Exercise caution, as the tip of the adapter is very fragile. Then
tighten the adapter with a 1/4" wrench, using an additional
wrench on the flats of the column inlet to support the detector.
5. Connect the 1/8" column to the packed column adapter with the
EZRU21 reducing union supplied in the fittings kit.
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Testing for Leaks

It is critical for the system to be leak-tight and an additional check at this point can
save many headaches later on. To test for leaks:
1. Cap the tube and pressurize the entire system with helium to 138 kPa (20 psi).
2. If the system does not hold pressure, check all the fittings with an electronic
helium leak detector. DO NOT use leak detecting liquids.
3. Tighten fittings as required.
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Page: 303
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Thermionic Specific Detector (TSD) - Detectors
THERMIONIC SPECIFIC DETECTOR (TSD)
The Thermionic Specific Detector (TSD) is also known as Nitrogen Phosphorus

Detector is a very sensitive but specific detector that responds almost
exclusively to nitrogen and phosphorous compounds. It is based on the flame
ionization detector but differs in that it contains a rubidium silicate (glass) bead
situated in a heater coil, a little distance from the hydrogen flame. If the detector
is to respond to both nitrogen and phosphorous then the hydrogen flow should
be minimal so that the gas does not ignite at the jet. If the detector is to respond
to phosphorous only, a large flow of hydrogen is used which is burn at the jet.
The heated bead emits electrons by thermionic emission. These electrons are
collected under a potential of a few volts by an appropriately placed anode and
provides a background current. When a solute containing nitrogen or
phosphorous is eluted from the column, the partially combusted nitrogen and
phosphorous materials are adsorbed on the surface of the bead. The adsorbed
material reduces the work function of the surface and, as consequence, the
emission of electrons is increased which raises the current collected at the
electrode. The sensitivity of the detector to phosphorous is about 10-12 gram
per mL and for nitrogen about 10-11 gram per mL at a signal to nose ratio of 2.
The bead has a finite life and needs regular replacement. These instructions
refer to the installation and operation of the Thermionic Specific Detector (TSD)
on the 450-GC. The TSD detector tower is installed on a 450-GC detector oven.
The TSD Electrometer Board is installed in the GC electronics cabinet on the
left side of the instrument. The TSD is controlled through the keyboard on the
front panel of the GC. Gas flows are controlled at the pneumatics panel of the
GC, or in the Adjustments section of the method if Detector EFC is installed.
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User Manual 450-GC
Page: 305
Detectors Thermionic Specific Detector (TSD)
Initial Set-Up
To set up the TSD for operation, proceed as follows. Note that when the 450GC is first powered up all heated zones with the exception of the column oven
are powered off and all detector electronics are turned off.
the DETECTOR screen. The TSD should be listed in location Front ( ),
Middle ( ) or Rear ( ). If your 450-GC is equipped with detector EFC,
verify the makeup gas you will be using with your TSD.
3. Install a chromatographic column in the GC (refer to the Column installation

information on page 23). If the analytical column is not well conditioned, use
a no-hole ferrule in the detector column nut while conditioning the column
and leave the column end loose in the oven. If the analytical column is well
conditioned, follow the usual procedure for column installation.
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4. Condition the TSD bead. The following bead conditioning and optimization
procedures assume use of a short, non-polar column such as the Varian
test column, 03-912300-30 (packed, COLUMN, 1/8" X 50 CM 5%, OV101)
or CP887098 (capillary CP-Sil 5 CB, 4M X .32). If you use a different type
of column, you should adjust conditions accordingly.
Operation and Operating Recommendations

TSD operation requires hydrogen, air+make-up and either nitrogen a or helium
carrier gas. The amount of hydrogen relative to the other gases will affect
nitrogen-to-carbon and phosphorus-to-carbon selectivity of the detector. The
nitrogen-to-phosphorus selectivity also may vary somewhat but the detector
cannot be tuned to respond to only nitrogen or only phosphorus.
When power is first applied to the TSD, the bead may require 2 to 3
minutes to re-light, i.e. stabilize the bead surface temperature and gas
phase reactions. If the bead does not re-light, check for other errors and
review the bead conditioning procedure and the bead optimization
procedure.
Bead Conditioning
This TSD bead probe requires additional conditioning to perfect detector
performance. Follow these recommended procedures to ensure maximum
lifetime and reliability of your TSD bead. Failure to follow these procedures may
result in poor performance and reduce TSD bead probe lifetime.
Each bead probe will have a particular bead current (i.e. bead surface
temperature) at which its gas phase chemistry will initiate. In order to operate
the detector, it is necessary to allow the bead to reach this ignition temperature
in a controlled manner. Attempting to accelerate this procedure may decrease
the lifetime of the TSD bead probe.
1. Check the position of the TSD bead in the detector tower. The TSD bead
must NOT make contact with the TSD collector screen. The bead should be
located in the center of the collector, with the collector positioned so that
both edges of the screen are equidistant from the bead.
2. Install a short, non-polar column such as the Varian test column, 03912300-30 (packed, COLUMN, 1/8" X 50 CM 5%, OV101) or CP887098
(capillary CP-Sil 5 CB, 4M X .32). If you use a different type of column, you
should adjust conditions accordingly.
a Nitrogen will prolong the bead life time and performance.

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Page: 307
3. Set gas flow rate (should be measured at the flame tip):

Air
175 mL/min.
Hydrogen
4.0 mL/min.
Carrier gas (+ make-up)
30 mL/min.
4. Set temperatures:
Packed Column
Capillary Column
Injector
Detector
175 C (isothermal).
80 C (1 min), 20 C/min to 200 C (2 min).
230 C.
300 C.
5. Set the initial Column oven temperature. Set the desired Injector
temperature to which your TSD column is connected. Check that the
Injector oven power is ON. Detector temperature is set by pressing the
key, selecting the TSD, setting the temperature to 300 C
DETECTOR
and turning the Oven Power ON. Leave the Electronics and beadcurrent
OFF at this point. Set the detector to range 12 and AUTOZ. unchecked.
6. Allow the TSD detector to reach temperature and allow the bead to
thermally equilibrate for at least 15 minutes prior to turning on the
electronics.
7. Set the initial Autozero OFF. Set the bead current to 3.100 A. Turn on the
Bead Power. Allow the bead to condition for at least 15 minutes.
8. Increase the bead current in steps of 0.100 Ampere, waiting at least 15
minutes for the bead to equilibrate between increases. When increasing the
bead current causes the TSD Signal to go above 64 mV, the bead has
reached its ignition point. Allow the bead current to remain at this setting for
a minimum of 12 hours (preferably overnight). This completes the initial
conditioning of the TSD bead probe. Now optimization of the bead probe for
N/C selectivity is required.
The Clear Autozero button removes the Autozero offset so that you can
observe the detector background signal.
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Optimization of the TSD Using the Varian Test Sample

The sensitivity of the TSD is highly dependent on bead temperature and the
selectivity is dependent on hydrogen flow. In addition, there are slight variations
from bead to bead and a bead changes slowly as it ages. Therefore, optimum
operating conditions for a given TSD cannot be specified exactly; the user
should determine optimum operating conditions for the application and TSD
bead.
The detector responds to both nitrogen and phosphorus. It is not possible to
significantly change the relative response of nitrogen to phosphorus.
Determining Optimum Hydrogen Flow
Although a nominal hydrogen flow of 4.0 mL/min is suggested, the nitrogen-tocarbon selectivity versus hydrogen flow often differs slightly from bead to bead.
Consequently, for each new bead it is useful to chromatograph the detector test
sample at several values of hydrogen flow (from 4 to 5.5 mL/min) to determine
the best hydrogen flow for that bead.
1. Zero the TSD signal. Inject 1 L of TSD test sample (82-005048-04). A
normal response will result in the bead quenching during the solvent peak
(i.e. a negative deflection of the pen will occur) and a positive response for
the azobenzene, heptadecane, methyl parathion and malathion peaks.
Adjust the detector range to keep the peaks on scale.
2. If the azobenzene peak (see the appropriate chromatogram below) is less
than 3 times the height of the heptadecane peak, decrease the hydrogen
flow rate (in small steps) and re-inject the sample. If injection of the test
sample results in quenching by the solvent peak and the bead fails to reignite, simply increase the bead current slowly (use small steps), with
intervening pauses of ~15 minutes, until the bead re-ignites. Then repeat
step 1.
3. Over the next few days, the background current of the bead will decrease
and the sensitivity will also decrease to a steady level. At this point the
sensitivity of the bead will remain relatively constant, with low baseline drift
and low noise.
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User Manual 450-GC
Page: 309
1. Azobenzene:
2 ng Azobenzene contains 310 pg nitrogen
2. Heptadecane:
4 g heptadecane contains 3.4 g carbon
3. Methylparathion:
Capillary Column
Packed Column
4. Malathion:
4 ng Malathion contains 380 pg phosphorus
Figure 52: Structure of Components in the TSD Test Sample & Chromatogram examples
Maintaining Optimum Conditions

If the detector is used daily, the power to the bead may be left on when not in
use at 2.4 to 2.6 Amps. As the bead ages, it will require a higher current to
maintain a given bead sensitivity. Therefore, detector background signal should
be checked every few days. Eventually sensitivity will be lost and it will be
necessary to replace the bead (03-906074-01 conditioned or 03-906074-00
UNconditioned). The hydrogen flow does not need to be changed during the
lifetime of a bead.
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Column Bleed
To minimize contamination of the detector by column bleed, all new columns
should be conditioned before they are connected to the detector. Condition new
columns for a minimum of 24 hours at 40 C (or 2 hours at maximum analysis
top) below the maximum temperature of the column packing liquid phase.
Since the TSD detects compounds containing nitrogen or phosphorus, column
packing materials containing these elements should be avoided. Common liquid
phases containing nitrogen are OV-225, OV-275, FFAP, XE-60 and TCEP. If
you must use such columns, it is important that they be well conditioned and
operated at as low a temperature as possible in order to minimize column
bleed. High column bleed produces high background signals, making it difficult
or impossible to set the bead current and can result in the occurrence of
negative peaks in the chromatogram.
Solvent Considerations
When the TSD is used for trace level analysis, only solvents free of nitrogen,
phosphorus, sulfur, or halogenated compounds should be used. Depending on
the volatility of the impurity in a solvent, it can produce excessive solvent tailing
or extraneous chromatographic peaks.
Chlorinated Solvents
Chlorinated solvents can be used with the TSD. However, these solvents
generally cause an abrupt increase in both detector background signal and
sample response. These effects appear to be associated with a temporary
adsorption of chlorinated species onto the surface of the hot alkali-ceramic
bead. Repetitive injections of samples in chlorinated solvents yield constant
responses. However, once the injection of chlorinated solvents is stopped, the
background and sample response will decay back to the response levels that
existed before the initial injection of the chlorinated solvent. Therefore, when
chlorinated solvents are used, calibration standards should be run frequently.
You can minimize the effect of chlorinated solvents on the bead by turning off
bead current during the time that the solvent elutes, using the time
programming table of the detector method. The total time that the bead is
turned off should be less than 2 minutes in order to minimize thermal reequilibration times of the detector. (Any peaks eluting during this off time will not
be measured.)
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User Manual 450-GC
Page: 311
Effect of Silylation Reagents

Silylation reagents affect the TSD in 2 ways. First, such reagents sometimes
contain nitrogen which will cause tailing of the solvent peaks. Second,
decomposition of the reagent on the hot bead produces SiO2 which deposits on
the bead surface causing loss of response. Generally, SiO2 deposits can be
removed by cleaning the bead and usually produce no permanent damage to
the bead.
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TSD Assembly
It may be necessary to remove the TSD detector components for inspection,
cleaning, parts replacement, or installation of another detector. Disassembly/reassembly instructions are detailed below for both the TSD and the detector
oven.
Exploded view
1
2
3
4
5
16
17
18
8
19
9
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
---
Screws, 8-32 x Fillister head (1214200804)

TSD Top Clamp (800022900)
O-ring (2740928202)
Tower Screws, 8-32 x 3 (391866301)
Upper Insulator (2100003100)
Collector Tube (390607900)
Ceramic Insulator (2100003200)
Tower Top Plate (3400073100)
Detector Tower Body (390607700)
Flame Tip, 0.010 in. Standard Tip (200193800)
Ferrule: Vespel (100%) max. 350C (CR212200)
Graphite/Vespel 40/60 max. 400C (CR213200)
Graphite (100%) max. 450C (CR211200)
Aluminum Seal Washer (1500334701)
Detector Base (392547501)
Column Ferrule
Column Nut (394955100)
Signal Cable (200187700)
TSD bead cable (392548801)
TSD Signal Probe (390607600)
TSD bead, unconditioned (390607400)
, conditioned (390607401)
Flow Tube (200187600)
Varian, Inc.
10
11
12
13
14
15
Figure 53: TSD Exploded View
User Manual 450-GC
Page: 313
TSD disassembly
1. The TSD is mounted on the ion detector base in the detector oven.
2. Turn the TSD Oven Power and Bead Power OFF. Allow the detector to cool
to ambient temperature.
3. Turn off the main GC gas supplies to the detector at the pneumatics panel.
4. Disconnect the signal and the igniter cables from the TSD tower.
5. Remove the 2 tower mounting screws and lift the detector tower vertically
from the detector base until clear of the flame tip. Remove the 2 screws
from the top clamp.
Use clean cotton gloves or tweezers when handling internal parts of

the TSD.
Avoid contamination of ceramic insulators and probes. If the detector
is not completely cool, use a metal tool (such as tweezers or a
hooked wire) to remove parts from the tower assembly.
6.
Remove the upper insulator.
7. Remove the signal probe. There may be some resistance to removal, due
to the O-ring seals. Do not rotate probe as it is withdrawn from electrical
contacts in tower.
8. Remove the collector and the lower insulator with tweezers.
9. Remove the bead probe. There may be some resistance to removal, due to
the O-ring seals. Do not rotate probe as it is withdrawn from electrical
contacts in tower.
10. Carefully remove the flame tip assembly from the detector base.
11. Remove and discard the aluminum seal washer from detector base. In
some cases this washer may remain in the detector tower. If so, be sure to
remove and discard this washer so that the detector is not accidentally
reassembled with both the old washer and a new washer.
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TSD Re-assembly
Refer Figure 53 for re-assembly orientation.
1. Re-assembly is the reverse of removal.
2. Install the flame tip in the detector base. This is a 0.020-inch ID ceramic
flame tip. The TSD and FID flame tips are identical. DO NOT use a
0.010-inch flame tip for the TSD.
a. If you are installing the flame tip assembly with a used Vespel
ferrule, tighten the assembly finger-tight plus an extra 1/6-turn.
b. If you are installing the flame tip assembly with a new Vespel
ferrule, tighten about 1/3-turn past finger-tight.
3. The Vespel ferrule supplied with the GC has a maximum temperature limit
of 350C. If it is ever necessary to operate the detector above 350 C,
replace the Vespel ferrule with a graphite ferrule.
4. Install a new aluminum seal washer onto the shoulder of the detector base.
For a reliable tower seal, use a new aluminum washer each time the
detector is installed.
5. Measuring the nominal 4.0 mL/min H2 flow for the TSD may be simplified at
this time by attaching a tube to the flame tip and then connecting the tube
to a flowmeter. Make sure the makeup gas is turned of and adjust the
hydrogen flow.
6. Replace the detector tower on the detector base and secure with the 2
screws. Tighten screws alternately as tower is tightened into place.
Handle the ceramic insulators and probes with tweezers to avoid

contamination. Use care when handling to make sure bead probe is not
bent or dropped, as the ceramic bead on the probe is fragile.
7. Carefully insert bead probe into lower arm of detector tower. Align probe
key with tower arm slot.
8. Secure bead probe by tightening knurled nut.
9. Insert lower insulator with shoulder down into detector tower, then insert
collector tube with grid down. Make sure the punch mark on the top edge of
the collector is toward the probe arm.
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User Manual 450-GC
Page: 315
10. Insert signal probe into upper arm of detector tower. Carefully align the
spring clip with the collector. Be sure the key on the probe and the tower
arm are aligned. Secure signal probe by tightening knurled nut.
11. Assemble the upper insulator and top clamp over the collector. The O-ring
will provide slight resistance to complete insertion. Take care not to tear the
O-ring or the tower will not seal properly.
12. Look down the tower assembly to verify that the bead does not touch the
collector. Carefully adjust the collector as necessary.
13. Assemble the top clamp to the tower and secure with the 2 screws.
14. Connect the signal cable to the signal probe (top) and the igniter cable to
the bead probe (bottom). If cables were totally disconnected from the GC,
reconnect signal cable and the bead current supply cable at the top of the
TSD Electrometer Board.
1
2
3
4
5
Collector with Screen Bottom

Ceramic Bead with Heater Coil
Flame Tip
Bead Probe
Signal Probe
Figure 54: TSD Cross-Sectional View
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Varian, Inc.
MAINTENANCE
Cleaning / Maintenance
When the TSD exhibits low sensitivity or high background noise, cleaning is
indicated. Visual inspection may also indicate a need for cleaning. The ceramic
bead, collector, or flame tip are all parts that are deposit prone, depending on
the type of samples being used. Clean these parts as indicated in the following
paragraphs.
Always handle detector components with tweezers to avoid
contamination.
Bead Cleaning
Non-volatile deposits can be removed from the bead by gently scraping the
bead surface with a sharp tool or abrasive paper. The bead should be
supported while being cleaned to prevent bending the lead and cracking the
ceramic coating on the leads.
Flame Tip and Internal Parts Cleaning

Follow the steps below to clean the flame tip and internal parts.
Use proper eye and skin protection. Methanol and

acetone are toxic and flammable chemicals. Exercise
appropriate precautions when these chemicals are used.
1. Remove the detector and internal parts. Handle internal parts with tweezers
and place on a clean, uncontaminated surface.
2. Clean deposits from the surface of the collector with water or abrasive
paper.
3. Remove deposits which form on top of the flame tip by scraping. If flame tip
is plugged, clear by inserting wire (approximately 0.012 inch diameter) into
flame tip orifice.
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User Manual 450-GC
Page: 317
4. Flush cleaned components with methanol and air dry.
Replace the Flame-Tip Ferrule

After a period of prolonged use, the flame-tip ferrule may deteriorate and crack.
As a consequence, a leak may develop around the base of the flame tip
assembly that causes unstable baseline noise and reduced sensitivity. In this
situation, or when the detector is to be operated at temperatures above 400 C,
you must replace the ferrule. Be sure to select the proper ferrule for the
application. The Vespel/graphite ferrule has a maximum temperature limit of
400 C see Figure 53 on page 313.
Test Chromatogram
For an FID test chromatogram see section Detector Test Chromatograms,
on page 421.
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Thermal Conductivity Detector (TCD) - Detectors
THERMAL CONDUCTIVITY DETECTOR (TCD)
A TCD detector consists of an electrically-heated wire or thermistor. The

temperature of the sensing element depends on the thermal conductivity of the
gas flowing around it. Changes in thermal conductivity, such as when organic
molecules displace some of the carrier gas, cause a temperature rise in the
element which is sensed as a change in resistance. The TCD is not as sensitive
as other detectors but it is non-specific and non-destructive.
The Thermal Conductivity Detector (TCD) is mounted directly above the column
oven on the 450-GC. The TCD electronic Board is installed in the electronics
cabinet on the left side of the instrument.
TCD operating parameters are set at the 450-GC Display/Keyboard: These
include carrier gas type, detector temperature, range, temperature limit and
filament temperature. The gas flows are set and controlled either from the 450GC Display/Keyboard (if detector EFC is installed) or at the pneumatics panel.
Varian, Inc.
User Manual 450-GC
Page: 319
Detectors Thermal Conductivity Detector (TCD)
Before Operating the TCD

Do not operate the TCD until you have connected carrier gas to both inlets of
the TCD. The TCD accommodates 2 columns (a column for the reference cell
and a column for the detector cell) or a column and a reference line. The
columns can be packed or capillary columns and you can combine a capillary
column with a packed column. To avoid contaminating the detector, condition
all columns before you connect them to the TCD.
Initial Set-Up
To set up the TCD, proceed as follows:
Note that the TCD is a 2 channel detector and requires both a sample flow of
carrier gas and a reference flow of the same gas. Either channel can be used
as the sample stream but there must always be a reference stream.
There are TCD parameters which need to be set before using the TCD for
analysis. These are the choice of carrier, make-up and reference gas and the
filament temperature limit.
1. Refer to the Pre-installation Instructions for additional information on gas
2. Check the gas supply pressures. Flow controllers with turn dials are
calibrated for Helium at 80 psig. Recalibrate the flow controllers if you use a
different supply pressure or carrier gas.
key on the 450-GC Display/Keyboard. Select the
3. Press the SETUP
TCD by location. Select the carrier, Make-up gas and TCD oven
temperature limit. Press OK.
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key on the 450-GC Display/Keyboard. The
TCD should be listed in Position Front ( ), Middle ( ) or Rear ( ).
5. Set the detector and filament temperature limit and time-constant. To

protect the filaments, always operate the detector with the 390 C limit
selected unless you require the maximum dynamic range available to the
TCD.
6. Establish carrier gas flow through the Sample (right) side of the TCD and
an equal Reference gas flow through the Reference (left) side of the
detector. If you are using a capillary column, the total of column flow and
makeup flow should equal the Reference gas flow. Perform a Leak Check
on both the Sample and Reference pneumatics before proceeding to apply
power to the TCD filaments. Even a small leak can supply enough oxygen
to cause filament oxidation and consequent baseline drift.
Varian, Inc.
User Manual 450-GC
Page: 321
TCD Adjustments
With prolonged use, the filaments slowly oxidize and their resistances increase.
At some point this will cause the largest peaks in your chromatogram to
become flat topped, indicating that the filament protection software has been
activated. (Note that if the TCD signal is sufficiently large the output may go to
zero and become unresponsive. If this occurs, adjust your injection site and
conditions to avoid over range conditions.) To adjust for this increase in
resistance, set the Filament Temperature Limit to 490 C, even for filament
temperature setpoints below 390 C.
The TCD filament is automatically protected in the GC. The GC turns off the
filament current after 4 minutes if it detects that the carrier gas flow has stopped
or that the filament current is low. Also, the GC turns off filament current when it
detects that carrier gas is flowing through one side of the detector cell but not
through the other (e.g., a septum or column is not installed, or a leak exists in
one cell and not the other).
If you select Helium or H2 as the carrier gas, the GC operates in the standard
way to protect the TCD filament. However, because the filament protection
feature in the GC operates through the detection of air (or N2) in the detector
cells, the filament protection feature is disabled when you use nitrogen or argon
as the carrier gas.
Set the Filament Temperature Limit to 390 or 490 C, according to the highest
filament temperature setpoint required. With the Limit set to 390 C, the
maximum filament temperature is limited to approximately 450 C. The
temperature limit is approximately 550 C at the 490 C setting. The 450 C
limit protects filaments from oxidation when exposed to air over an extended
period of time. However, at the 550 C temperature limit the filament can
degrade after only a few minutes.
If you select N2 / Ar as the carrier gas, the filament protection feature is

disabled. Because the GC does not turn off the filament current, the TCD
filaments can rapidly oxidize if you operate the TCD filament
temperature above 390 C without carrier gas flowing through the TCD
cells. If you plan to operate the TCD after the carrier gas has been
turned off, purge the air from the TCD cells with carrier gas for 5
minutes before operating the TCD.
The TCD can be used with 2 different types of EFC. The EFC14 provides
make-up flow to one channel of the TCD and reference flow to the other
channel for Helium, Argon or Nitrogen as carrier gas. The EFC16 is used
for operating the TCD with hydrogen as carrier gas.
Page: 322
User Manual 450-GC
Varian, Inc.
Operation
To operate, the TCD requires only carrier gas. Helium, Argon or Hydrogen (only
with special EFC16) are recommended as carrier gases. You can use nitrogen
as a carrier gas, but you may lose some sensitivity and see an increase in the
detector noise.
If hydrogen is used as a carrier gas, vent the hydrogen from

the TCD to a safe place. Hydrogen is very flammable.
Assume that the analytical column is attached to the right side of the TCD and
the reference column or reference gas supply to the left side of the TCD.
However, you can configure the GC with the analytical column connected to the
left side of the TCD, simply reverse the TCD polarity.
If you plan to operate the TCD after the carrier gas has been turned off
for an extended period of time, turn on the carrier gas for 5 minutes
before turning on the filament current to purge air from the system. This
prevents oxidation of the TCD filaments.
At the factory, the carrier gas flow rate for TCD is set at 30 mL/min. (Carrier
gas: He) through both sides of the detector. The carrier gas flow rate is
adjusted at the pneumatics cabinet or the Detector page of the display and
measured at the 2 exit ports on the TCD. Once the carrier gas is flowing
through the TCD, set up the TCD for operation as follows:
1. Set the TCD oven to the desired temperature and allow it to come to the
setpoint. Usually, set the TCD temperature at least 20 C higher than the
maximum temperature the column oven reaches in your analysis.
2. Set TCD filament temperature. A filament temperature 50C above the
detector temperature should provide a good starting point for most
applications. After the TCD oven reached its set temperature, turn the TCD
Electronics ON to begin heating the filaments.
3. Allow system to equilibrate 10 to 15 minutes.
4. Monitor the filament current through the detector status display. Initially, the
current is higher than the final operating current. Gradually, however, the
current decreases as the detector thermally equilibrates. For best
performance of the detector, do not permit the filament temperature to
exceed the detector temperature by more than 200 C. Generally, use the
lowest detector current possible for the sensitivity your application requires.
Varian, Inc.
User Manual 450-GC
Page: 323
5. Un-check AutoZ. (Autozero OFF). Press the Autozero button to set the
initial signal to 0. Monitor the detector signal. A continuous drift, either
positive or negative, may indicate an air leak in either the carrier or
reference gas stream.
6. Note that it is normal for the TCD baseline to drift until the detector
thermally equilibrates. The time it takes to reach equilibrium always
exceeds the time it takes for the detector oven to reach its temperature.
When the baseline is stable, you can begin your analysis. Check the AutoZ.
(Autozero ON). Autozero is automatically disabled when the GC method is
in RUN.
The Autozero button applies an immediate zeroing of the detector signal.

The Clear Autoz. button will clear the autozero.
Time box allows time programming events such as range, autozero and polarity
changes.
Initial Autozero = YES allows the system to balance the bridge automatically
before each run for maximum dynamic range. The current status of the balance
control, from -99 to +99%, is shown on the display.
A continuous drift in the balance value over time may indicate you have an air
leak which is causing one set of filaments to oxidize, changing their resistance
and unbalancing the detector bridge.
Page: 324
User Manual 450-GC
Varian, Inc.
If you inject a standard or sample into the reference side of the TCD, peaks
appear in the negative direction. If you want to integrate or process these peaks
with a data system, you must convert the polarity of the peaks from negative to
positive. Use the checkbox Polarity.
Use the time program when you would like the polarity to be automatically
reversed during a chromatographic run.
Range Setting
Use the 0.05 mV range in the following cases:
Low currents (100-150 mA).

High Currents (300 mA).
Output Signal Fed to Computer or Integrator.
Low Currents (100-150 mA)

Analyses that required a high filament current and a less sensitive range can
often be performed also better at lower currents and a more sensitive range.
For example, a filament current of 120 mA and a range of 0.05 mV yields about
the same output signal as a filament current of 300 mA and a range of 0.5 mV.
At the lower current, the detector noise is lower, the stability is higher and the
filament lifetime is extended. Thus, Varian recommends that, whenever
possible, you operate the TCD at the lowest practical filament current.
The chromatograms in Figure 55 illustrate the high sensitivity and detectivity
(18 ppm of Neon in air) that is possible with the TCD detector. Also, a
comparison of chromatogram A with chromatogram B shows that with the use
of the bridge output signal amplifier, you can obtain the same analytical results
at half the filament current, thereby extending the lifetime of the TCD filament.
The Neon peak in chromatogram C illustrates how you can use a high filament
current (300 mA) with a high amplification setting to increase the effective
sensitivity of the TCD.
Varian, Inc.
User Manual 450-GC
Page: 325
A.
Filament current: 290 mA
Filament temperature: 300 C
At 1.5 minutes, range and attenuation
changes from 2 x 0.5 mV to 128 x 5.0
mV.
B.
mV.
C.
mV.
Conditions: Carrier gas: He

Sample: Air, 2 mL
Column: 10 ft. molecular sieve 5A
30/60 mesh at 50 C
Injection: Gas sample valve
TCD oven temperature: 120 C
Figure 55: TCD Sensitivity and Amplification
High Currents (300 mA)

To obtain the highest possible sensitivity, operate the TCD at the 0.05 mV
range with a high filament current. In this configuration, TCD noise is primarily
noise derived from filament vibration and fluctuations in carrier gas flow through
the detector. However, at high filament currents, the detector is very susceptible
to air leaks into the gas lines, improperly conditioned columns, imbalanced
reference and analytical flow rates, or impure carrier gas supply, which cause
the baseline to drift. Baseline drift from any of these sources generally
increases as the absolute filament temperature increases. Therefore, operate
the TCD with as low a filament current as practical for your application.
Also, operate the TCD with the lowest filament and detector temperatures
appropriate. If possible, avoid operating the TCD with a filament temperature
greater than 390 C. To operate the TCD with filament temperatures between
390 and 490 C, set the Filament Temperature Limit to 490 C. See Figure 55
for an example of the performance of the TCD at a high current.
Page: 326
User Manual 450-GC
Varian, Inc.
Calculate Detector Sensitivity

To calculate the sensitivity of the TCD, proceed as follows:
EXAMPLE 1: Known Sample Weight
S=
P Fc
W
Where:
S = Sensitivity in mV x mL/mg.
P = Integrated peak area in mV x min.
W = Weight of sample in carrier gas in mg.
FC = Carrier gas flow in mL/min corrected to detector temp
Td Pw
Fc = Fo
1
Pa
Ta
Where:
FO = Flow rate measured at detector outlet (at ambient temperature) in
mL/min.
TD = Detector temperature in K (Kelvin).
TA = Ambient temperature in K (Kelvin).
PW = Partial pressure of H2O at ambient temperature in torr.
PA = Ambient pressure in torr.
Note:
The
flowmeter.
Pw
1
Pa
expression applies only if using a bubble
EXAMPLE 2: Known Concentration of Sample in Detector
S=
E
Cd
Where:
S = Sensitivity in mV x mL/mg
E = Detector signal (peak height) in mV
CD = Concentration of test substance in the measured
peak volume in mg/mL
Varian, Inc.
User Manual 450-GC
Page: 327
Peak volume =
Peak width at half height (in min.) x gas flow rate at detector
(in mL/min) = W h/2 x FC
Calculate Detector Detectivity
To calculate the detectivity of the TCD, proceed as follows:
Detectivity =
Adjust TCD Carrier Gas
2 Noise
Sensitivity
Flow Rates
All 450-GCs equipped with TCDs are factory tested at the flow rate listed below.
Carrier Gas:
Helium
Inlet Pressure:
80 psig
Purity:
99.999%
Column Flow Rate:
30 mL/min
Reference Column Flow Rate: 30 mL/min
MAINTENANCE
The Thermal Conductivity Detector is not user serviceable and has no
replacement parts. To condition the TCD, set the detector temperature to 350C
and allow it condition for 4 hours or overnight. The Electronics (filaments) box
must be Unchecked (switched OFF) during this procedure.
TCD Test Chromatogram

For a TCD test chromatogram see section Detector Test Chromatograms,
on page 422.
Page: 328
User Manual 450-GC
Varian, Inc.
Electron Capture Detector (ECD) - Detectors
ELECTRON CAPTURE DETECTOR (ECD)

The Electron Capture Detector contains a beta-emitting
radioactive isotope, Ni63. Users of this detector are
required by regulations of the Nuclear Regulatory
Commission (NRC) to read the radiation safety
procedures described in the Radiation Safety Manual
(03-913999-00). Manual is included with the ECD.
The electron capture detector (ECD) is a highly sensitive detector capable of detecting
picogram amounts of specific types of compounds. The high selectivity of this detector
can be a great advantage in certain applications. Compared with the FID, it has much
more limited linear response. The response can vary significantly with temperature,
pressure and flowrate.
The ECD is installed on the detector oven, directly above the column oven. The ECD
electronic Board is installed in the electronics cabinet. The electronics of the ECD are
controlled through the 450-GC keyboard, whereas gas flows are set and controlled at
the pneumatics panel and in the Adjustments section of the Method if Detector EFC is
installed.
An ECD equipped with a detector cell is included in the ECD Kit. Varian is authorized to
distribute this kit to General Licensees, as defined in the Radiation Safety Manual.
The Radiation Safety Manual(s) can be found on the CD-rom CP501425 which is
included in the ECD package.
Due to the NRC regulations on the testing, packaging and labeling of radioactive
materials, additional or replacement ECD detector cells are available only as kits.
Varian, Inc.
User Manual 450-GC
Page: 329
Detectors Electron Capture Detector (ECD)
Initial Set-up
To set up the ECD, proceed as follows. Note that when the 450-GC is first
powered up all heated zones with the exception of the column oven are
powered off and all detector electronics are turned off.
the DETECTOR screen. The ECD should be listed in Position Front ( ),
Middle ( ) or Rear ( ). If your GC is equipped with detector EFC verify the
makeup gas you will be using with your ECD.
3. Install a chromatographic column in the GC, on page 13. If the analytical

column is not pre-conditioned, use a no-hole ferrule in the detector column
nut while conditioning the column and leave the detector end of the column
loose in the oven. If the analytical column is pre-conditioned, follow the
usual procedure for column installation.
Page: 330
User Manual 450-GC
Varian, Inc.
ECD Adjustments
There are ECD adjustments which should be set before operating the detector.
Cell-Current
In order to obtain the optimum linear and dynamic ranges of response, you
must select the proper ECD cell current. Your choice of cell current depends on
the specific carrier gas that is used and the baseline signal (frequency, f0) with
only carrier gas present. One of 4 values may be selected for the cell current:
Ar/CH4 (1710 pA)

CAP (480 pA)
N2STD (290 pA)
N2HIGH (146 pA)
In addition, a Zero cell current setting is provided for convenience in setting the
cell contact potential (see below).
For normal operation with nitrogen carrier gas, use the N2STD setting. When a
greater linear range is desired, select the Ar/CH4 setting and use 90%
Argon/10% Methane as the carrier gas.
Set the switch to CAP when using capillary columns. For capillary columns, the
column bleed is low and the baseline is usually below 1 mV when current is set
to N2STD on Range 1.
You may encounter applications in which high column bleed is unavoidable
when using nitrogen as the carrier gas. In such instances, the baseline signal
may be too high. Select the N2HIGH setting in these situations.
In general, the baseline signal should never exceed 25 mV when measured on
Range 1. A value above 25 mV indicates that you have selected the wrong
reference current for the chromatographic conditions (column, phase, sample
matrix). A baseline signal above 25 mV decreases the useful linear range of the
ECD detector.
Time Constant Switch

The time constant has 2 settings: SLOW (200 msec) and FAST (50 msec). For
most applications, select the SLOW setting. For capillary applications with peak
widths at half height of less than 2 seconds, select the FAST setting.
Varian, Inc.
User Manual 450-GC
Page: 331
Setting the Contact Potential

An extremely clean ECD system can yield a contact potential that must be
nulled for optimum performance. The contact potential may vary with time and
detector temperature for several days after the cell is first put into operation,
therefore you may need to repeat this adjustment procedure daily until the
contact potential stabilizes.
Install a conditioned column and establish carrier gas and makeup flow. If the
column is not well conditioned, remove the column from the detector inlet and
cap off the inlet to the ECD. Condition the column as recommended by the
supplier, then reconnect the column to the detector. NEVER operate the ECD
cell at high temperature without a source of inert gas, either carrier gas from the
column or makeup gas. Conditioning a column connected to the ECD detector
can severely contaminate the detector, requiring a costly cleaning to restore
proper function!
1. Set the ECD detector to the desired operating temperature for your
application, typically 300 C and setting the Oven Power to ON.
2. Turn the Electronics ON and set the Range to 1 a.
3. Un-check the AUTOZ. (Autozero) box.
4. Allow the detector to come to temperature and equilibrate for several hours,
or preferably overnight.
5. Press the Clear Autoz. button.
6. Select a Cell Current of Zero.
7. Set the contact potential to -760 mV.
8. The ECD signal on the 450-GC display should read between -12.7 and 13.5 mV.
9. Increase the contact potential to +760 mV.
10. The ECD signal should increase by several mV, but may still be negative.
11. Now adjust the contact potential in a negative direction until the ECD signal
is within 0.5 mV of its original value, e.g., if the signal was -12.7 mV, adjust
the contact potential until the ECD signal reads -12.2 mV.
12. Now set the cell current to the desired value.
The Clear Autoz. button clears the previously stored detector background signal
level.
a Range 10 is the most sensitive and preferred range for analytical use. If the range is set to 1, the signal
will be attenuated with a factor 10, the signal value will be 10 times lower then range setting 10.
Page: 332
User Manual 450-GC
Varian, Inc.
ECD Operation
Observe the following procedures when operating with an ECD.
Column and Septum Bleed

The ECD can become contaminated by chemicals that bleed from columns and
septa. Such column and/or septum bleed can seriously decrease the ECD cell
current which may result in an unacceptable increase in the output signal. To
prevent such contamination, condition all columns and septa before you use
them with the ECD.
Column Conditioning
NEVER condition a column while it is connected to the ECD detector. Instead,
remove the column from the detector, cap the ECD column fitting with a nut and
a no-hole ferrule. Maintain makeup gas flow to the detector to keep the ECD
cell clean. Condition new columns for a minimum of 10 hours at 40 C below
the maximum temperature of the column stationary phase, or as directed by the
column supplier. Complete the column conditioning phase before you connect
the column to the ECD.
Column Oven and Detector Oven Temperature Selection
In selecting ECD oven temperatures, consider the following:
Varian, Inc.
The maximum permissible operating temperature of the radioactive foil is

400 C. This foil temperature cannot be reached, even when the detector
oven temperature is set to 450 C. Do not add additional insulation material
around the detector tower. Added insulation can raise the foil temperature
and reduce its operating lifetime.
A high detector oven temperature reduces the likelihood of contaminating

the foil with material bleeding from the column.
The higher the temperature of the foil, the greater the rate of migration of
the 63Ni into the backing material. Rapid migration of the 63Ni reduces the
electron flux and the lifetime of the foil.
Background noise increases with an increase in the detector and column

oven temperatures.
User Manual 450-GC
Page: 333
Use these guidelines to select the detector oven temperature:
Detector temperature should be at least 30 C higher than the maximum

column oven temperature, but not lower than 150 C.
To prevent column bleed from fouling the detector, wait for the detector to
reach its operating temperature before you increase the column
temperature.
ECD Pneumatics
The 450-GC is tested at the factory at the flow rates listed in Table 10 on page
26. Use these flow rates as a starting point. Measure the flow rate at the exit
tube of the ECD cell.
You may need to clean the detector cell periodically with carrier gas. Flow rates
for the thermal cleaning procedure are also listed in Table 10 on page 26.
Refer to the installation section for a list of gas filters recommended for packed
column or capillary applications.
Each ECD kit is equipped with a Teflon flow tube assembly. When
setting/checking the flow rate, attach the end of the flow tube with the
ferrule to the 1/16-inch OD exit tube of the ECD cell. Attach the other end
of the flow tube assembly to a flowmeter. To prevent crosscontamination between detectors, use the flow tube only with the ECD
and store the assembly with the ECD kit.
After prolonged use of the ECD detector, radioactive

contaminants may build-up on the detector cap and exit
tube. In such cases, it is possible that you could come
in contact with radioactive material when checking or
adjusting the carrier gas flow rate. Refer to Radiation
Safety Manual.
Always wash your hands after handling the top of the
ECD.
Gas
Inlet Pressure
at
Gas Cylinder
Minimum
Purity
Carrier:
N2, He, or Ar/CH4 (90:10)
150 psig
99.999%
Detector Make-Up
(capillary):
N2 or Ar/CH4
150 psig
99.999%
Recommended
Flow Rate
(mL/min)
30 (packed column)
5 (capillary
columns)
20 to 30
Table 52: ECD Gases, Pressures, Purity and Flow Rates

Page: 334
User Manual 450-GC
Varian, Inc.
Installation/Disassembly
In the ECD Kit (P/N 02-001972-00) the detector cell,
which contains the radioactive ionization source, is
fixed within the detector tower and cannot be
removed. Do not attempt to remove the cell from the
tower. Regulations for the handling of radioactive
materials strictly prohibit unlicensed disassembly.
Evidence of removal voids the warranty. Violations of
these regulations are reported to NRC.
Exploded View
1.
2.
3.
12
2
Tower Top Cover (100102300)

Tower screw (391866300)
Rebuilt ECD SPECIFIC license (200197271)
Rebuilt ECD GENERAL license (USA only 200197270)
4. Pulser Probe (200197400)
5. Pulser Cable (390837603)
6. Signal Probe (200197300)
7. Signal Cable (391783000)
8. Shim (392576801)
9. Detector Base (392547501)
10. Column Ferrule
11. Column Nut (394955100)
12. Tool (7200008100)
--- Flow Tube (200196700)
4
5
8
9
6
7
10
11
Figure 56: ECD Exploded View
Varian, Inc.
User Manual 450-GC
Page: 335
If you need to remove the detector components to inspect, clean, or replace

parts, or to install another detector, refer to the following disassembly/reassembly instructions for the ECD.
1. Cool the ECD to 50 C.
2. Remove the detector tower cap and insulation.
3. Remove the signal probe and pulser probe.
4. Insert the installation tool into the detector tower assembly (located over the
detector cell). Loosen the hex nut until the cell turns freely.
5. Remove the 2 tower mounting screws.
6. Remove the detector from the detector oven.
After removing the ECD, place the cap on the tower and place the cooled
detector and installation tool in the ECD case. Store the detector in an area that
is clean and of a low humidity. Refer to the Radiation Safety Manual for
instructions on the storage and shipping of the ECD detector.
If the ECD is to be transferred to another GC, transfer the CAUTION
RADIOACTIVE MATERIAL label to the front of the other GC as well. However,
if you removed the detector only to gain access to the detector oven and you
plan to reinstall the detector, place the ECD in a clean, uncontaminated area
and proceed to the next paragraph.
Page: 336
User Manual 450-GC
Varian, Inc.
ECD Installation
Because of the sensitivity of the ECD to oxygen, check the pneumatics
for leaks prior to its installation.
1. Turn the detector oven power OFF.
2. Remove the Detector cover and the GC Top-Cover.
3. Remove both probes (pulser and signal) from the tower arms (see Figure
56, on page 335) of the detector assembly.
Be sure both probes have been removed from the detector tower arms
before attempting to install the detector tower. If you insert the
installation tool before you have removed the probes you will damage
the probe electrode contacts.
NON-SERVICEABLE ASSEMBLY. Do not attempt to remove the cell

assembly which is fixed inside the tower.
4. Check to see whether the detector tower, base and detector cell fittings are
clean. Install the ECD shim on the detector base.
Poor metal-to-metal contact between the tower contact area and the
detector oven can produce a temperature gradient.
5. Remove the insulated detector cap.

6. Position the tower assembly on the detector base and install the 2 tower
mounting screws loosely in the tower assembly.
The tower mounting screws must not be over tighten.
7. Insert the installation tool into the detector tower assembly (located over the
detector cell). Engage the hex nut at the lower end of the cell assembly.
Tighten the cell assembly into the base to provide a leak-free seal. Do not
over-tighten.
8. Alternating between the 2 tower mounting screws, evenly tighten the tower
into place.
Varian, Inc.
User Manual 450-GC
Page: 337
9. Carefully install the signal and pulser probes in the tower arms. The signal
probe (bottom) has a twist-lock cable connector and a narrow clip to
engage the collector cylinder. The pulser probe (top) has a threaded cable
connector and a wide clip to engage the foil cylinder. Insert the probes into
the tower arms with the keys on the probes lined up with the notches in the
tower arms. If you encounter any resistance during the insertion of the
probes, check that the probes are being installed in the correct positions.
10. Install the insulated detector tower cap. The label shown is factory installed
on a detector tower registered as a General License Device or Specific
License.
Figure 57: Radioactive Caution Label General License Device
Figure 58: Radioactive Caution Label Specific License
11. Connect the pulser and signal cables to the appropriate probes of the ECD.
Refer to the designation on each cable connector.
12. Cable connections for the operation of the ECD require installation of the
ECD Electrometer Board.
13. Connect the gas supplies at the rear of the GC.
14. Replace the GC Top-Cover and the Detector cover.
Page: 338
User Manual 450-GC
Varian, Inc.
15. Install the CAUTION RADIOACTIVE MATERIAL label (P/N 31-00034700) in a location on the front of the GC that is clearly visible. This label
describes the ECD radioactive isotope and the amount of radioactivity.
Figure 59: Radioactive Caution Label
16. Return the installation tool to the ECD case. You will use this tool each time
you remove the ECD. Retain the ECD case should you need to store the
ECD or to return the detector to Varian. See the Radiation Safety Manual.
Varian, Inc.
User Manual 450-GC
Page: 339
MAINTENANCE
Chemical contaminants may deposit on the components of the detector
assembly as the ECD is operated. In many cases, you can remove
contaminants deposited on the radioactive foil or cell ceramic insulators by
heating.
Refer to the Radiation Safety Manual (P/N 03-913999-00) for detector repair,
radioactive decontamination, foil replacement and leak-test information.
Although all heated zones on the 450-GC have a potential upper
temperature of 450 C, Varian recommends that you do not operate the
ECD above 420 C. (The radioactive source temperature is less than
400 C even when the detector set temperature is 450 C).
Thermal Cleaning With Carrier Gas

Use N2 or Ar/CH4 as the make-up gas to thermally clean the ECD. Refer to
Table 10, on page 26 for flow rates.
1. Remove column from the detector, cap the detector inlet using a no-hole
ferrule (28-694590-01) and column nut (03-949551-00).
2. Confirm makeup gas is flowing out of the ECD vent tube, flow should be at
least 30 mL/min. Increase the DETECTOR TEMP to 400 C.
Do not attempt to chemically clean the source.
Submerging the cell in liquid or running a liquid
through the cell will cause radioactivity to migrate,
contaminate the exterior of the cell and damage the
insulators. The cleaning of the radioactive ECD source
can by performed only by an NRC licensee. Cleaning
of the ECD source by persons other than registered
NRC licensees is strictly forbidden by law.
AVOID FOIL DAMAGE. The carrier gas must be flowing through the
detector cell before setting the DETECTOR TEMP above room
temperature. Failure to do so may damage the radioactive foil, which
is not covered by warranty.
Page: 340
User Manual 450-GC
Varian, Inc.
3. Monitor the output signal while the detector heats to its maximum
temperature. The signal will increase initially, then gradually decrease as
chemical contaminants vaporize from the detector surfaces.
4. Allow the DETECTOR TEMP to remain at 400C until the signal reaches a
stable level. A stable signal indicates that the foil has been cleaned as
much as it can be by this method.
5. Set the detector at normal operating temperatures and flow carrier gas
through the detector overnight. Check and readjust the Contact Potential
setting if necessary.
6. If the performance of the detector is not restored by these cleaning
methods, refer to the Radiation Safety Manual (P/N 03-913999-00) for
information on replacement of the foil.
Varian, Inc.
User Manual 450-GC
Page: 341
Page: 342
User Manual 450-GC
Varian, Inc.
Pulsed Flame Photometric Detector (PFPD) - Detectors
PULSED FLAME PHOTOMETRIC DETECTOR (PFPD)
Description
The Pulsed Flame Photometric Detector (PFPD) is the newest member of the
family of flame-based gas chromatographic detectors. The PFPD operates in a
pulsed-flame rather than continuous-flame mode and offers a number of
significant improvements over the conventional flame photometric detector:
Increased detectivity.
Increased selectivity (relative to hydrocarbons).
Decreased hydrogen and air consumption.
Basic Components of the PFPD
Varian, Inc.
PFPD assembly.
PFPD electrometer board.
PFPD pneumatics.
User Manual 450-GC
Page: 343
Detectors Pulsed Flame Photometric Detector (PFPD)
Features of the PFPD Assembly
Figure 60: PFPD Assembly
Page: 344
User Manual 450-GC
Varian, Inc.
Item
Description
Function
Igniter coil assembly
Provides the heat that ignites the flame.
Photomultiplier tube (PMT)
Igniter cap
Detector tower
Quartz combustor
Detector base
Light pipe
Combustor support
Combustor support seal
10
Hydrogen-air center flow inlet
11
Hydrogen-air wall flow inlet
12
Air2 inlet
13
Crunch washer, upper
14
Crunch washer, lower
15
Allen screws, 9/64"
Secures the igniter cap to the detector tower.
16
Allen screws, 8/32 x 1-1/2"
Secures the detector tower to the detector base.
17
Phillips-head screws, 8/32 x 3/8"
Secures the photomultiplier tube assembly to the

support bracket.
Varian, Inc.
Converts the photons emitted in the flame into a current

for measurement.
Holds the igniter coil and minimizes reflected light from
the igniter coil.
Supports the optics, quartz combustor tube and igniter
cap.
A transparent inert surface that contains the column
effluent for combustion and the transmission of emitted
light.
Holds the detector tower and secures the
chromatographic column to the detector.
Carries light from the combustion region toward the
optical filter and photomultiplier tube.
Holds and positions the quartz combustor within the
detector tower.
Seals the space between the combustor support and
detector base.
Hydrogen-air mixture enters here and flows up through
the center of the quartz combustor.
Hydrogen-air mixture enters here and flows along the
outside wall of the quartz combustor and into the igniter
chamber.
Air2 enters here and mixes with wall flow.
Seals the space between the igniter cap and detector
tower.
Seals the space between the detector tower and
detector base.
User Manual 450-GC
Page: 345
Features of the PFPD Electrometer Board
Description
Function
J1: Electrometer input signal cable BNC connector Photomultiplier signal output is directed to the
electrometer board through this BNC connector.
J2: Photomultiplier tube high voltage cable TNC
High voltage source on the electrometer board is
connector
directed to the photomultiplier tube through this
TNC connector.
J3: Igniter cable Molex connector
Current to the igniter coil is directed through this
Molex connector.
SIGNAL (TP1): Test point
With an oscilloscope, used to set the Gate Width
and Gate Delay.
TRIGGER (TP2): Test point
Used to monitor the gate trigger (threshold).
GATE (TP3): Test point
Used to monitor when the integration period
(Gate Width) begins.
J4: Top
These are the same signals provided at TP1, TP2
and TP3, organized to provide easy connection to
Signal
a cable. Used to connect to the PFPD Analytical
Trigger
Software.
Gate
Ground
Theory of Operation of the PFPD

By limiting the flow rates of air and hydrogen to approximately one tenth those
typically used in an FPD, the PFPD achieves substantial improvements in both
detectivity and selectivity. At these low flow rates, a continuous flame cannot
exist.
Instead, the combustor and igniter chambers fill with the combustible mixture of
air and hydrogen. When this mixture enters the igniter, the mixture ignites and a
flame front propagates back through the combustor, terminating when the flame
reaches the combustor support.
The detector then refills with the combustible mixture and the process repeats.
Page: 346
User Manual 450-GC
Varian, Inc.
Stages of Flame Pulsation

The flame in the PFPD pulses because the flow rates of hydrogen and air will
not sustain continuous combustion. Flame pulsation involves 4 stages:
Varian, Inc.
Fill: Air and hydrogen mix and enter the combustion chamber at two points.
Part of the combustible gas stream mixes with the column effluent and
moves upward through the interior of the quartz combustor tube. A second
part of the gas stream sweeps along the outside of the quartz combustor
tube and into the igniter chamber.
Ignite: The igniter chamber contains a continuously heated igniter coil.

When the combustible gas mixture reaches the heated coil, the mixture
ignites.
Propagate: The flame front propagates downward into the combustion

chamber. At the bottom of the combustion chamber, the flame extinguishes.
During this propagation phase, the sample molecules in the flame are
broken down into simpler molecules or atoms.
Emit: During and after flame propagation, the sample atoms of interest
undergo further reaction to form electronically excited species, from which
light is emitted. The flame background emission is complete within less
than 3-4 milliseconds after propagation, whereas phosphorus and sulfur
molecular species emit over a much longer time. This difference in
emission times yields the enhanced detectivity and selectivity of the PFPD.
User Manual 450-GC
Page: 347
How Does the PFPD Achieve its Greater Detectivity and Selectivity?
The enhanced detectivity and selectivity of the PFPD are a consequence of two
main factors:
Separation (in time) of the specific element emission from the background
emission.
Concentration (in time) of the emitted light.
Background Emission in a Pulsed-flame

Like the conventional FPD, the PFPD utilizes an air:hydrogen flame. Hydrogenrich flames favor a variety of gas phase chemical reactions, some of which yield
molecular products that emit light (e.g., chemiluminescent reactions). Important
excited combustion products include CH*, C2* and OH*. The light from such
combustion products is referred to as the background emission. Hydrogen-rich
air:hydrogen flames typically yield chemiluminescence hydrocarbon
background emission in the blue region with a maximum near 436 nm.3
Time-dependence of Emission Profiles
An important advantage of pulsed-flame operation is the time-dependence of
the resulting emission profiles. Flame pulsation enables the molecular
emissions of sulfur- and phosphorus-containing compounds to be separated or
resolved in time from the flame background emission itself. This resolution is
possible because the emission time of the flame background is much shorter
than the emission time of the excited molecular products of compounds of
analytical interest. As an example, CH* and OH* emission in a hydrogen-rich
flame occurs within the time it takes the flame to propagate through the
combustor, typically 2 to 4 msec. In contrast, S2* emission reaches its
maximum 5-6 msec after the CH* and OH* emission has ceased. This
separation in time enables the sulfur emission to be monitored when the flame
background has dropped to a negligible level. The result is a great improvement
in the detectivity and selectivity of sulfur and phosphorus detection.
Emission Profiles
The following figure shows the hydrocarbon and sulfur emission profiles as a
function of time (Cheskis, S.; Atar, E.; Amirav, A. Anal. Chem. 1993, 65, 539).
Page: 348
User Manual 450-GC
Varian, Inc.
Concentration (in time) of the Emitted Light

In the PFPD, detectivity is greater because all the emission occurs during and
immediately following the flame pulse. This increases the brightness of the
analytical signal relative to the dark current and other electronic noise. For
example, at a typical pulse rate of 2.5 Hz, all the sample eluting from the
column during 400 msec is burned in a single pulse, emitting over perhaps 10
msec. This results in a signal which is not only approximately 40 times as bright
as that from a continuous flame source, but also is resolved in time from the
interference of the flame background.
In addition to the general improvement in detectivity and selectivity as a result
of flame pulsation, a further increase in the relative emissions of elements of
interest is achieved through the appropriate choice of gas composition. As an
example, the formation of S2* is favored in cooler hydrogen-rich air:hydrogen
flames. Hydrogen content has less effect on phosphorus emission.
Separation of the Element Emission from Background Emission
The flame pulsation in the PFPD yields time as an added dimension to flame
photometric detection. Both selectivity and detectivity are improved through the
ability to:
Varian, Inc.
Resolve emissions of sulfur or phosphorus from the flame emission

background.
Resolve emissions of sulfur and phosphorus from each other.
User Manual 450-GC
Page: 349
As mentioned, the emission times in an air:hydrogen flame of such excited

molecular entities as S2* or HPO* are generally much longer than the emission
times of species responsible for the background emission (e.g., CH*, C2* and
OH*). This delay allows the sulfur or phosphorus emission to be integrated after
the flame background has dropped to a negligible level. The result is a lower
overall noise level and thereby greater detectivity.
The electrometer Gate Delay and Gate Width are used to select the time period
of the emission that is to be integrated. In this way, only a small segment of the
background noise is integrated during any pulsation. For example, if the time
between pulses is 400 msec and the Gate Width is set to 20 msec, 95% of the
total background noise is discarded, which further contributes to an
improvement in detectivity.
Effect of Gate Control
The following figure illustrates the effect of Gate Delay on selectivity and
detectivity.
Page: 350
User Manual 450-GC
Varian, Inc.
Adjustment of the Gas Composition

The flow rates of air and hydrogen affect the detectivity and selectivity of the
PFPD. The total flow rates of air and hydrogen set the operating frequency (rate
of pulsation) of the PFPD. Typical operating frequency for the PFPD is near 2-4
pulses/second. The relative proportions of air and hydrogen influence the
selectivity by favoring the formation of an emitting species or suppressing the
formation of an unwanted interfering species. For example, when detecting
phosphorus pesticides in plant tissues, the use of a slightly more air rich flame
than usual will suppress formation of the interfering S2* molecule, improving
P/S selectivity.
PFPD Flow Path

The figure below shows the flow path of gases entering and exiting the PFPD.
The air:hydrogen mixture enters the PFPD at two points: around the outer wall
and through the center of the quartz combustor tube. The wall flow is used to
refill the upper igniter chamber of the detector after each pulse, while the
combustor flow mixes with the column effluent and refills the combustor. For
proper operation, the combustor should refill just slightly faster than the igniter.
The refill rates are balanced by use of a needle valve on the air:hydrogen
mixture and by the flow of Air2, which bypasses the combustor and goes
directly to the igniter.
Varian, Inc.
User Manual 450-GC
Page: 351
References
Refer to the following articles for additional information on the PFPD.
S. Cheskis, E. Atar and A. Amirav, Pulsed Flame Photometer - A novel

Gas Chromatography Detector, Anal. Chem., 65 539-555 (1993).
Amirav and H. Jing, Pulsed Flame Photometer Detector for Gas

Chromatography, Anal. Chem., 67, 3305-3318 (1995).
H. Jing and A. Amirav, Pesticide Analysis with the PFPD and a Novel
Direct Sample Introduction Device, Anal. Chem., 69, 1426-1435 (1997).
H. Jing and A. Amirav, Pulsed Flame Photometric Detector, A Step

Forward towards Universal Heteroatom Selective Detection, J. Chromatog.
A., 805, 177-215 (1998).
J. A. Jacobsen, F. Stuer-Lauridsen and G. Pritzl, Organotin Speciation in

Environmental Samples by Capillary Gas Chromatography and Pulsed
Flame Photometric Detection (PFPD) Appl. Organometallic. Chem. 11, 737741 (1997).
Amirav and H. Jing, Simultaneous Pulsed Flame Photometric and Mass

Spectrometric Detection for Enhanced Pesticides Analysis Capabilities, J.
Chromatog. A., 814, 133-150 (1998).
Specifications
Specification
Detectivity
Sulfur Performance
1 pg S/sec
Phosphorus Performance
0.1 pg P/sec
Selectivity
106 S/Carbon
NOTE: The selectivity of Sulfur/Carbon is a
function of the sulfur concentration at any
time (from 105 near its detection limit to 106
at higher sulfur concentrations).
106 P/Carbon
Linear Dynamic
Range
Drift (in 20 minutes)
103
105
10 x peak to peak noise
10 x peak to peak noise
Table 53: Specifications PFPD
Page: 352
User Manual 450-GC
Varian, Inc.
Nitrogen or Other Element Operation

The nitrogen mode enhancement to the Pulsed Flame Photometric Detector
extends the range of wavelengths available for detection of element-specific
emissions to 900 nm in the near infrared. This not only allows detection of the
nitrogen emissions between 700 nm and 800 nm, but also permits the detection
of other elements, such as tin and arsenic. Section 4 of this manual gives
details of operation in the nitrogen mode, as well as some preliminary
information on detection of additional elements.
Nitrogen Mode Specifications
Detectivity:
20 pg N/sec
Selectivity:
>105 N/C
Linear Dynamic Range:
>102
Drift:
<10X peak to peak noise in 20 minutes

Table 54: Specifications Nitrogen Mode PFPD
Varian, Inc.
User Manual 450-GC
Page: 353
Installation
Inspecting the PFPD
The PFPD is installed and tested at the factory before the GC is shipped.
Carefully inspect the PFPD. If there is evidence of damage or if parts are
missing from the PFPD or its accessory kit, please contact your nearest Varian,
Inc. subsidiary or Varian, Inc. representative.
PFPD Accessory Kit

The PFPD accessory kit (03-925190-90) contains tools (Items 1-9 below) to
disassemble the PFPD and a supply of parts used in its routine maintenance.
Item
Part Number
Qty
Description
Teflon combustor extraction device
(wide bore, 3 mm ID)
Teflon combustor extraction device
(narrow bore, 2 mm ID)
03-925180-00
03-925181-00
03-925192-00
Combustor support wrench
29-898500-00
Teflon tweezers
03-925194-04
Allen wrench, 9/64" (cleaned)
15-003347-00
15
Crunch washers (Aluminum)
03-925138-00
10
Combustor support seal (Aluminum)
88-189610-00
Teflon pipe thread tape, not shown
16-000327-00
Reducing union (flow check)
Table 55: Accessory Kit PFPD
Page: 354
User Manual 450-GC
Varian, Inc.
Please note that Item 16, Sulfur Linearization Software, is not used with the
450-GC PFPD. Several important parts for Sulfur mode include Items 10, 11
and 12 while parts for Phosphorus mode include Items 13, 14 and 15.
Item
Part Number
Qty
Description
10
03-925176-00
Quartz combustor (2 mm ID, Sulfur)
11
03-925178-00
Combustor support (2 mm ID, Sulfur)
12
03-925151-01
Filter assembly, Sulfur
13
03-925177-00
Quartz combustor (3 mm ID, Phosphorus)
14
03-925179-00
Combustor support (3 mm ID, Phosphorus)
15
03-925151-02
Filter assembly, Phosphorus
16
Software, sulfur linearization software
PFPD Diffusion Source Kit

The PFPD diffusion source kit (03-925157-00) is supplied as an option to the
PFPD.
1
5
4
3
ltem
Part Number
Qty
Description
03-925132-00
Adapter seal
03-925195-00
Permeation tube, Sulfur
03-925196-00
Diffusion source holder
03-949786-00
Spring
03-925200-00
Injector adapter Cap
88-189610-00
Teflon pipe thread tape, 1/2" (not shown)
Table 56: Diffusion Source Kit PFPD

Varian, Inc.
User Manual 450-GC
Page: 355
Installing a Chromatographic Column

The following procedure describes the installation (or reinstallation) of a gas
chromatographic column in a Varian GC equipped with a PFPD.
To ensure good chromatographic performance with the PFPD, the tip of the
column must extend 0.5-1.5 mm above the top of the combustor support.
Prepare the Column End

Item
1
2
3
4
5
Description
Capillary Column Nut
Capillary Column
Ferrule
Correct Column Cut
Incorrect Column Cut
Tools and Equipment Needed

These tools are needed to complete the following procedure.
Refer parts and supplies, on page 412.
Tungsten ceramic scorer or a scoring tool.
Magnifying lens.
Follow these steps to prepare the end of the chromatographic column for
insertion into the PFPD.
1. Before cutting the end of the column, slide the capillary column nut (Item 1)
over the fused silica column end (Item 2).
2. Install the appropriate Vespel/Graphite or graphite ferrule (Item 3) over
the column end.
Make certain that the tapered edge of the ferrule is toward the inside of the
column nut (or away from the column end).
Page: 356
User Manual 450-GC
Varian, Inc.
Typically, graphite ferrules contain sulfur as a contaminant. If you use

graphite ferrules, expect a higher background during pre-conditioning of
the chromatographic column. The background may be particularly high
when using a new graphite ferrule that has not been used and
conditioned in the past.
3. Hold the column securely between the thumb and forefinger of one hand.
Use the scoring tool to score the column once lightly about 1 to 2 cm from
the end of the column.
4. With your thumbs and forefingers, grasp the column on each side of the
score and bend the column carefully away from the score mark until it
breaks at the score mark.
5. Examine the cut with the magnifying lens to decide whether the column was
properly cut (Item 4) or improperly cut (Item 5).
If you observe small splinters of silica or bits of the outer coating on the
column end, repeat the above procedure and make a fresh cut.
If you observe a clean cut, you may use either of 2 techniques to install the
column. If you wish to visually confirm the position of the column end above
the combustor support, go to Disassemble the PFPD, below. If you would
rather not disassemble the detector, see Page 360, Insert the Column.
Disassemble the PFPD

Refer to on page 344.
These tools are needed to complete the following procedure:
Varian, Inc.
Phillips-head screwdriver.
9/64" Allen wrench.
Metal forceps.
Teflon combustor extraction device.
Teflon tweezers.
Lab tissues.
User Manual 450-GC
Page: 357
1. Turn the column oven OFF to stop the oven fan.

2. Open the column oven door and wait for the column to cool to room
temperature (or to a temperature at which you can comfortably handle the
column).
3. Turn OFF the PFPD electronics and oven power and allow detector to cool
to near room temperature.
4. Remove the Detector cover from the top of the GC.
5. Before using, thoroughly clean the 9/64" Allen wrench, 1/4" wrench, Teflon
combustor extraction device and Teflon tweezer with methanol or isopropanol. Set these tools aside on a clean lab tissue.
NOTE: Dust and dirt inside the combustor can interfere with emission
and thereby lower the sensitivity of the PFPD. Therefore, never touch
the internal parts of the PFPD with bare hands. Always use a clean lab
tissue, Teflon combustor extraction device, or Teflon tweezer to
remove or replace detector parts. Place parts on a clean lab tissue as
they are removed from the PFPD.
6. Use the 9/64" Allen wrench to remove the 2 Allen screws (Item 15) from the
top of the igniter cap (Item 3). Place the Allen screws on a clean lab tissue.
The igniter cap and Allen screws may be very hot. Wait until the igniter
cap and Allen screws have cooled or use metal forceps to remove the
Allen screws from the igniter cap.
7. Use the metal forceps to lift the igniter cap (item 3) from the detector tower
(Item 4). Place the igniter cap bottom up on a clean surface (e.g., a clean
lab tissue). The top of the quartz combustor (Item 5) is visible in the center
of the detector tower.
The igniter cap may be very hot. Wait until the igniter cap has cooled or
use metal forceps to remove the igniter cap from the detector body.
8. Gently insert the appropriate Teflon combustor extraction device into the
opening in the top of the combustor. Wait 2-3 seconds for the Teflon
combustor extraction device to seat, then lift the quartz combustor from the
combustor support (Item 8). Place the quartz combustor on a clean surface
(e.g., a clean lab tissue).
9. Use the metal forceps to remove the top aluminum crunch washer (Item 13)
from the detector tower. Discard this used crunch washer.
Page: 358
User Manual 450-GC
Varian, Inc.
Remove the Detector Tower (Optional)

If you wish to view the column insertion depth directly, or you wish to replace
the combustor support, proceed with the following steps. If not, proceed on
page 360.
1. Remove from the top of the detector tower the 2 Allen screws that hold the
detector tower to the detector base. Also, remove the screw that holds the
PMT assembly support bracket to the GC.
2. Hold the PMT assembly with one hand and the detector tower with the
other. Carefully lift the detector tower straight up from the detector base.
Set the detector tower with the PMT assembly aside on a clean surface.
3. Use the metal forceps to remove the bottom aluminum crunch washer.
Discard this used crunch washer.
4. If you are changing combustor size, remove the combustor support using
the clean combustor support wrench. Use the clean combustor support
seal extraction tool (or clean capillary pick) to remove the combustor
support seal. Replace with a new combustor support seal. Replace the
previous combustor support with the new combustor support. Snug down
the new combustor support with the support wrench but DO NOT
OVERTIGHTEN.
5. If you are visually checking the insertion depth of the column, proceed to
insert the column on page 360, ignoring the instructions regarding use of
the Column Depth Gauge.
Varian, Inc.
User Manual 450-GC
Page: 359
Insert the Column

Refer for details on page 344.
These tools are needed to complete the following procedure
Refer to parts and supplies, on page 412.
5/16" wrench.
Capillary pick or combustor support seal extraction tool.
Ceramic scoring tool.
Magnifying lens.
3 mm combustor extraction tool/Column Depth Gauge.
To Insert the Column Visually

1. Check that the capillary column nut and the ferrule (reversed) are installed
on the column as described in the manual. Check that approximately 20 cm
of the detector end of the column is free so that it can be inserted into the
detector. If you are reinstalling a used column, be sure that the burnt end of
the column is trimmed off, leaving a clean, square end.
2. Insert the column into the detector and push the column up until it is
approximately 1 mm above the end of the combustor support. Tighten the
column nut to secure column in place. Next, proceed on page 361.
To Insert the Column Using the Column Depth Gauge
To insert the column with Column Depth Gauge on page 361 and follow
instructions through step 3, then proceed as follows:
1. Check that the capillary column nut and the ferrule (reversed) are installed
on the column as described in the manual. Check that approximately 20 cm
of the detector end of the column is free so that it can be inserted into the
detector. If you are reinstalling a used column, be sure that the burnt end of
the column is trimmed off, leaving a clean, square end.
2. Insert the Column Depth Gauge into the hole from which the combustor
was removed. Insert the column into the detector and push the column up
until it begins to push up the depth gauge. Tighten the column nut gently
until a small amount of force is required to move the column. Gently apply
force to the depth gauge to push the column down until the depth gauge
Page: 360
User Manual 450-GC
Varian, Inc.
contacts the detector tower. See the following figure. Tighten the column
nut to secure the column in this position.
3. Continue with step 4 in Reassemble the PFPD.
Column Depth Gauge
Detector Tower
Column
Combustor
Support
Reassemble the PFPD

Refer on page 344.
Tools and equipment needed to complete the following procedure:
Varian, Inc.
9/64" Allen wrench.
Teflon combustor extraction device.
Metal forceps.
User Manual 450-GC
Page: 361
1. Use the clean metal forceps to place a new bottom aluminum crunch
washer (Item 14) on the detector base.
2. Hold the PMT assembly (Item 2) with one hand and the detector tower with
the other. Sight the top of the combustor support (Item 8) through the
detector tower. Keep the combustor support centered as you lower the
detector tower (Item 4) over the support.
Be very careful not to crush the end of the column.
3. Reinstall the 2 Allen screws (Item 16) that hold the detector tower to the
detector base (Item 6). Tighten the screws alternately. Note: If installing the
column with the aid of the column depth gauge, follow instructions on page
360.
4. Use the Teflon combustor extraction device (of the correct taper) to insert
the quartz combustor (Item 5).
5. Use the clean metal forceps to place a new top aluminum crunch washer
(Item 13) on the detector tower.
6. Replace the igniter cap (Item 3) on the detector tower. Use the 9/64" Allen
wrench to reinstall in the top of the igniter cap the 2 Allen screws (Item 15)
that secure the igniter cap to the detector tower.
7. Reinstall the Detector cover on the top of the GC.
8. Turn on the PFPD electronics and PFPD Oven Power. Be sure that the
detector gases are turned on. The detector may not begin pulsing normally
until the detector tower has begun to heat up somewhat. Allow the detector
to come to temperature and equilibrate for at least 15 minutes. During this
equilibration period the polyimide coating on the portion of the column
exposed to the flame is burned off, leaving a clean fused silica surface.
9. Did you install a quartz combustor with a different diameter?
Page: 362
If Yes, go to Optimizing the PFPD for instructions on optimizing the

performance of the PFPD with the quartz combustor just installed.
If No, the PFPD is ready for operation.
User Manual 450-GC
Varian, Inc.
Operation
Adjusting the Gas Flow Rates
The following procedure describes the adjustment of the flow rates of the gases
to the PFPD. If you frequently adjust the column flow rate or change the carrier
gas, you may want to calibrate the air and hydrogen flow controllers. Once the
flow controllers are calibrated, you can quickly select new flow rates and use
the optimization tables that are provided.
If the PFPD Detector EFC option is installed on your 450-GC, detector gas
flows are set by pressing the Detector key, selecting the PFPD tab.
The Split Valve adjustment is described below.
Split Valve
A split valve is used to finely adjust the flow rate through the combustor section
of the PFPD combustor. Follow these directions when adjusting this split valve:
1. Disconnect the outlet line from the needle valve and replace with a
flowmeter.
2. With Air1 and Hydrogen turned on, close the needle valve by turning the
knob fully clockwise. The flowmeter should indicate a flow of less than
1 mL/minute. If this is the case, disconnect the flowmeter and reattach the
outlet line.
3. If the flow from the needle valve exceeds 1 mL/minute, remove the knob by
loosening the set screw. Rotate the valve stem clockwise gently until the
flow from the outlet drops below 1 mL/minute. Do not overtighten the valve
stem, as the needle valve does not need to shut off completely to function
properly and overtightening can damage the delicate needle in the valve.
After making the adjustment, reinstall the knob on the valve stem and
secure with the set screw.
Varian, Inc.
User Manual 450-GC
Page: 363
PFPD Gas Flow Diagram with EFC15

Refer to the following figure when adjusting the flow rates of the gases to
the PFPD.
Page: 364
Item
Description
Air1 mass flow controller
Air2 mass flow controller
Center flow tee
Hydrogen mass flow controller
Split valve
Wall flow (H2 + Air1 + Air2)
Center flow (H2 + Air1)
Igniter cap
User Manual 450-GC
Varian, Inc.
Adjust the Gas Flow Rates

Tools and equipment needed to complete the following procedure.
Varian Intelligent Digital Flowmeter or Soap flowmeter
Stopwatch
Flow measuring adapter (1/8"-to-1/16" Swagelok reducing union)
1/4" flat blade screwdriver
For best stability of flows, flow controllers should have pressure applied
to them for at least 24 hours before adjustments are made. A moderate
flow of gas through the flow controller during this conditioning period is
also helpful in stabilizing the flow controller.
1. Turn the igniter OFF.
2. Locate the Air1 mass flow controller valve (Item 1). Note the current dial
setting. Turn Air1 OFF.
3. Locate the Air2 mass flow controller valve (Item 2). Note the current dial
setting. Turn Air2 OFF.
4. Locate the Hydrogen mass flow controller valve (Item 4). Note the current
dial setting. Turn Hydrogen OFF.
5. Install the flow measuring adapter (Swagelok 1/8" to 1/16" reducing union)
to the threaded hole in the igniter cap. Connect a 2-3" piece of tube to 1/8"
end of the union. Use Teflon thread tape to make the connection to the
igniter cap gas tight. Measure and record the column flow rate, then turn
the column flow OFF.
A Varian Intelligent Digital Flowmeter is highly recommended for this
procedure.
Be sure the igniter seal is completely leak tight before attempting to

measure flow rates. This seal can loosen due to temperature cycling
during normal operation. This does not affect detector performance, but
can lead to serious errors in setting flow rates. Tighten securely before
beginning to measure flows.
6. Adjust the Air1 mass flow controller valve until flow rate is near 17 mL/min.
Write down and save the dial setting for the Air1 mass flow controller valve.
Turn the Air1 flow controller Off.
Varian, Inc.
User Manual 450-GC
Page: 365
7. Adjust the Air2 mass flow controller valve until flow rate is near 10 mL/min.
Write down and save the dial setting for the Air2 mass flow controller valve.
Turn the Air2 flow controller Off.
8. Adjust the Hydrogen mass flow controller valve until flow rate is near
12 mL/min.
If you will be using hydrogen as your carrier gas, the total hydrogen flow
to the detector should be approximately 12 mL/minute. The flow rate set
in this step should thus be 12 mL/min minus the anticipated column flow
rate. Write down and save the dial setting for the Hydrogen mass flow
controller valve.
9. Restore the Air1 and Air2 flow controllers to the settings recorded above.
Restore the carrier gas flow to the column. Remove the flow measurement
adapter, remove any Teflon thread tape residue from the igniter cap.
Leave the flow controllers ON at all times unless you must turn them off
to re-plumb or reconfigure the gas chromatograph. If you turn the flow
controllers off for an extended period then on again, they must
equilibrate overnight before the PFPD can achieve optimum
performance.
10. Turn the PFPD and thereby the igniter ON.
Calibrating the Flow Controllers

For best stability of flows, flow controllers should have pressure applied
to them for at least 24 hours before adjustments are made. A moderate
flow of gas through the flow controller during this conditioning period is
also helpful in stabilizing the flow controller.
Tools and equipment needed to complete the following procedure. Refer to
parts and supplies, on page 412.
Varian Intelligent Digital Flowmeter or Soap flowmeter.
Stopwatch.
Flow measuring adapter (1/8"-to-1/16" Swagelok reducing union).
1/4" flat blade screwdriver.
1. Turn off the column flow. Or, if you want flow to continue to the column,
disconnect the column from the detector and use a column nut and 1/16"
no-hole ferrule to seal the detector.
2. Write down the current dial settings for Air1, Air2 and Hydrogen, then turn
off each flow controller.
3. Install the flow measuring adapter (1/8" to 1/16" reducing union). Use
Teflon thread tape to make a gas-tight seal.
Page: 366
User Manual 450-GC
Varian, Inc.
A Varian Intelligent Digital Flowmeter is highly recommended for this

procedure.
Be sure the igniter seal is completely leak tight before attempting to

measure flow rates. This seal can loosen due to temperature cycling
during normal operation. This does not affect detector performance, but
can lead to serious errors in setting flow rates. Tighten securely before
beginning to measure flows.
4. Connect the flowmeter to the adapter (Swagelok 1/8" to 1/16" reducing

union). Turn the Air1 flow controller (clockwise) until the flowmeter indicates
flow through the system. Slowly turn the Air1 flow controller (counterclockwise) until the flow just stops. Again, write down the dial setting.
It is recommended that the flow controller dial be set so that it reads zero
at this setting. Remove the knob then loosen the 2 set screws holding
the dial to the flow controller shaft. While holding the flow controller
shaft so that it does not rotate, turn the dial to 000. Retighten the set
screws and replace the knob.
5. Set the dial to 100, 200, etc. and allow the flow to equilibrate. Measure the
flow and record. When you have completed all measurements, turn off flow.
6. Repeat steps 1-5 for the Air2 and Hydrogen flow controllers.
Chart the flow rate versus dial setting so that you have a reference when
setting flow rates as suggested in Optimizing the PFPD.
7. If you removed the column prior to calibrating the flow controllers, reinstall it
now.
Varian, Inc.
User Manual 450-GC
Page: 367
Optimizing the PFPD

The PFPD is optimized to maximize:
Detectivity of Sulfur or Phosphorus.
Selectivity of Sulfur and Phosphorus to Carbon or each other.
Analytical throughput (shorten total analysis time).
Detectivity
Detectivity is the minimum detectable quantity (MDQ) of Sulfur or Phosphorus
(usually expressed as picograms of Sulfur (or Phosphorus) per second.
Detectivity is the preferred method of expressing the sensitivity of a detection
method because it includes a consideration of the Signal-to-Noise ratio.
Sensitivity alone is insufficient in that the sensitivity of the PFPD can be
increased simply by increasing the voltage of the photomultiplier tube, but the
noise increases as the signal increases, yielding little enhancement in the
minimum amount detectable.
Selectivity
An important question when optimizing the selectivity of the PFPD is, "Selective
relative to what?" In some situations, the Sulfur or Phosphorus response is
best optimized relative to Carbon (the principal background emission in the airhydrogen flame). At other times, it may be more important to optimize the
Phosphorus response relative to the Sulfur response, as when Phosphorus is
analyzed in certain plant tissue extracts that are high in Sulfur content.
Throughput
The additional selectivity of the PFPD can result in shorter analysis times and
thereby greater sample throughput. As an example, by optimizing the sulfur
response relative to hydrocarbons, the PFPD may detect fewer peaks thereby
simplifying the chromatogram and increasing the chromatographic resolution.
With greater resolution, the chromatography can be adjusted such that the
peaks of interest elute faster thereby decreasing the analysis time. In addition,
when hydrogen is used as the carrier gas, the PFPD can be operated at higher
flow rates without greatly affecting the detectivity of the method. Higher carrier
gas flow rates translates into shorter analysis times and greater sample
throughput.
Page: 368
User Manual 450-GC
Varian, Inc.
Suggested Fuel Gas Flow Rates

The following table lists flow rates for several carrier gases that are often used
in common analysis situations when operating the PFPD. Use these flow rates
as starting points when optimizing the performance of the PFPD.
Carrier Gas Flow Rate

(mL/min)
Helium
H2
(mL/min)
Air1
(mL/min)
Air2
(mL/min)
13
17
10
13
20
10
10
20
34
10
11
17
10
18
10
10
15
31
10
14
17
10
16
21
10
10
24
34
10
Hydrogen
Nitrogen
Table 57: Flow Rates PFPD
You May Not Need to Adjust Flow Rates

The difference in optimum gas flow rates between sulfur and phosphorus is
small. If you dont require the maximum sensitivity for an analysis, leave the
flow rates as they are and change only the optical filter, gate delay and
integration time, when shifting between the sulfur and phosphorus detection
modes.
Varian, Inc.
User Manual 450-GC
Page: 369
Suggested PFPD Adjustment Settings

The following adjustment settings are recommended for setup and routine
operation of the PFPD. These adjustments are accessed by pressing the
Adjustments button in the PFPD detector section of the 450-GC method.
Element
Sulfur
Gate Delay
6
Gate Width
20
Trigger
200
Phosphorus
10
200
3.5
200
Nitrogen
Optimization Criteria
Refer to the following table when optimizing the PFPD.
Page: 370
User Manual 450-GC
Varian, Inc.
To Maximize ...
Consider ...
Phosphorus
response
Install wide bore quartz combustor.
Use moderately hydrogen-rich flame.
Adjust split valve such that detector is just out of tick-tock.
Set detector temperature 300 C.
Install narrow bore quartz combustor.
Set hydrogen carrier gas flow rate to a value that is near, but
just above, the minimum of the van Deemter curve for the
column and maximum column temperature used.
Use optimum hydrogen-rich flame.
Increase Air2 to enhance ignition and flame propagation in the

hydrogen-rich flame.
Set detector temperature 200 C.
Sulfur response
NOTE: For some compounds, sulfur response decreases with

increasing detector temperature. Set the detector temperature
as low as possible while preserving chromatographic peak
shape.
Phosphorus-toCarbon selectivity
Use hydrogen as carrier gas.
Adjust split valve such that detector is just out of tick-tock, then
turn counterclockwise an additional 1/2 turn.
Detector temperature 300 C.
NOTE: The Gate Delay can be adjusted to increase or decrease

selectivity. However, as the selectivity increases, the
detectivity often decreases. Set the Gate Delay to balance
these performance criteria at levels that are appropriate to the
application. Also, the gate should be set to open (or trigger) as
close to the main peak as possible rather than before or after.
Setting the gate correctly prevents the hydrocarbon and
phosphorus responses from overlapping as the flame
propagation slows in hydrocarbon-rich flames.
Varian, Inc.
User Manual 450-GC
Page: 371
To Maximize ...
Consider ...
Sulfur-to-Carbon
selectivity
Adjust split valve such that detector is just out of tick-tock, then
adjust counterclockwise an additional 1/2 turn.
Set detector temperature ~200 C.
Increase sample amount injected (inject larger volume or more

concentrated form of sample).
The trigger level should be set to trigger on the main flame peak.
Setting the trigger level correctly prevents the hydrocarbon and
sulfur responses from overlapping as the flame propagation slows
in hydrocarbon-rich flames.
The Sulfur response is proportional to the square of the Sulfur
concentration in the flame whereas the Carbon response is directly
proportional to the Carbon concentration. Therefore, when the
amount of sample that is injected is doubled, the Sulfur-Carbon
selectivity doubles (all other parameters being equal).
Phosphorus-toSulfur selectivity
Page: 372
Use slightly hydrogen-rich flame. Increasing Air1 flow until

phosphorus response decreases by a factor of 2 will improve
P/S selectivity greatly.
Set detector temperature ~300 C.
Inject the smallest amount of sample consistent with adequate

phosphorus signal. Sulfur interference is reduced in direct
proportion to the reduction in sample size. For example, a 5
fold reduction in sample size will result in a 25 fold reduction in
sulfur interference response, but only a 5 fold reduction in
phosphorus response, for a net enhancement in selectivity of a
factor of 5.
Decrease Gate Delay and Gate Width as much as possible

while maintaining an acceptable Carbon selectivity.
Because Phosphorus emits sooner than Sulfur, a shorter Gate

Delay and Gate Width improves the Phosphorus-Sulfur
selectivity.
User Manual 450-GC
Varian, Inc.
To Maximize ...
Analytical
throughput
(decrease analysis
time)
Consider ...
Additional phosphorus/sulfur selectivity can be achieved using

the PFPD Analytical Software (03-925943-92). This option
allows you to collect the full emission profile for the
chromatogram and then post-run subtract out the sulfur
response mathematically. For additional details contact your
Varian representative.
Use hydrogen as the carrier gas at flow rates up to 10 mL/min.
Bracket only the region of the chromatogram that the PFPD

can detect and for which the detector conditions have been
optimized.
NOTE: Because the van Deemter curve for hydrogen is flat at

very high flow rates, there is little loss of efficiency as the flow
rate is increased to shorten the analysis time. The wide bore
quartz combustor permits the use of higher flow rates, but this
may not be a good choice if maximum Sulfur response is also
the objective of the application.
Effect of PFPD
temperature
Varian, Inc.
An initial detector temperature of 200 C is recommended when

optimizing the PFPD, but your sample may require a higher detector
temperature to adequately separate and detect higher boiling
sample components. The figure below shows the effect of
increasing the PFPD temperature by 100 C. The sample eluted
from the column at a column temperature of 260 C. At a detector
temperature of 200 C, the peak is broad with a slight shoulder.
When the detector temperature was increased to 300 C, the peak
sharpened and the shoulder disappeared. The higher temperature
also helps to assure uniform response for a wide range of samples.
User Manual 450-GC
Page: 373
To Maximize ...
Consider ...
200 C
300 C
Page: 374
User Manual 450-GC
Varian, Inc.
Establishing Tick-Tock
Tick-tock occurs when the combustible mixture ignites in the igniter chamber
but does not propagate into the combustor chamber because the combustor
has not yet filled with a combustible gas mixture. Optimum performance is
generally achieved when the detector is operating near, but not in, the tick-tock
mode.
Establishing Tick-Tock and subsequently the proper setting of the Air-Hydrogen
needle valve is accomplished using either the scope mode of the PFPD
Analytical Software or the procedure outlined below. The PFPD Analytical
Software is available for desktop (03-925943-92) or laptop PCs (03-92594391).
Follow these steps to adjust the gas flow rates for optimum performance of the
PFPD. This adjustment should be done with the column oven at the highest
temperature which will be used in the analysis. This will assure that the detector
will remain in the normal operating mode throughout the column temperature
program.
1. To monitor the detector baseline, connect a strip chart recorder or PC to the
detector analog output. Turn off the AutoZero function (in the Detector
section of the GC method). Set the Gate Delay to 4 msec and the Gate
Width to 10 msec. Leave the trigger level at the default value, 200 mV.
(This makes Tick-Tock easier to observe. Remember to switch back to the
desired gate delay and width settings after setting the needle valve.)
2. Adjust the gas flow rates so that the PFPD is pulsing at about 2-4 Hz
(pulses/second).
3. Adjust the Air-Hydrogen needle valve fully clockwise. This shuts off the flow
of air-hydrogen to the combustor chamber while permitting the air-hydrogen
mixture to pass around the outside of the combustor and enter the igniter
chamber. The pulse rate should increase. As the flame stops propagating
into the combustor, the detector baseline drops and becomes smoother
(less noisy).
At low column flow rates (particularly with the 3 mm combustor), there
may be enough diffusion of fuel mixture into the combustor chamber
that the baseline is not completely smooth (noiseless).
4. Slowly turn the Air-Hydrogen needle valve counterclockwise. With each turn
of the needle valve, more of the combustible mixture enters the combustor
chamber. As the amount of combustible mixture entering the combustor
chamber increases, the flame begins to propagate into the combustor
chamber. First, the flame propagates into the combustor chamber on every
third or fourth pulse and then, as the flow rate of the combustible mixture
increases, on alternate pulses (tick-tock mode) and then finally on every
Varian, Inc.
User Manual 450-GC
Page: 375
pulse. As you increase the flow rate of combustible mixture that enters the
combustor, the baseline should rise sharply and become very noisy as the
detector enters tick-tock. As the detector leaves the tick-tock mode, the
baseline will rise and then fall and become less noisy. The pulse rate will
also decrease as you pass through tick-tock, since more of the combustible
mixture is burned on each pulse as you adjust the needle valve for normal
operation.
5. Once the baseline reaches a steady value, you may adjust the needle valve
an additional 1/2-turn counterclockwise to ensure stable operation of the
PFPD. If you changed the gate delay and width, reset them to the proper
values for your analysis.
Page: 376
User Manual 450-GC
Varian, Inc.
Baseline noise changes as needle valve is opened.
Varian, Inc.
User Manual 450-GC
Page: 377
Photomultiplier Tube (PMT) High Voltage

The PFPD detector is shipped with the electrometer and detector set up for the
mode specified or the phosphorus mode, if not specified. The PMT (R647) high
voltage is set at 510 volts typically for phosphorus. For the sulfur mode, the
recommended voltage is somewhat higher, usually 550 volts. For the nitrogen
mode, 580 - 620 volts is typical, since the R5070 PMT has a lower gain. This
voltage range is also typical for S and P mode operation with the R5070 PMT.
Adjusting the Photomultiplier Tube (PMT) Voltage

The following procedure describes how to adjust the Multiplier Voltage when
changing from one mode to the other, or to compensate for aging of the PMT
over time.
1. If you have not already done so, adjust the detector gas flow rates for the
mode of operation desired (Sulfur or Phosphorus). Use flow rate values that
you determined previously or the recommended flow rates listed in the Gas
Flow Rates table on Page 369.
2. When the detector is pulsing normally, press the Detector, select the
PFPD tab,
3. If the Multiplier Voltage (PMT) voltage is:
Within 10-20 volts of the nominal value for the desired mode of
operation, you may not need to make any further adjustment.
Not within this range, enter a new PMT voltage while observing the
PFPD output on a strip chart recorder or on the Workstation System
Control display.
4. If you want to optimize the detector sensitivity with respect to PMT voltage:
Page: 378
Set up the PFPD to operate in the desired mode. Set the detector to
Range 10.
Slowly adjust the PMT setting while watching the baseline noise
(displayed on a strip chart recorder or other output device).
User Manual 450-GC
Varian, Inc.
Starting at ~450 volts, increase the PMT voltage in increments of 20 to

50 volts while observing the peak to peak noise. At low PMT voltages,
the baseline will rise with increasing voltage, but the peak to peak noise
will remain unchanged. Continue increasing the PMT voltage until the
peak to peak noise is approximately twice as great as it was at the
lowest voltage. This PMT voltage should provide optimal detectivity and
maximum dynamic range.
5. Note the PMT value displayed on the GC Detector Status display as

above.
As the PMT ages, the voltage required to generate adequate sensitivity
gradually increases. Replace the PMT when you can no longer achieve
adequate sensitivity within the range of PMT available.
Optimizing the PFPD

The PFPD can be optimized in 2 ways:
Repeated injections of standard.
Continuous infusion of standard.

These tools are needed to complete the procedure for optimizing the PFPD
using the method of repeated injections of standard. Refer to parts and
supplies, on page 412.
Flat tipped screwdriver.
Printer/plotter or stripchart recorder.
FPD test sample.
10 L syringe.
Repeated Injections of Standard

Follow these steps to optimize the PFPD using the method of repeated
injections of a standard.
1. Install the test column.
2. Set the Detector temperature to 200 C for S mode, or 300 C for P mode.
Set Injector temperature to 200 C for isothermal Injectors; 80 C initial, 0
hold, program to 200 C for 1079 PTV or 1177. Set column oven to 80 C
initial, hold 0.5 minutes, then program at 25 C/minute to 200 C and hold 2
minutes, or until the last peak of interest elutes.
3. Allow the chromatographic system to equilibrate for 1 hour.
Varian, Inc.
User Manual 450-GC
Page: 379
4. Turn the stripchart recorder or other display device ON.

5. Adjust the gas flow rates to those recommended for your carrier gas and
flow rate in the Suggested Fuel Gas Flow Rates table on Page 369.
6. If necessary, adjust the Air2 flow rate to give a flame pulse rate of 2-4
pulses/second.
7. Inject 1.0 L of the FPD Test Sample split ~20:1 if using a 1079 PTV or
1177 split injection. Inject 1 L of a 20:1 dilution of the test sample in isooctane if using a 1079 PTV or 1177 splitless or on-column injection or a
1041/1061 Injector.
8. Note the peak height of the sample peak eluting last, methyl parathion.
When the GC is Ready again, increase the hydrogen flow by 20 digits on
the counter, or 0.2-0.5 mL/min with Detector EFC inject the sample again
and note whether the peak height increases. If so, continue to increase the
hydrogen flow and reinject the sample until the peak height no longer
increases.
If the peak height does not increase by increasing the hydrogen flow, then
decrease the flow by 20 digits on the counter, or 0.2-0.5 mL/min with
Detector EFC and reinject the sample. Continue this procedure until the
methylparathion peak is maximized.
Allow the system to equilibrate for 2-3 minutes between flow rate
adjustments so that the air and hydrogen filters are completely flushed
with the new gas composition.
9. When the peak height is maximized, tune the fill time of the igniter volume
to be just slightly greater than the fill time of the combustor volume. See
Establishing Tick-Tock on Page 375.

These tools are needed to complete the procedure for optimizing the PFPD
using the method of continuous infusion of standard:
Page: 380
Sulfur diffusion source kit.
User Manual 450-GC
Varian, Inc.
Continuous Infusion of Standard

Follow these steps to optimize the PFPD response using the method of
continuous infusion of a standard.
1. Install the Sulfur diffusion source.
Disconnect the column at the Injector end. Insert the sulfur permeation tube
into the diffusion source holder, wrap the threads of the holder with Teflon
thread sealant tape and attach the Injector adapter. Tighten the cap just
enough to make a gas-tight seal.
Insert an aluminum adapter seal in the end of the Injector adapter. Check
that the crunch washer is properly seated at the bottom of the holder and
not resting on the threads. Screw the Injector adapter-end of the diffusion
source holder onto the Injector outlet fitting. Tighten the holder just enough
to make a gas-tight seal.
If the permeation tube has not been used recently, set the Injector and
column temperature to 50 C and pass carrier gas over the permeation
tube for ~1/2 hour. This decreases the surface concentration of the
permanent.
If the test column is installed, shorten the length of column extending above
the Injector nut to ~5 mm.
Insert the column into the column-end of the diffusion source holder.
Tighten the column nut as usual. The outlet of the holder uses the same
fitting as the Injector outlet except that the holder requires an insertion
depth of only
1-2 cm.
3. Set the Injector and Column temperatures to 60 C.
The concentration of standard that enters the detector is adjusted by
increasing or decreasing the Injector and Column temperatures.
However, 60 C should be near optimum for the optimization procedure.
4. Adjust the column flow rate as required (~2 mL/min for the 320 test
column). Allow the chromatographic system and permeation tube and
diffusion source holder to equilibrate for 1 hour.
5. Adjust the gas flow rates to the recommended flow rates listed in the Gas
Flow Rates table of Optimizing the PFPD on page 369. Set the detector
range to 10. Set Autozero to OFF. Adjust the attenuation to keep the
emission on scale.
Varian, Inc.
User Manual 450-GC
Page: 381
6. If necessary, adjust the Air1 and Hydrogen flow rates to give a flame pulse
rate 2-4 pulses/second. Alternately increase or decrease Air1 and
Hydrogen so that the flow rate remains approximately the same as the gas
composition is changed. Allow the system to equilibrate for 2-3 minutes
between flow rate adjustments so that the air and hydrogen filters are
completely flushed with the new gas composition.
When adjusting the flow rate, turn the Air and Hydrogen flow controller
dials in increments of 10 or 20, or make 0.2-0.5 mL/min adjustments
using PFPD Detector EFC.
7. Increase the flow rate of Hydrogen by 10 dial units. Examine the emission
on the stripchart recorder. Monitor the emission after each flow rate
adjustment. If the sulfur emission increases, continue to increase the
hydrogen flow rate until the response no longer increases. If the pulse rate
increases beyond 4 Hz, reduce the Air1 flow by 10 units and continue the
procedure. Typically, noise is relatively independent of gas composition so
that the relative gas composition can be adjusted with little or no effect on
the noise.
Sulfur emission is maximized when the gas mixture is very rich in
hydrogen.
8. Once the sulfur emission has been maximized, adjust the fill time of the
igniter volume so that it is just slightly less than the fill time of the combustor
volume. See Establishing Tick-Tock on Page 375.
9. Remove the column from the diffusion device holder, remove the diffusion
device holder from the Injector outlet and reinstall the test column or the
appropriate analytical column in the Injector.
Testing the PFPD Performance

The following procedure describes how to test the performance of the PFPD
after it has been optimized for the desired detectivity and selectivity.

These tools are needed to complete the following procedure Refer to parts and
supplies, on page 412.
FPD test sample.
10 L syringe.
Test column, DB-1 320 x 4M.
Follow these steps to test the chromatographic performance of the PFPD.
Page: 382
User Manual 450-GC
Varian, Inc.
1. Configure the GC as described below:
Column: Test column (DB-1 320 x 4M).
Injector: 1079 PTV or 1177.
Printer/plotter, stripchart recorder, or Workstation printout.
2. Select the mode (sulfur or phosphorus):
Turn the PFPD electrometer OFF.
Remove the GC Top-Covers.
Install the correct optical filter for the element of interest.
Set the Gate Delay and Gate Width for the element of interest.
Install a 2 mm quartz combustor and support for sulfur mode, or a

3 mm combustor and support for phosphorus.
Replace the GC Top-Covers and turn the PFPD electrometer ON.

3. Set the GC method (or GC Workstation method) for the following bake-out
conditions:
Oven temperature: 240 C.
Detector temperature: 350 C.
Injector temperature: 250 C.
Disconnect the test column, cap off the detector and operate the GC for at least
4 hours to bake out the column. Set the oven temperature to room temperature
and wait until the oven and column are cool. Reconnect the test column to the
detector.
4. Set the GC method (or GC Workstation method) for the following test
conditions:
Injector: 200 C isothermal or 80 C initial, 0.00 hold, program to 200

C for 1079 PTV modes.
Detector: Temperature 200 C for S mode, 300 C for P mode, Range

10, Autozero ON.
Column Oven: 80 C initial, 0.50 min. hold, 25 C/minute to 200 C,

hold 2.00 minutes, or until last peak of interest elutes.
Set PMT voltage to 510V for phosphorus or 550V for sulfur. If you are using the
R5070 (N mode) PMT, set voltage to 600V or use values obtained in on page
378.
5. Operate the GC for at least 1 hour to ensure that the PFPD and its
electronics are thermally stable. Re-optimize the PFPD as recommended in
Optimizing the PFPD on Page 368.
Varian, Inc.
User Manual 450-GC
Page: 383
6. If you are using a split injection, inject 1 L of FPD test mix with a split ratio
of 20:1. If you are using a non-splitting Injector, dilute the FPD Test Sample
1:20 in iso-octane and inject 1.0 L of the diluted FPD Test Sample.
7. The resulting chromatographic peaks should have similar retention times,
heights and resolution to those shown below.
8. Are the peak retention times substantially different?
Page: 384
If Yes, adjust the column temperature and/or column flow rate and
repeat steps 5-6.
If No, replace the test column with the column to be used in your
particular application, adjust the GC conditions to appropriate values
and proceed with the analysis.
User Manual 450-GC
Varian, Inc.
PFPD Test Chromatogram: Sulfur Performance

Refer to the figure below to check the chromatographic performance of the
PFPD for sulfur. Compare the test chromatogram to the chromatogram shown
below in terms of peak retention times, peak heights and peak resolution.
Varian, Inc.
User Manual 450-GC
Page: 385
PFPD Test Chromatogram: Phosphorus Performance

Refer to the figure below to check the chromatographic performance of the
PFPD for phosphorus. Compare the test chromatogram to the chromatogram
shown below in terms of peak retention times, peak heights and peak
resolution.
Detectivity
Refer to the instructions below to calculate the detectivity for sulfur and
phosphorus with the PFPD:
Determine the peak-to-peak noise (Np-p) on the baseline. Collect at

least 5 minutes of baseline noise at an attenuation which will allow easy
measurement of the noise.
Inject a known amount of standard (100 x noise) and determine the

peak height (H) for Sulfur or peak area (A) for Phosphorus. The
instructions above will give a methyl parathion peak which contains
120 pg of both sulfur and phosphorus.
Determine the width (W) of the peak at half-height (W) for

phosphorus, or the width at 1/4 height for sulfur. Calculate detectivity
(D) according to the formula below:
o Dphosphorus = [Wt x (2 x Np-p)]/[W x H]
o
Page: 386
User Manual 450-GC
Dsulfur = [Wt/W] x SQRT [(2 x Np-p)/H]

Varian, Inc.
Detectivity is expressed in units of weight/time. Wt is the weight of the

specific element injected (e.g., weight of methyl parathion multiplied by
0.12 for either sulfur or phosphorus). W 1.5 x W. The term SQRT
means to take the square root of the product in brackets. If you are using
peak areas or peak heights that have been calculated by a data system,
use the counts-to-mm conversion factor from the data system.
PFPD Test Chromatogram: Sulfur Detectivity

Refer to the figure below to check the detectivity of the PFPD for sulfur.
Ds = [Ws /(1.5 x W1/2)] x SQRT(2 x N/H)
where Ds = Detectivity (pg/sec) for sulfur, Ws = Weight (pg) of sulfur, W1/2 = width (sec)
at half height of sulfur peak, N = peak-to-peak baseline noise (mm), H = height (mm) of
sulfur peak, SQRT = square root
As an example, for the following test chromatogram: Ws = 120 pg, W1/2 = 2.2 sec, N = 1
mm (1 mm x attenuation of 1), H = 4992 mm (78 mm x attenuation of 64) then
Ds = [120 pg /1.5 x 2.2 sec] x SQRT(2 x 1 mm/4992 mm) = 0.73 pg/sec
Varian, Inc.
User Manual 450-GC
Page: 387
PFPD Test Chromatogram: Phosphorus Detectivity

Refer to the following figure to check the detectivity of the PFPD for phosphorus.
Dp = [(Wp x 2 x N)/(H x W1/2)]
where Dp = Detectivity (pg/sec) for phosphorus, Ws = Weight (pg) of phosphorus, W1/2 =
width (sec) at half height of phosphorus peak, N = peak-to-peak baseline noise (mm), H
= height (mm) of phosphorus peak
As an example, for the following test chromatogram: Wp = 120 pg, W1/2 = 2.5 sec, N =
16 mm (4 mm x attenuation of 4), H = 17152 mm (67 mm x attenuation of 256) then
Dp = [(120 pg x 2 x 16 mm)/(17152 mm x 2.5 sec) = 0.090 pg/sec
Using the Gate Delay and Gate Width Parameters

Through the Gate Delay and Gate Width parameters you have access to the
control functions of the gated integrator located on the PFPD electrometer
board. These control functions enable you to select the time period (or region)
of the emission spectrum that is to be integrated, thereby improving the
sensitivity and selectivity of the PFPD.
Page: 388
User Manual 450-GC
Varian, Inc.
What Can Be Controlled Through the Adjustments?

Three functions can be controlled through the Adjustments:
Trigger Level: signal required to start (trigger) the delay and width timer.
Gate Delay: time in milliseconds after triggering before integration of the

detector signal begins.
Gate Width: time in milliseconds after the Gate Delay during which the
detector signal is integrated.
The appropriate values for the Gate Width and the Gate Delay are determined
from the emission profile (time x emission intensity) of the element of interest.
Appropriate values for a number of elements are listed in the following table.
Preset and Range of the Control Functions

Refer to the table below for a description of the preset values and ranges of the
functions that can be adjusted.
Function
Preset
Range
Trigger Level
200 mV
10 - 2000 mV
Gate Delay
4 msec
0.5 - 20 msec
Gate Width
10 msec
0.5 - 20 msec
Table 58: Preset Values PFPD
For those users interested in gaining a more detailed understanding of the

PFPD emission profile, the analog detector signal, the trigger state and the
integrator gate state are available at test points on the edge of the electrometer
board and on the pins of connector J4 on page 346.
When displayed on an oscilloscope, these signals allow detailed investigation of
the emission time profiles of the flame background and of elements of interest,
so that the detector parameters may be fine tuned for optimum selectivity and
detectivity.
These signals may also be displayed and manipulated using the PFPD
Analytical Software: 1) 450-GC and Desktop PC (03-925943-92) and 2) 450GC and laptop PC (03-925943-91).
For more information on the use of these signals, please contact your Varian
representative.
Varian, Inc.
User Manual 450-GC
Page: 389
Setting the Trigger Level

These tools and equipment are needed to complete the following procedures.
FPD test sample.
10 L syringe.
The trigger level is preset to 200 mV. You may need to set the trigger level
lower if you are using a narrow band interference filter which does not transmit
much of the flame background. You may need to set the trigger level higher
than 200 mV for optimum operation with some elements which have no delayed
emission, or very short emission delay times.
To set the trigger level, follow the steps below:
1. Press the Detector key and select the PFPD you wish to adjust. Turn OFF
initial Autozero in the active method.
2. Press the Adjustments button to access the integrator parameters. Set
Gate delay to 3.5 ms. This allows the tail of the prompt flame background
emission to be integrated as a test signal. This figure shows a typical flame
background emission profile.
Trigger Level
OK
NOISY
OK
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3. Set the trigger level to the minimum and observe the noise on the detector
output using a strip chart recorder or the Star Workstation status display.
Gradually increase the trigger level. The signal level should decrease and
the noise should also decrease. Select a trigger level which gives minimum
noise. This will usually be triggering on the preliminary emission pulse.
4. If you will be detecting an element such as nitrogen, which emits very
promptly after the main flame propagation, you may get better results by
continuing to increase the trigger level until triggering is occurring on the
main background emission pulse itself. As you increase the trigger level,
the noise will increase substantially at one point. This is due to the trigger
occurring sometimes on the apex of the preliminary emission pulse and
sometimes on the main pulse. Increasing the trigger level 10 to 20% above
this point should provide very stable triggering for detection of prompt
emitting elements. This setting is also preferred when the effects of large
amounts of hydrocarbons on emission timing must be minimized. The
following figure illustrates the signal observed during such an adjustment.
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Setting Gate Delay and Gate Width

The following table contains gate delay and gate width settings which are
recommended for routine detection of common elements. Try these settings
first when setting up your PFPD to detect these elements.
Element
Gate Delay
Gate Width
Sulfur
20
Phosphorus
10
3.5
Nitrogen
Table 59: Recommended Settings for common elements
Set the Gate Delay by Repeated Injections of Standard

The appropriate Gate Delay can be determined by injecting a standard and
adjusting the Gate Delay until the required selectivity is achieved.
To set the Gate Delay by the method of repeated injections of standard, follow
these steps:
2. Set the Detector temperature to 200 C for S mode, 300 C for P mode. Set
Injector temperature to 200 C for isothermal Injectors; 80 C initial, 0.00
hold, program to 200 C for 1079 PTV mode. Set column oven to 80 C
initial, hold 0.50 minutes, then program at 25 C/minute to 200 C and hold
2.00 minutes, or until the last peak of interest elutes.
3. Allow the chromatographic system to equilibrate for 1 hour.
4. Turn the stripchart recorder ON.
5. Adjust the gas flow rates to those recommended for your carrier gas and
flow rate in the Suggested Fuel Gas Flow Rates table in Optimizing the
PFPD (Page 369). The Air2 flow rate has little effect on the detectivity of the
PFPD and can be set to 10 mL/min.
6. If necessary, adjust the Air1 and Hydrogen flow rates to give a flame pulse
rate 2-4 pulses/second.
7. Inject 1.0 L of the FPD Test Sample split ~20:1 if using a split Injector.
Inject 1.0 L of a 20:1 dilution of the test sample in iso-octane if using a
non-splitting Injector. Or, inject another sample of interest.
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8. If the desired selectivity has not been achieved, increase the Gate Delay by
0.5 msec and inject the standard to check the effect of this change.
Continue to increase the Gate Delay until the desired selectivity is
achieved.
In the case of elements which emit very near the flame background peak,
selectivity may be improved by opening the combustor flow needle valve
somewhat beyond the position determined in the procedure Establishing
Tick Tock. An increase of 1/4 to 1/2 turn counterclockwise is usually
sufficient.
Set Gate Width

These tools and equipment are needed to complete the following
procedures. Refer to parts and supplies, on page 412.
FPD test sample or other standard.
10 L syringe.
1. Set Gate Width to minimum

2. Inject an appropriate standard, calculate the detectivity for this Gate Width.
3. See: Testing the Performance of the PFPD on page 382 for instructions on
calculating the detectivity of sulfur or phosphorus with the PFPD.
4. Increase Gate Width by 1 msec, inject standard, calculate detectivity.
5. Continue to increase Gate Width as long as detectivity continues to
improve.
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Building a GC Method
The procedure for building a GC method involves 4 tasks:
Turn the PFPD electrometer on.
Set the detector temperature.
Set the range of the PFPD electrometer.
Set the gated integrator parameters.
1. Press the Detector key and select the PFPD tab.

2. Turn the detector oven ON and set the desired detector temperature.
3. Turn the detector electronics ON.
4. Select the Range you wish to use and turn on initial Autozero if desired.
You may also time program Range and Autozero functions if your analysis
requires it.
5. Enter the Gate Delay, Gate Width and Trigger Level parameters as
determined in the preceding procedures, or from the table provided.
6. If you wish to use the analog output from your detector, select one of the
Analog Output ports, enter the position of the PFPD detector you are using
(Front, Middle, or Rear) and enter an attenuation value. If the analog output
is going to a data system or integrator, an attenuation of 1 is strongly
recommended. If the output is going to a strip chart recorder, note that you
may time program the attenuation of the analog output port.
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Building a GC Workstation Method

The procedure for building a PFPD Detector section as part of a GC method
involves 4 tasks:
Turn on the PFPD electrometer.
Set the detector temperature.
Set the range of the PFPD electrometer.
Set the Gated Integrator parameters.
1. Open the method to which you wish to add the PFPD section. Select the
450-GC section and select the Detector page. Select the PFPD tab.
2. Set the Electronics and Detector Oven to ON.
3. Set the Detector Temperature to an appropriate value for your analysis.
4. Set the Range and Autozero as required. Note that these parameters are
time programmable.
5. Set the Trigger level, Gate Delay and Gate Width as required.
6. If you wish to use the Analog Output in addition to the digital signal used by
the Star Workstation, select the Analog Output page, select the output
channel you wish to use and select the PFPD position and attenuation.
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Quantitation
Quantitation with the PFPD
When using the PFPD, it is important to understand how its pulsing flame can
affect the accuracy and precision of a quantitative analysis.
As described previously, the combustor and igniter chambers of the PFPD fill
with a combustible mixture of air and hydrogen. The combustor chamber fills
with the combustible mixture at about the same time as the igniter chamber.
When the gas mixture enters the igniter, the mixture ignites and the flame
propagates back through the combustor and then extinguishes. The combustor
then begins to fill with the gas mixture and the process repeats. The rate of this
repetitive process can vary, but for optimum performance of the PFPD, you
must adjust the gas flow rates in order to strike a balance between the fill time
of the combustor chamber and the fill time of the igniter chamber. It is important
that the combustor chamber fill slightly before the igniter chamber in order to
ensure that the flame propagates completely back to the combustor chamber.
However, the combustor chamber should not fill too fast (relative to the igniter
chamber) or some of the sample exits the detector before it is combusted
resulting in poorer detectivity.
Because the PFPD pulses, the emission derived from the PFPD appears as
discrete signals separated in time. This requires electronics that are quite
different from the conventional non-pulsed FPD in which the emission signal
increases then decreases without interruption. That is, the PFPD electronics
are not sampling discrete points on the eluting peak, as in the case of a
conventional FPD. Rather, the PFPD stores the emission output derived during
each pulse and generates a peak (or waveform) that may or may not be
identical to the actual eluting peak shape, but which contains all the signal
information from the chromatographic peak.
Given these unique properties of the PFPD, there are differences between
quantitation based on the height or area of the chromatographic peaks.
Peak Area Quantitation

In general, quantitation based on peak areas is preferred because it is least
affected by the pulsing nature of the PFPD and the way the PFPD electronics
handles the resulting emission signal. Peak areas are best because once the fill
rates of the PFPD are appropriately adjusted, any sample that enters the
detector contributes to the resulting signal (i.e. all the sample that enters the
detector between pulses is combusted), no matter how narrow the
chromatographic peak.
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Peak Height Quantitation

Quantitation based on peak height, on the other hand, is less precise and
depends, somewhat, on the widths and resolution of the eluting peaks. Peak
height is determined by the pulse which contains the maximum concentration of
the eluting peak and to some extent is dependent on how well centered the
concentration maximum of the eluting peak is relative to a pulse. The
quantitative precision of the PFPD is not affected much by very narrow or very
wide peaks. For very narrow peaks, almost the entire peak is combusted in one
pulse and the resulting peak height is thereby equivalent to the total emission.
For very broad peaks, the pulsed output follows the chromatographic peak
shape. There may be some intermediate width peaks for which peak height
precision is worse, but these cases can be addressed by changing the pulse
repetition rate appropriately. For these intermediate width peaks, the peak is
eluting during 2 or 3 pulses and the position of these pulses relative to the peak
position can cause peak height to vary. Peak area is not greatly affected.
Peak Resolution with the PFPD

Higher repetition rates (up to 10 Hz) are necessary when you must resolve 2
closely spaced peaks. Higher repetition rates give the best possible peak
shape definition (at a small cost in detectivity). However, peak resolution is not
usually a problem at lower repetition rates since the number of possible sulfur
or phosphorus containing peaks is fairly small at the beginning of a
chromatogram where peak resolution is likely to be a problem.
Quantitation in the Sulfur Mode

Since the electronically excited S2 molecule is the emitting species in the sulfur
mode, the signal generated by the PFPD is proportional to the square of the
sulfur concentration in the combustor. Because it takes 2 sulfur atoms to
form each excited S2 molecule, detectivity is improved by increasing the
concentration of sulfur in the combustor by confining the emission to a
smaller volume (i.e. 2 mm combustor).
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Square Root Function

The PFPD electrometer (through a square root function) converts the quadratic
response (sulfur emission varies as the square of sulfur concentration) to a
linear response (sulfur signal varies as a direct function of the sulfur
concentration) by taking the square root of the response. The square root
function can be used for the determination of total sulfur in a hydrocarbon
matrix, for example, where individual resolved peaks may not be present and a
total area of sulfur response is needed.
Normal/Square Root setting

The square root mode is selected by the NORMAL/Square Root field. When
Square Root is selected, the output from the PFPD is the square root of the
sulfur emission. When NORMAL is selected, the output of the PFPD is not
converted or adjusted. Use this NORMAL setting when operating the PFPD in
the phosphorus mode and when the sulfur signal is to be processed by a data
system using the square root of height.
Detectivity of the NORMAL Versus Square Root Modes

In the Square Root mode, the amplifier signal is applied to the input of a square
root circuit which produces an output equal to 10 times the square root of
Vin/10. This output is linear with sulfur concentration but by the nature of the
square root function is noisy. Detectivity in the hardware Square Root mode is
often 2 to 4 times worse than in the Normal mode under the same detector
conditions.
How to Minimize Quenching of Sulfur Response

When a large amount of hydrocarbon coelutes with a sulfur compound of
interest, the sulfur response may be quenched. This quenching is the result of a
reaction of CO, formed by combustion of the hydrocarbon, with S atoms. In
some cases this quenching can be avoided by use of a more selective column
to eliminate the coelution, e.g., COS/propylene, benzene/thiophene,
toluene/methylthiophene. Use of a 3 mm ID combustor with somewhat
increased Air1 flow may also help to reduce quenching. Finally, injection of the
smallest amount of sample which gives an adequate signal to noise ratio will
minimize quenching.
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Advanced Operation
This section describes the operation of the PFPD in the Nitrogen mode,
including:
Theory of operation, describing the basis for nitrogen detection and

including suggested gas flow rates.
Installation of the nitrogen mode parts - for users who are adding the
nitrogen mode capability to an existing PFPD. Includes an exploded view of
the parts.
Nitrogen mode operation - provides some suggestions for enhancing or

modifying nitrogen mode performance.
Phosphorus mode/Sulfur mode operation - describes some changes which

may be required to detect phosphorus or sulfur using the nitrogen mode
PMT.
Spare Parts and Supplies.
Additional Elements - describes preliminary operating conditions for the

detection of the following elements: Arsenic, Selenium, Tin and
Manganese.
Theory of Operation
Nitrogen mode is based upon combustion of nitrogen containing compounds to
form NO. NO then reacts with hydrogen atoms remaining in the combustor after
the flame is extinguished to form HNO*, an electronically excited molecule
which emits light in the 700 - 800 nm range of the near infrared. Because these
emission wavelengths are beyond the range of the photomultiplier tube used in
the standard PFPD, the Nitrogen mode requires a new red-sensitive
photomultiplier and PMT holder hardware, along with an appropriate dark red
colored glass filter.
Because N mode is based on complete combustion of the sample molecule to
form HNO*, the PFPD response is much less dependent on the chemical
nature of the sample than is the TSD response, which depends on the
presence of a C-N bond in the molecule. Thus even inorganic nitrogen
compounds such as ammonia, hydrazine and nitrogen oxides are detectable by
the N mode PFPD, whereas these compounds give no response on the TSD.
The only nitrogen compound known to give no useful response on the PFPD is
molecular nitrogen, N2. Compounds such as nitroglycerin and other nitrate
esters, nitroaromatics and nitroso compounds give a somewhat enhanced
response when compared to more reduced nitrogen compounds, but the
enhancement amounts to only ~20%, so for most purposes the N mode PFPD
can be considered to give a uniform response to all nitrogen compounds, as it
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does for sulfur and phosphorus compounds. Uniformity of response may be

enhanced by increasing the oxygen flow into the combustor, at the cost of some
reduction in sensitivity.
Oxidation of nitrogen requires a hotter flame than either phosphorus or sulfur.
This is reflected in the following table of recommended flame gas flow rates. In
general, the nitrogen mode requires a more air rich flame and suffers a larger
reduction in sensitivity as carrier flow rate increases. Use of the 3 mm
combustor provides best detectivity.
Table of Optimum Flow Rates

Carrier Gas
Hydrogen
Helium
Nitrogen
Flow Rate, mL/minute

2
5
10
2
5
10
2
5
Optimum Flow Rate, mL/minute

Air1
Hydrogen
Air2
12.5
7
15
12.5
8
15
28
3
15
14
14
15
17.5
20
15
17
17
15
15.5
18
15
18
19
15
Table 60: Optimum Flow rates PFPD
Installation of the Nitrogen Mode Parts

If you are upgrading a Phosphorus/Sulfur PFPD to add the Nitrogen mode, you
will need to replace the photomultiplier tube housing and filter currently
installed on your PFPD with the PMT assembly and filter supplied with your
upgrade kit. Refer to the figure below for identification of the components of the
N mode assembly. The steps involved are:
1. Turn off the PFPD. Alternatively, turn off GC power.
2. Disconnect the high voltage and signal cables from the base of the P/S
PMT housing.
3. Remove the PMT housing by removing the 2 thumb screws securing the
housing to the light pipe flange. Store the P/S PMT housing so as to protect
it from mechanical damage and bright light.
4. Insert the Nitrogen mode filter in the recess in front of the PMT in the N
mode housing. Be sure the silicone O-ring is in its place in the groove on
the face of the housing flange. Using the 2 screws supplied with the
upgrade kit, attach the N mode PMT housing to the light pipe flange. Be
sure that the O-ring makes a light-tight seal.
5. Reconnect the signal and high voltage cables to the connectors on the
base of the N mode PMT housing. Restore power to the PFPD.
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6. Press the Detector key, select the PFPD and press the Adjustments soft key.
Set a Gate Delay of 3.5 msec, a Gate width of 8 msec and a PMT Voltage of
600 volts.
Item
1
2
3
4
5
6
7
8
9
10
Description
Filter Mount
O-ring
O-ring, PMT Mounting
PMT Housing
Set Screws
O-ring
PMT
Socket
Retainer
Connectors with Mounting Plate
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Nitrogen Mode Operation

Operation in the nitrogen mode is very similar to the sulfur and phosphorus mode
operation described in detail elsewhere in the manual. The following differences
should be noted:
1. The nitrogen mode uses a Hammamatsu R5070 red sensitive photomultiplier
tube. This PMT may be operated at a somewhat higher voltage than the
standard phosphorus/sulfur photomultiplier. A typical voltage of 600 volts has
been used for the nitrogen mode.
2. Nitrogen emission duration is similar to but somewhat shorter than
phosphorus emission, occurring over a period of up to ten milliseconds. A
good starting point for Nitrogen mode tuning would be a gate delay of 3.5
milliseconds and a gate width of 8 milliseconds.
3. The Nitrogen mode requires somewhat finer control of the needle valve, since
the best sensitivity is achieved just after the tick tock mode of operation is
corrected. The needle valve should be opened only enough to bring the
detector out of tick tock and reduce the background noise to a usable level.
Then evaluate the signal to noise ratio of a nitrogen standard while adjusting
the Gate Delay until the optimum signal/noise is achieved.
4. The optimized flame gas flow rates in the table above give the best overall
detectivity for all nitrogen compounds, with somewhat enhanced response
from oxidized nitrogen species. If you require more uniform response
regardless of nitrogen compound type, you may increase the Air1 flow by 10
to 20%. This will enhance the response of reduced nitrogen relative to
oxidized nitrogen, at the expense of some loss in overall detectivity. We have
found a mixture of 2-nitrotoluene, 2,6-di-t-butylpyridine and N,N-diethylaniline
useful as a probe of response uniformity.
5. When properly tuned, the Nitrogen mode PFPD shows no response to simple
alkanes at fluxes up to about 1 microgram/second hydrocarbon. Above this
flux the response increases until flame propagation is completely inhibited at
about 30 micrograms/second. Selectivity against hydrocarbon interference
can be increased by opening the needle valve 1/2 to 1 turn beyond the
optimum for detectivity.
6. The near-IR sensitive PMT may respond to emissions from the detector itself
at very high detector temperatures. If you need to operate at temperatures
above 320 C, you may need to increase the trigger level to be sure that the
trigger point is well above the near-IR background. You may also find that
addition of a short pass filter which cuts off wavelengths longer than those of
your element of interest will improve detectivity and dynamic range. Optimum
detector temperature for most nitrogen compounds is about 250 C.
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Parts and Supplies (Nitrogen Mode)

In general, the parts and supplies needed to operate the N mode PFPD are the
same as those used with the P/S mode PFPD. The following are additional
parts which may be required.
Part Number
Description
03-925119-01
Filter Mount with Nitrogen Mode (RG9) filter.
03-925119-02
Filter Mount with Phosphorus mode (GG495) and

Red Absorbing (BG39) filters.
03-925128-00
Photomultiplier tube, Nitrogen mode.
Phosphorus Mode Operation

Operation in the phosphorus mode is the same with the Nitrogen mode PMT as
it is with the standard PMT. To eliminate interference of nitrogen in the
detection of phosphorus, a Schott BG39 red blocking filter may be used in
conjunction with the Schott GG495 phosphorus filter. The PMT voltage may be
run slightly (~20-50 volts) higher than the standard PMT.
Sulfur Mode Operation

No changes in operation are required to use the Nitrogen mode PMT in the
Sulfur mode. The PMT voltage may be run slightly (~20 - 50 volts) higher than
the standard PMT.
Options to Aid Optimization with Other Elements

Two options which may prove very helpful in developing optimum conditions for
the detection of additional elements are the ChromatoProbe Kit (03-925677-91)
and the PFPD Analytical Software (03-925943-92 for desktop PCs or -91 for
laptop PCs). The ChromatoProbe, used in conjunction with a 1079 PTV
Injector, allows the introduction of a controlled, continuous flux of the element of
interest into the PFPD by vaporization of a volatile compound of the element
from a temperature-controlled cup held in the 1079 PTV Injector. The PFPD
Analytical Software displays the time profile of emissions on a pulse by pulse
basis on the PC screen and allows post-run optimization of gate delay and gate
width for maximum signal to noise ratio for any desired element. Please consult
your Varian representative for more information on these options.
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Multi-element Detection
In some applications, it may be desirable to detect more than one heteroatom
simultaneously. Several combinations which may be of interest are: Sulfur plus
phosphorus mode use a WG345 filter with the standard PMT or WG345 +
RG39 filters with the R5070 PMT if nitrogen interference is undesirable. Use a
gate delay of 4 msec and adjust gate width to balance sulfur and phosphorus
response.
Sulfur + phosphorus + nitrogen mode WG345 filter with
R5070 PMT. This combination will also detect Sn, Se and As.
Sulfur + Nitrogen mode R5070 PMT with BG3 filter for
suppression of phosphorus response.
Arsenic Selective Detection

The following recommendations are based upon work reported by Prof. Aviv
Amirav and Hongwu Jing and are accurate to the best of our knowledge. This
is an area of ongoing research, so you may find that your application
requires modification of some parameters.
Emission Wavelengths
Arsenic exhibits a very broad emission spectrum, extending from 360 to
800 nm. The choice of the wavelength at which to observe As emission is
determined largely by the emission characteristics of interfering elements.
Emission Timing
Arsenic emission is longer delayed than sulfur, with a correspondingly longer
emission duration. Use the Gate Delay and Gate Width recommended for
sulfur, or increase delay even further for additional selectivity against nitrogen
and phosphorus. A 3 mm combustor provides best sensitivity.
Flame Composition
Delayed arsenic emission is optimized in hydrogen rich conditions similar to
those used for sulfur. Arsenic may also be detected in an air-rich flame, as
described below.
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Filters
Arsenic may be detected at a variety of wavelengths, depending upon the
requirements of the analysis. Good detectivity (~6 pg/second As) and selectivity
are achieved using an RG9 (nitrogen) or RG695 filter with the Nitrogen mode
R5070 photomultilplier tube. Interference by P and N compounds can be
reduced by using a long gate delay time. Tailing of the delayed emission can be
reduced by operating the detector at the highest practical temperature, or by
operating below 200 C.
An alternative approach to arsenic detection uses an air-rich flame, a GG495
(phosphorus) filter and a very short gate delay. This air-rich mode gives very
good detectivity, ~3 pg/second As. and very good selectivity against sulfur
interference, but at the expense of reduced selectivity against hydrocarbon
interference. This air-rich mode also eliminates the tendency to peak tailing
observed with the hydrogen-rich flame emission.
Linearity and Dynamic Range

Arsenic response is linear. No information is available on linear dynamic range,
although it is expected to exceed 103.
Other Considerations
Arsenic detection provides the most opportunities for optimization of any of the
common PFPD-detectable elements. Selectivity can be optimized by the choice
of air-rich or hydrogen-rich flame conditions, by the choice of gate delay and by
the choice of optical filter. In some applications, it may even be desirable to
reduce the selectivity among heteroatoms and instead look to selectivity only
against hydrocarbons. For example, the ability to detect simultaneously arsenic,
phosphorus, sulfur and nitrogen, while totally rejecting hydrocarbon response,
is extremely important in the detection of chemical warfare agents for treaty
verification purposes.
Selenium Selective Detection

Amirav and Hongwu Jing and are accurate to the best of our knowledge. This is
an area of ongoing research, so you may find that your application requires
modification of some parameters.
Selenium exhibits a fairly broad emission spectrum in the PFPD, extending
from ~360 to ~550 nm, attributed to emission of the Se2 molecule.
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Emission Timing
Selenium emission is somewhat longer delayed than sulfur, with a
correspondingly longer emission duration. Use the Gate Delay and Gate Width
recommended for sulfur.
Flame Composition
Selenium emission is optimized in cool, hydrogen rich conditions similar to
those used for sulfur. Since emission is due to Se2, use the 2 mm combustor
and keep all gas flows as low as practical to minimize dilution of the selenium
concentration in the flame.
Filters
Selenium may be detected using either the BG12 (sulfur) or the GG495
(phosphorus) filter. Best detectivity, ~10 pg/second Se, is achieved using the
BG12 filter, but this also gives the most interference from sulfur compounds.
Detectivity with the phosphorus filter is ~20 pg/second Se, but sulfur
interference is considerably reduced. Either filter gives essentially complete
specificity against hydrocarbon interference.

Selenium response is quadratic, like the sulfur response and can be treated by
the same approaches used for sulfur signal processing. Dynamic range is
approximately 103 for a given electrometer range.
Since selenium emission depends upon recombination of Se to form
electronically excited Se2 molecules, use the lowest detector temperature which
gives satisfactory chromatographic peak shapes. Selenium also exhibits a
prompt emission which may be used to distinguish it from sulfur.
Tin Selective Detection

Amirav and Hongwu Jing and are accurate to the best of our knowledge. This is
an area of ongoing research, so you may find that your application requires
Tin exhibits a fairly broad emission spectrum in the PFPD. A broad band
between ~380 and 540 nm is attributed in the literature to interaction between a
tin species and the quartz surface. The sharper bands at 610 and 695 nm have
been attributed to SnH emission. The relative and absolute amplitudes of these
bands may be a function of the PFPD flame composition.
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Emission Timing
Tin emission is somewhat longer delayed than phosphorus and emission
duration is intermediate between phosphorus and sulfur. Use the phosphorus
gate delay and width for best sensitivity; use the sulfur gate delay and width for
best selectivity against carbon interference.
Flame Composition
Tin emission is optimized in hydrogen rich conditions similar to those used for
phosphorus or sulfur. Increasing Air1, Air2 and hydrogen by 50 - 100% each
will help to reduce peak tailing. Either the 2 or 3 mm combustor may be used,
with a slight preference for the 3 mm.
Filters
Tin may be detected using either the BG12 (sulfur) or the OG590 filter. Best
detectivity, ~100 fg/second Sn, is achieved using the BG12 filter, but this also
gives the most interference from high levels of sulfur compounds. Detectivity
with the OG590 filter is ~1 pg/second Sn, but sulfur response is considerably
reduced. Response with the OG590 filter is best with the red sensitive R5070
photomultiplier tube. A 610 nm interference filter has also been found useful in
conjunction with the R5070 PMT.

Preliminary results indicate that the tin response is linear and extends over
more than three orders of magnitude.
Tin compounds exhibit tailing in the PFPD, probably due to limited volatility of
the tin combustion products. This tailing can be reduced by using higher gas
flow rates and by raising the detector temperature to 350 C to help volatilize
the tin compounds. You may also find it helpful to insulate the detector tower
using the PFPD tower cover, or by wrapping the tower with fiberglass cloth,
being careful not to cover the outlet.
An alternative approach to tin tailing is to reduce the detector temperature as
much as possible without impairing the chromatography. This reduces the tail
amplitude, but spreads it out in time. Several minutes may be required for the
detector to clean itself of tin deposits. Refer also to: J. A. Jacobsen, F. StuerLauridsen and G. Pritzl, Organotin Speciation in Environmental Samples by
Capillary Gas Chromatography and Pulsed Flame Photometric Detection
(PFPD), Appl. Organometallic. Chem. 11, 737-741 (1997).
Manganese Selective Detection

Amirav and Hongwu Jing and are accurate to the best of our knowledge. This
is an area of ongoing research, so you may find that your application requires
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Manganese exhibits a strong atomic emission line at 403 nm, along with other
weaker lines and bands in the 380 - 600 nm range. The 403 nm line is the only
emission of analytical interest with the PFPD.
Emission Timing
Manganese shows no delayed emission, as expected for atomic emission. Use
the minimum delay time and a gate width of 2 to 4 msec, depending on your
flame propagation rate.
Flame Composition
Manganese emission is favored by a hot flame, which is achieved by a
stoichiometric or slightly air rich air1/hydrogen mixture and minimum dilution of
the flame by carrier gas flow. The manganese emission is not very sensitive to
the exact gas composition, so you may vary the composition somewhat to
enhance selectivity against other elements. Emission is enhanced by the use of
the 3 mm ID combustor.
Filters
Because the manganese emission is not separated in time from the flame
background emission, a narrow band interference filter is required to provide
adequate selectivity against hydrocarbons and other interfering elements. A
404.7 nm interference filter with 10 nm bandwidth was used in Prof. Amiravs
work. This filter is commonly available as part of a set of filters for the isolation
of mercury emission lines and may be obtained from many sources of
interference filters. Using this filter, detectivity of ~100 fg Mn/second and a
selectivity against hydrocarbons of ~104 have been observed by Prof. Amirav.

Manganese response is linear. No information is available on linear dynamic
range, although it is expected to exceed 103.
Manganese containing peaks show some tailing due to incomplete clearance of
the manganese from the combustor. This tailing is minimized using nearstoichiometric flame conditions. It may be further reduced by using a detector
temperature below 225 C, but this may result in long term buildup of
manganese deposits in the combustor, although this was not observed by Prof.
Amirav.
Page: 408
User Manual 450-GC
Varian, Inc.
Maintaining the PFPD

Replacing the Optical Filter
The choice of optical filter depends on the detection mode that is to be used.
Item
1
2
3
4
5
6
7
8
Sulfur mode: Use the BG-12 deep-violet glass filter.
Phosphorus mode: Use the GG-495 yellow glass filter.
Sulfur + Phosphorus mode: Use the optional WG-345 glass filter.
Description
Ignitor cap
Photomultiplier tube (PMT) high voltage cable
Photomultiplier tube (PMT) signal cable
Photomultiplier tube (PMT) housing
Light pipe assembly
Glass filter
Filter holder
O-ring
Varian, Inc.
User Manual 450-GC
Page: 409

These tools are needed to complete the following procedure:
Glass filter in filter holder.
Lab tissues.
Capillary pick.
Disassemble the PFPD and Remove the Optical Filter

1. Turn OFF the PFPD electronics.
2. Remove the Detector cover from the top of the GC.
3. Remove the 2 thumbscrews holding the PMT housing (Item 4) to the light
pipe assembly (Item 5). Carefully remove the PMT housing from the
detector tower. The filter (Item 6) is loosely held in the filter holder (Item 7)
that is recessed in the end of the PMT housing.
4. Invert the PMT housing over a clean lab tissue and allow the filter holder to
drop out of the recess in the end of the PMT housing. If the filter holder
should stick in the PMT housing, free it by using gentle pressure with a
capillary pick or other clean utensil. Place this filter on a clean surface (e.g.,
lab tissue) or in its storage container.
Handle the filter holder by its outside edge. Do not touch the optical
surface of the filter.
Replace the Optical Filter
1. If you are cleaning the optical filter, remove the C-clip holding the filter in
the filter holder. Moisten a clean lab tissue with methanol or iso-propanol.
Hold the filter by its outer edge and gently wipe both surfaces of the filter
with the lab tissue. Wipe away the excess solvent with a clean dry lab
tissue. Place the filter in the filter holder and reinstall the C-clip.
2. Hold the filter that is to be installed by its outside edge and slide it into the
recess in the end of the PMT housing. Check that the filter is correctly
seated so that its surface is flush with the rim of the PMT housing and the
O-ring (Item 8) is properly seated in its groove.
3. Carefully join the PMT housing to the light pipe assembly and install and
tighten the 2 thumbscrews.
Page: 410
User Manual 450-GC
Varian, Inc.
Change the Detection Mode and Reassemble the PFPD

1. Go to the Adjustments page of the PFPD section.
2. Adjust the Gate Delay and Gate Width to correspond with the emission
profile of the element(s) you wish to detect.
3. Turn on the PFPD electronics.
4. Go to Optimizing the PFPD on page 368 for instructions on optimizing the
performance of the PFPD with the optical filter just installed.
Changing the Combustor Size

Although the PFPD can accommodate both narrow and wide bore quartz
combustors, either quartz combustor will work adequately when operating in
either the Sulfur or Phosphorus mode. If detectivity is not critical, you can
switch between the 2 modes without changing the size of the quartz combustor.
However, if you require the maximum detectivity for an analysis, the choice of
the appropriate diameter (narrow bore or wide bore) of quartz combustor
depends on the detection mode that is to be used.
Sulfur mode: Use the narrow-bore (2 mm ID) quartz combustor for

sulfur, selenium, or tellurium detection.
Phosphorus mode: Use the wide-bore (3 mm ID) quartz combustor for

all other elements.
S + P mode: Use the narrow-bore (2 mm ID) quartz combustor to

enhance S response. Use a 3 mm ID combustor to enhance P response
or when quenching of S response is a problem.
For column flow rates over 5 mL/min, use the wide bore quartz
combustor.
Proceed as on page 363.
Replacing a Dirty Combustor

The quartz combustor can become fouled after prolonged use, particularly with
samples containing high levels of organometallics. However, the PFPD has a
remarkable ability to clean itself of many deposits. Therefore, before replacing a
combustor, try baking the detector at high temperature with normal pulse rate
overnight or longer. If this does not restore expected noise and detectivity
levels, proceed as described on page 363.
Varian, Inc.
User Manual 450-GC
Page: 411
Ordering Parts and Supplies for the PFPD

To order parts or supplies for the PFPD, refer to the information below:
In the USA and Canada, call 800-926-3000.
In Europe, call your local Country office.
Or, call your local Varian representative.

Part Number
Description
1/16" No-Hole Ferrule
Page: 412
SG0726841
FPD test sample
82-005048-03
Test Column, DB-1 320 x 4M
03-912805-99
10 L Syringe
47-000007-00
Permeation Tube, Sulfur
03-925195-00
Diffusion Source Holder
03-925196-00
Diffusion Source Kit, Sulfur
03-925157-00
PFPD Accessory Kit
03-925190-90
Spring
03-949786-00
Injector Adapter Cap
03-925200-00
450-GC PFPD High Voltage Cable
03-925490-01
Igniter Assembly with Cable
03-925461-01
Crunch Washers (Aluminum)
15-003347-00
Adapter Seal (Aluminum)
03-925132-00
O-ring, 1.487" ID x 0.103" Wall, Silicone
27-402826-00
Combustor, Quartz (2 mm ID, Sulfur)
03-925176-00
Combustor, Quartz (3 mm ID, Phosphorus)
03-925177-00
Combustor Support (2 mm ID, Sulfur)
03-925178-00
Combustor Support (3 mm ID, Phosphorus)
03-925179-00
Combustor Support seal (Aluminum)
03-925138-00
Combustor Support Wrench
03-925192-00
Allen Wrench, 9/64" (cleaned)
03-925194-04
Teflon Pipe Thread Tape
88-189610-00
Reducing Union (flow check)
16-000327-00
Teflon Combustor Extraction Tool (wide bore, 3 mm ID)
03-925180-00
Teflon Combustor Extraction Tool (narrow bore, 2 mm ID)
03-925181-00
Teflon Tweezers
29-898500-00
Tungsten Ceramic Scorer
01-900158-00
User Manual 450-GC
Varian, Inc.
Part Number
Description
Varian, Inc.
Varian Intelligent Digital Flowmeter
01-900115-00
Soap Flowmeter
03-949846-00
Magnifying Lens
00-997369-00
Filter Assembly, Sulfur
03-925151-01
Filter Assembly, Phosphorus
03-925151-02
Filter Assembly, Tin (Sn)
03-925151-03
Filter Assembly, Sulfur+Phosphorus
03-925151-04
Filter Assembly, Arsenic
03-925151-05
Filter, Sulfur + Phosphorus
03-925158-00
Screw, Detector Tower (8-32 x 1-1/2 SHCS)
03-925194-02
Screw, Igniter Adapter and Column Guide (8-32 x 3/4 SHCS)
03-925194-01
User Manual 450-GC
Page: 413
Troubleshooting
Overview
The following section describes how to troubleshoot and correct problems with
the Pulsed Flame Photometric Detector (PFPD).
Using the Troubleshooting Guide

This troubleshooting guide outlines typical problems that you might encounter
during the routine operation of the PFPD. To use the guide, first identify the
symptom or problem (e.g., the PFPD flame does not ignite). Then, locate the
problem in the following guide. Likely causes as well as instructions for
correcting the problem are listed.
The troubleshooting guide also refers you to other sections of the Manual that
may be helpful. Should you have questions when troubleshooting the PFPD,
contact a Varian Customer Service Representative.
Flame Does Not Ignite

Possible Cause
Gas flow rates are too low or off.
PFPD electrometer is OFF.

Detector tower too cold.
Igniter coil is broken.
Detector is leaking gas from around

washers and/or seals.
Air:hydrogen gas composition is
incorrect.
Solution
Check that the carrier, air and hydrogen regulators read correct
pressures. Check that air and hydrogen are flowing through the
PFPD at the expected flow rates.
Turn the PFPD electrometer ON.
Be sure that detector oven power is On and allow enough time
for the tower to approach the operating temperature. This is
particularly important with very hydrogen rich conditions.
Use a mirror to check that the igniter is glowing. If the coil is not
glowing, the igniter coil may be broken. Disconnect the igniter
cable from the electrometer board. Check for continuity. Replace
the igniter coil and assembly if defective.
Check whether gas is leaking from around the aluminum crunch
washers or the light pipe seal.
If the igniter is glowing dimly, the gas composition may be too
rich in hydrogen. To adjust the air:hydrogen composition,
proceed as follows:
Note the current hydrogen dial setting, then turn the

hydrogen flow rate OFF
Column is installed incorrectly.
Page: 414
Check that air flow rates are approximately:

Air1 = 10-15 mL/min., Air2 = 15 mL/min.
Reset the hydrogen flow to the correct setting.
Check whether the column is leaking or is improperly secured.
Install the column correctly.
User Manual 450-GC
Varian, Inc.
Possible Cause
Carrier gas flow rate is too high.
Problem with hydrogen gas supply.
Solution
This is a particular problem when using helium as a carrier gas,
as helium tends to cool the flame excessively, preventing the
flame from propagating into the combustor. Decrease carrier
gas flow rate to an appropriate value, or increase Air1 flow
and/or increase the combustor flow to create a hotter flame in
the combustor.
Check the hydrogen gas supply as follows:
Is the hydrogen flow rate correct?
Is the hydrogen line plumbed correctly?
Is a hydrogen gas source connected to the hydrogen

line?
Are the inlet manifold and tank connections free of

leaks or other problems?
Is the hydrogen line obstructed (e.g., valve in the

hydrogen line is turned off)?
Baseline Noise is Too High

Possible Cause
Solution
Gas flows are improperly set.
Check the gas flow rates and readjust.
Combustor is dirty.
Bake the detector at high temperature overnight with flame

pulsing. Replace the quartz combustor only if this treatment
does not improve the baseline.
Column end is dirty or broken, or

extends too far into the combustor.
The end of the column may be dirty, the column may have
broken off in the combustor, or the column may be inserted too
far into the combustor. If this is the case, splinters of glass may
be fluorescing, thereby increasing the background signal.
Reinstall the column.
Detector parts are dirty.
Detector parts may be contaminated from handling. Mild

contamination often responds to a high temperature bakeout. If
this proves unsuccessful, clean the parts with reagent grade isopropanol in an ultrasonic bath. Repeat with several rinses of isopropanol.
Light pipe window is dirty or broken.
Contact Varian Service.
Photomultiplier tube is aging.
As the PMT ages the voltage must be increased to achieve the

same gain. This results in greater dark current noise. Replace
the photomultiplier tube when acceptable detectivity can no
longer be achieved.
Photomultiplier tube gain is too high.
Decrease the photomultiplier tube voltage to an acceptable

level.
Gate Width/Gate Delay is incorrect.
The Gate Delay has been set too close to the hydrocarbon
emission. Reset the Gate Delay.
Varian, Inc.
User Manual 450-GC
Page: 415
Possible Cause
Solution
Normal/Square Root setting is

incorrect.
Check that the Square Root Mode is not On, unless you wish to
operate in that mode, in which case a high noise level is
expected.
Gas flow rates are unstable.
Check for leaks. Check that the mass flow controllers are
operating properly. Replace if necessary.
NOTE: To prevent steps in the baseline when the
AutoSampler cycles, DO NOT drive the AutoSampler with
the PFPD air line.
Detector temperature is too high.
This is a particular problem when using the near-IR sensitive

R5070 PMT at temperatures above 320 C, as the PMT is
sensitive to emissions from the walls of the detector itself. If you
cannot operate the detector at a lower temperature, you may
need to add a short pass filter which will block the near-IR
wavelengths.
Detector is in the tick-tock mode.
Tick-tock mode indicates that the igniter volume is filling faster

than the combustor volume. The cure is to either slow the igniter
volume fill rate, or speed the combustor volume fill rate.
To decrease the igniter volume fill rate, while viewing the
baseline, slowly decrease the Air2 flow rate until the noise
abruptly decreases. Then, turn the Air2 mass flow controller
1/10 of a turn more.
To increase the combustor volume fill rate, turn the split valve
counterclockwise slowly while watching the baseline. When the
pulse becomes regular and background becomes constant,
increase the split valve an additional 1/2 turn.
Trigger Level Set Incorrectly.
Increase or decrease trigger level ~20%. You may need to reoptimize Gate Delay after changing trigger level.
Flame propagating past end of the

combustor support.
A rather characteristic pulse pattern (short pulse-long pulsepause) suggests that the flame front is propagating past the end
of the combustor support. This may happen at high detector
temperatures or when using a narrow-bore column with
hydrogen as the carrier gas. In such situations, the polyimide
coating on the column end will be burned off below the
combustor support.
Increase the Hydrogen flow rate by 10%. This cools the flame
and limits the propagation of the flame below the end of the
combustor support.
Alternatively, you may connect your analytical column to a 15
cm length of 0.53 mm ID deactivated fused silica tubing using a
Press-Fit connector, inserting the deactivated tubing into the
PFPD in place of your analytical column. This minimizes the
clearance between the column and the combustor, preventing
unwanted flame propagation.
Page: 416
User Manual 450-GC
Varian, Inc.
Baseline is Erratic (tick-tock)

Possible Cause
Solution
Ratio of combustor flow to igniter

flow is too small.
If possible, increase the center flow rate by turning the split

valve 1/4 turn counterclockwise.
Decrease the Air2 flow rate.
Varian, Inc.
User Manual 450-GC
Page: 417
Page: 418
User Manual 450-GC
Varian, Inc.
Detector Test Chromatograms
DETECTOR TEST CHROMATOGRAMS
The following table lists the series of test samples available for Varian GC
detectors.
Test Sample
Part Number
Compound Concentrations
TCD
82-005048-01
3.00 g/L of C14, C15 and C16 in iso-octane
ECD
82-005048-02
33.0 pg/L of lindane and aldrin in iso-octane
FPD
82-005048-03
TSD
82-005048-04
FID
82-005048-07
20.0 ng/L of n-dodecanethiol, tributylphosphate, methyl

parathion; 4000 ng/L of n-pentadecane in iso-octane
2.00 ng/L of azobenzene, methyl parathion; 4.00 ng/mL
malathion and 4.00 g/L C17 in iso-octane
30 ng/L of C14, C15 and C16 in iso-octane
Note: If the FID sample is not available, the TCD test sample can be used if first diluted 100:1
Varian, Inc.
User Manual 450-GC
Page: 419
FID Test Mix
The following figures show typical chromatograms of the Varian test mixes for
the detectors.
Figure 61: FID Test Mix Chromatogram
Column: Non-polar, e.g., 0.25m film thickness, 15m x 0.25 mm, CP-Sil 5 CB
Carrier: Nitrogen, 5 mL/minute
Injection: 1079 PTV, 200 C, 1 L splitless
Temperature Program: 80 , hold 1 minute, 20/minute to 200, hold 1 minute
Detector: 300 C, Range 12
Page: 420
User Manual 450-GC
Varian, Inc.
TSD Test Mix
Figure 62: TSD Test Mix Chromatogram
Temperature Program: 80, hold 1 minute, 20/minute to 200, hold 1 minute
Detector: 300 C, Range 12
Varian, Inc.
User Manual 450-GC
Page: 421
TCD Test Mix
Figure 63: TCD Test Mix Chromatogram
Carrier: Helium, 5 mL/minute
Detector: 220 C, Range 0.05, Filament Temperature 270 20, Filament current 200 10 mA
Page: 422
User Manual 450-GC
Varian, Inc.
ECD Test Mix
Figure 64: ECD Test Mix Chromatogram
Detector: 300 C, Range 1, Capillary current setting
Varian, Inc.
User Manual 450-GC
Page: 423
PFPD P Mode
Figure 65: PFPD P Mode Test Mix Chromatogram
Injection: 1079 PTV, 220 C, 1 L splitless of a 1:30 dilution of FPD test mix in iso-octane
Detector: 300 C, Range 10, Air1 17 mL/min., Hydrogen 14 mL/min., Air2 10 mL/min.
Gate Delay 4 msec., Gate Width 10 msec, Trigger level 200 mV
Page: 424
User Manual 450-GC
Varian, Inc.
PFPD S Mode
Figure 66: PFPD S Mode Test Mix Chromatogram
Injection: 1079 PTV, 220 C, 1 L splitless of a 1:30 dilution of FPD test mix in iso-octane
Detector: 300 C, Range 10, Air1 17 mL/min., Hydrogen 14 mL/min., Air2 10 mL/min.
Gate Delay 6 msec., Gate Width 20 msec, Trigger level 200 mV
Varian, Inc.
User Manual 450-GC
Page: 425
Page: 426
User Manual 450-GC
Varian, Inc.
Maintenance
GENERAL GC MAINTENANCE
Overview
In this section maintenance information is presented in 4 headings:
1.
2.
3.
4.
General GC maintenance, on page 428.

Injector maintenance, on page 432.
Detector maintenance, on page 436.
Pencil Filters, on page 437,
Note that some maintenance procedures, such as repair or replacement of

electronic components, should be performed by a qualified Varian service
representative. For maintenance problems where mechanical or electrical
assemblies need to be repaired or replaced please call your local Varian
service center.
There are certain maintenance tasks that should be performed on a routine
basis. These regular procedures are done to ensure that the 450-GC will
continue to operate at optimum performance. The following is a brief summary
of some common maintenance tasks and their typical frequency:
Maintenance Task
Frequency
Change septa
Typically 50 - 100 injections
Check column nuts are tight
Daily, or when performance

determinate
Condition column
Daily or as required
Change Injector inserts
Weekly, or as required
Check gas supplies
Weekly
Leak check
Monthly
Change gas cylinders
Quarterly or as required
Condition system
Semiannually
Clean detectors or parts
When performance deteriorates
Replace gas purifiers
Annually or as required
Pencil Filters
On a yearly base.
Change/Replace column
When performance deteriorates
Table 62: Maintenance Frequency

Varian, Inc.
User Manual 450-GC
Page: 427
Maintenance
General GC Maintenance
The common general GC maintenance tasks are checking and changing gas
supply cylinders, leak checking and changing gas purifier filters. These should
be performed at the frequency suggested above. The following procedures are
critical to the successful long term operation of a Gas Chromatograph. It is very
important to leak check the system on a routine basis and to ensure the quality
of gas supplies, particularly the carrier gas and H2 (Safety Reasons).
Check and Renew Gas Supplies
The pressure of the various GC gas supplies should be checked on a weekly
basis and the following guidelines used for frequency of renewing supplies:
Carrier gas: The carrier gas supply cylinder should be changed when its
pressure drops below 200 psi. This ensures that high purity carrier gas is
always supplied to the instrument. With typical usage on one Gas
Chromatograph an A-size cylinder of carrier gas should last for 3 to 6 months.
Note that this usage includes also using the carrier gas as the supply of makeup to the detectors. When a new cylinder is installed the regulator and tubing
should be purged with carrier gas before connecting to the GC. This will avoid
introducing a large amount of air into the GC. Flush the GC for a few minutes
before heating the Column.
Detector fuel gases: The typical detector fuel gases are hydrogen and air.
These should be changed when the supply pressure drops below 200 psi.
Typically an A size cylinder of hydrogen used on one GC with one Flame
Ionization Detector lasts about 6 months. However, due to the high flow rate of
air used in a Flame Ionization Detector this supply will need renewing more
frequently. For this reason it is worthwhile to consider a clean supply of
compressed air for FID equipped instruments.
Leak Check
Leak checking is one of the most important maintenance tasks for any Gas
Chromatograph. The following information refers to general leak checking
procedures for the 450-GC. Specific information regarding individual 450-GC
components will be presented in the relevant part of this maintenance section.
Leaks in the GC system can lead to poor chromatographic performance or
damage components such as the analytical column. The presence of oxygen in
the GC carrier gas at elevated temperatures can lead to permanent column
phase degradation. While the use of an oxygen filter on the carrier supply to the
instrument can help, leaks downstream of the filter are generally more likely to
be the problem.
Page: 428
User Manual 450-GC
Varian, Inc.
Maintenance
The use of soap-based leak detection fluids is NOT recommended for a high
performance capillary Gas Chromatograph due to the danger of introducing
contaminants into the system. If leak detection fluids are being used they
should only be used outside the Gas Chromatograph, i.e. to verify there are no
leaks in the plumbing to the Gas Chromatograph. If a leak detection fluid is
being used inside the Gas Chromatograph, an alcohol such as isopropanol or a
50:50 mixture of isopropanol and water should be used. Use a dropper or
syringe to place a few drops of leak detection fluid on the desired fitting and
monitor the area for bubble formation.
The most important step in leak checking is to verify that the GC system can
hold pressure. This is done by removing the column from the Injector, sealing
all exits from the Injector and pressurizing the system. Use the following
procedure to leak check 450-GC Injectors:
When conducting leak check procedures it is important to completely
seal all carrier gas exits, including septum purge and split vent outlets. If
more than one Injector is present, then the outlets of all the Injectors
must be sealed. The following procedure refers to one Injector but
should be duplicated for every Injector on the 450-GC.
1. Set the column oven and the Injector zone temperatures to 50C and allow
them to reach this temperature. This allows safe handling of Injector
surfaces.
2. Remove Injector septum nut and install a new septum. An older septum can
often be the source of a substantial leak.
3. Remove the column from the Injector. Use the appropriate nut and ferrules
to seal the base of the Injector. For packed column systems use a 1/4"
Swagelok blank off plug (SWB400P). For capillary systems use a capillary
nut (03-949551-00) with a no hole ferrule (28-694590-01).
4. If the Injector is either an 1177, 1093 or a 1079 PTV, then the septum purge
and split vent outlets must be sealed. The septum purge outlets are located
on the top frame surrounding the column oven, behind the column oven
door. The split vent outlets are located on the left side panel of the 450-GC.
Seal the septum purge by removing the outlet fitting from the septum purge
valve and replacing it with a blank off plug (P/N SWB200P). Seal the split
vent outlet by installing a Swagelok union on the outlet tube and sealing it
with a blank off plug.
5. With all outlet ports plugged, pressurize the system to 20 - 30 psi. This can
be accomplished by adjustment of manual pneumatic controls or Electronic
Flow Control (make certain that the split ratio is turned to off, constant flow
is not selected and the septum purge valve, if appropriate, is turned off).
For information on setting carrier gas pressure see the Basic Operation
section of this manual.
Varian, Inc.
User Manual 450-GC
Page: 429
Maintenance
6. Shut off the carrier supply at the source and monitor the displayed pressure
at the GC for 15 minutes. The pressure should not drop more than 0.5 psi
in 15 minutes.
Leak checking ensures that there are no leaks in the GC system up to and
including the Injector assembly. If the indicated pressure on the GC drops by
more than 0.5 psi (3 kPa) during the 15 minute test period, this indicates that
there is a positive leak in the system. Finding such a leak, particularly if it is a
small leak, can be very difficult. In general the best approach is to
systematically go through the pneumatic system from the source and tighten
each fitting until the leak is eliminated. It is important to note that leaks are often
found in the carrier gas supply to the GC.
Locate leaks preferably with an electronic leak detector or leak detection fluid.
An electronic helium leak detector is available from Varian (CP87610 110 VAC,
CP80610 220 VAC, CP83610 240VAC). This device can detect helium
concentration in the air as low as 2 ppm and is very effective at identifying the
precise location of a helium leak from a GC system.
Gas Purifier Replacement

The most common gas purifiers used in gas chromatography are moisture traps
for removing water vapor, hydrocarbon traps for removing low levels of
hydrocarbon contaminants and oxygen traps for removing low levels of oxygen.
In general the choice of filter depends on the application and detector used.
Carrier gas should contain less than 1 ppm oxygen, moisture and trace
hydrocarbon contaminants. A moisture and a hydrocarbon filter are
recommended for general applications to maintain detector background levels
at their lowest possible level. If the detector used is an ECD or MS an oxygen
filter should be employed as well.
Carrier gas filters are typically located on the side or at the rear of the 450-GC.
Varian supplies several types of carrier gas purifiers. These include a
hydrocarbon trap, moisture trap and oxygen trap. While the choice of purifier
depends on the individual configuration and performance expectations, the
following configuration is recommended for maximum carrier gas purity and
protection.
Page: 430
User Manual 450-GC
Varian, Inc.
Maintenance
The carrier gas should first pass through a hydrocarbon trap, then a moisture
filter and then an oxygen trap. As moisture reduces the effectiveness of an
oxygen trap, a moisture trap should always be placed in front of an oxygen trap.
The moisture trap should also be changed immediately when it changes color
to prevent breakthrough of moisture to the oxygen trap.
The minimum recommended carrier gas purifier configuration is a moisture and
hydrocarbon trap. This configuration can be used with routine GC analyses
using FID, TCD, TSD and PFPD detectors. If an ECD or mass spectrometer is
being used, an oxygen trap should also be added. For trace analysis the
combination of hydrocarbon trap, moisture trap and oxygen traps should be
used.
To install or replace the Gas Clean filter cartridges: remove new filter from
sealed bag. Unscrew the ring on the filter base, lift up the filter cartridge. Always
replace the 2 upper O-rings. The base contains check valves that shut off flow
when the cartridge is removed. Place ring over new cartridge, press and hold
cartridge to base and engage retaining ring.
The following are the gas purifiers available from Varian.
Check the Varian website for more information: www.varianinc.com.
Varian Gas Clean Filters
Part Number
Gas Clean oxygen filter
CP17970
Gas Clean charcoal filter
CP17972
Gas Clean moisture filter
CP17971
Gas Clean GC/MS filter
CP17973
Table 63: Varian Gas Clean Filters
Varian, Inc.
User Manual 450-GC
Page: 431
Maintenance
Injector Maintenance
The Injector is the component of the Gas Chromatograph that requires the most
frequent maintenance. This is due to the fact that the sample is deposited in the
Injector, thus leading to potential contamination and build up of non volatile
deposits. The most frequent Injector maintenance is septum replacement. In
addition insert replacement and Injector cleaning are very common. As septum
replacement is common to all liquid Injectors on the 450-GC this procedure is
presented first, followed by instructions for High-Temperature bake out of the
Injector, followed by specific maintenance procedures for the individual
Injectors.
Septum Replacement
The Injector septum is an expendable part and must be replaced on a routine
basis. The frequency of replacement depends on the number of injections and
whether the injections are by hand or with an autosampler. In general the
septum should be replaced every 50 - 100 injections or when symptoms of a
septum leak are seen. These symptoms include changing retention times,
reduced detector response or a drop in column head pressure. The latter
symptom is not always valid as some Injectors, such as the 1079 PTV, are
pressure controlled. With a pressure controlled Injector, the column head
pressure will remain constant even if a leak is present.
Use the following procedure to change a septum on any Varian Injector:
1. Cool the column oven and Injector oven to 50C. This ensures safe
handling of Injector parts and protects the column from elevated
temperatures while it is exposed to air.
2. Turn off the carrier gas supply to the Injector to prevent the septum from
being inadvertently ejected due to carrier gas pressure.
3. Remove the Injector nut by turning it counterclockwise.
4. Remove the old septum using metal tweezers or a septum pick (P/N 72000084-00). Do not to handle any internal parts of the Injector with hands or
gloves.
5. Install the new septum, again using tweezers to avoid contaminating the
Injector.
Page: 432
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Varian, Inc.
Maintenance
6. Replace the Injector nut and tighten it finger-tight until you feel resistance
from the septum, then tighten an extra 1/4 turn. Turn on the carrier gas
supply.
On occasion to save time you may want to change a septum while the Injector
is hot. Use an Injector wrench (P/N 03-908423-00) to remove and reinstall the
Injector nut. In all instances the column oven should be cool before removing
the Injector nut.
Instructions for High-Temperature bakeout of Injectors

From time to time, low volatility contaminants may build up in the Injector to a
level which interferes with proper operation. One way to remove these
contaminants is by a high temperature bakeout. Temperature sensitive parts
are removed from the Injector and replaced with the Bakeout nuts and seals
described below. This procedure applies to 1177 and 1079 PTV Injectors
installed on Varian 450-GC or 430-GC.
Injector
Item
Part
Number
Description
Bakeout NUT
03-92521701
BLACK
Bakeout DISK
03-92573102
0.34"OD x
3/32"
Bakeout NUT
03-92577201
RED
Bakeout DISK
03-92521602
0.55"OD x
3/32"
1177
1079 PTV
Table 64: Injector Bakeout Parts
1. Verify the GC is capable of normal operation and that clean, inert carrier
gas is supplied. Handle all parts using clean tweezers and place all parts to
be re-used on clean lab tissues. Remember that it is much easier to
Varian, Inc.
User Manual 450-GC
Page: 433
Maintenance
maintain cleanliness than it is to remove contaminants once they have been

introduced into the system.
2. Uninstall the analytical column from the Injector(s) to be baked out and
install a minimal flow restriction column such as 03-912805-99, or any piece
of scrap column more than 5 meters long and less than 0.53 mm ID, using
a graphite ferrule such as SG072627. The restrictor column should be
installed so that it just protrudes beyond the end of the ferrule into the
Injector, to allow the purge gas to sweep out the entire Injector volume
down to the ferrule. Do not install the scrap column into the detector!
Insert the free ends of the analytical column into a clean septum to prevent
the entry of contaminants during the bakeout period.
3. Enter Setup and edit the column parameters to reflect the restrictor column
you installed. Change the Gas Saver Timeout to 0.00 minutes. Change the
temperature limit(s) for the Injector(s) to be baked out to at least 400C.
4. Remove and discard the septum from the Injector(s). Take care to remove
any septum residues which may adhere to Injector surfaces to avoid further
contamination of the Injector with septum decomposition products during
bakeout. Remove the Injector insert from the Injector(s) and replace with a
clean insert and graphite O-ring (03-926119-40 1177 Injector). Note that
any deactivation treatment on the insert will probably be destroyed during
bakeout, so you may wish to retain this insert for use in future bakeouts.
5. Install the appropriate bakeout disk in the Injector and finger tighten the
special bakeout Injector nut. Set up the carrier gas flow to give a column
flow of about 5 mL/minute, a septum purge flow of about 10 mL/minutes
and a split ratio of 20 or more. Be sure that the Injector is set up in Split
mode. Slowly tighten the Injector nut until the Injector vent flow reaches the
expected value for the column flow and split ratio. When this value is
reached, the Injector is approximately sealed. A wrench may be required to
apply sufficient torque to make an adequate seal, but do not overtighten to
the point that the Injector is damaged. It is not necessary that the Injector
be sealed leak tight.
Page: 434
6.
Set the Injector temperature to 400 C and bake out for about 4 hours.
During this time you may want to maintain a column oven temperature of
about 300 C to assist in cleaning the Injector crossover. However, do not
heat the column oven above the temperature limit of any components,
such as valves, etc. which will remain in the oven during bakeout.
7.
Cool the Injector and column oven to about 50 C. Remove the bakeout
nut, bakeout seal, insert and sealing ferrule and scrap column and replace
with components appropriate to the intended analysis. Reset the column
parameters, Gas Saver Timeout and temperature limits you changed in
Setup. Restore the desired GC method parameters.
User Manual 450-GC
Varian, Inc.
Maintenance
8.
Varian, Inc.
To minimize contamination in the future, you may wish to install Varians

new Bleed and Temperature Optimized septa, see the specific Injector
section for more details about recommended septa.
User Manual 450-GC
Page: 435
Maintenance
Injector specified maintenance

1177 Injector, click here, on page 171.
1079 PTV Injector, click here, on page 195.
Detector specified maintenance

Flame Ionization Detector (FID), on page 292.
PDHID Detector, on page 296.
Thermionic Specific Detector (TSD), on page 317.
Thermal Conductivity Detector (TCD), on page 328.
Electron Capture Detector (ECD), on page 340.
Pulsed Flame Photometric Detector (PFPD), on page 409.
Page: 436
User Manual 450-GC
Varian, Inc.
Maintenance
Pencil Filter
The Pencil filters are used to protect the Injector and/or EFC (Injector
depending).
The Pencil Filter(s) are located underneath the left-Top cover.
Both pencil filters must be replaced on a yearly base.
It is advised to have the filters replaced by a Varian service engineer on a
regular maintenance visit.
Pencil Filters
2 types of Pencil Filters are available:

1. Molsieve/Charcoal filter (CP742210), silver color.
2. Charcoal filter (CP742211), gold color.
Varian, Inc.
User Manual 450-GC
Page: 437
Maintenance
Page: 438
User Manual 450-GC
Varian, Inc.
Shipping, Cleaning and Disposal Instructions
SHIPPING, CLEANING AND DISPOSAL INSTRUCTIONS

SHIPPING INSTRUCTIONS
If your 450-GC for any reason must send back to the nearest Varian, Inc.
subsidiary or Varian, Inc. representative, it is very important to follow these
additional preparation instructions:
1. Place the shipping restrain pin back.
2. Put protection plugs on the sample and/or carrier gas inlets.
3. Remove columns.
CLEANING INSTRUCTIONS
To keep the 450-GC surface clean, refer to the remarks given below:
Switch the 450-GC off.

Remove the power cable.
Put protection plugs on the sample and carrier gas inlets.
Put protection plugs on the Column vents.
Use a soft (no hard or abrasive) brush to carefully brush away all dust and
dirt.
If the outer case is dirty (never clean the inside!) clean it with a soft, clean
cloth dampened with mild detergent.
Never use alcohol or thinners to clean the 450-GC, these chemicals can
damage the case.
Be careful not to get water on the electronic components.
Do not use compressed air to clean.
DISPOSAL INSTRUCTIONS
When the lifetime of the 450-GC or parts of it has reached the end of its useful
life, disposal must be carried out in accordance with all (environment)
regulations applicable in your country.
Varian, Inc.
User Manual 450-GC
Page: 439
Shipping, Cleaning and Disposal Instructions
Page: 440
User Manual 450-GC
Varian, Inc.
Replacement Parts
REPLACEMENT PARTS
Replacement Parts for the CP-8400 AutoSampler, CP-8410 AutoInjector, 1177, 1041, 1061,
1079 PTV and 1093 Injectors, FID, TSD, ECD, TCD and PFPD detectors.
CP-8400/8410 Vials
2 mL Vials
2 mL Ultra GC/MS vials, screw top wide opening

clear glass, 9 mm caps, w/ Ultra GC/MS septa
392611979 100/pk
2 mL Ultra GC/MS vials, screw top wide opening

amber glass, 9 mm caps, w/ Ultra GC/MS septa
392612016 100/pk
2 mL screw top wide opening clear glass vials,

9 mm caps w/ PTFE/Silicone septa
392611549 100/pk
2 mL screw top wide opening amber glass vials,

9 mm caps w/ PTFE/Silicone septa
392611550 100/pk
2 mL crimp top wide opening clear glass vials, 11 mm

392611518 100/pk
caps w/ PTFE/rubber septa
100l polypropylene crimp top vial; 12 X 32 mm,
392611669 100/pk
11mm caps with PTFE/Butyl rubber septa
Crimping tool, 11 mm
5 mL Vials
AL666011 1 pc
5 mL Ultra GC/MS vials, 20 mm x 38 mm solvent vials 392611980 4/pk

and CP-8410 sample vials w/ snap cap and Ultra
392611981 50/pk
GC/MS septa
392611982 100/pk
392611970
392611975
392611974
10 mL Ultra GC/MS vials, 22 mm x 45 mm sample
392612006
vials for CP-8410 w/ snap cap and Ultra GC/MS septa 392612007
10 mL 22 mm x 45 mm sample vials for CP-8410 w/ 392611973
snap cap and septa
392611972
Ultra GC/MS Starter Kit (10 ea. 2 mL vials with caps
and Ultra septa, 6 ea. 5 mL vials and 5 ea. 10 mL
392611978
vials with 11 wide hole snap caps with Ultra septa)
5 mL 20 mm x 38 mm solvent vials and CP-8410
sample vials w/ snap cap and septa
10 mL Vials
Starter Kit
Varian, Inc.
User Manual 450-GC
4/pk
50/pk
100/pk
50/pk
100/pk
50/pk
100/pk
1 ea
Page: 441
Replacement Parts
CP-8400/8410 Syringes
1 L
Hamilton 1 L 7701 N Syringe
HM202950 1 ea
2 L
Hamilton 2 L 7702 N Syringe
HM202960 1 ea
Hamilton 5 L 701 syringe, 26 gauge
HM87900
SGE 5 L syringe, conical tip needle, 26 gauge
392590204 1 ea
5 L
1 ea
HM80300
1 ea
HM80366
6/pk
Hamilton 10 L 701 syringe, conical tip needle, 26 ga. SK0163520 1 ea
Hamilton 10 L 701N syringe, 26 gauge
10 L
SGE 10 L syringe, conical tip needle, 26 gauge
SG002980
1 ea
100 L
SGE 100 L syringe, Teflon tip, removable needle
SG005333
1 ea
250 L
SGE 250 L syringe
SGS006157 1 ea
CP-8400/8410 Replacement Carrousel/Tray

CP-8400 AutoSampler 100-vial Sample Carrousel
CP738642
1 ea
CP-8410 AutoInjector Sample Tray
CP739656
1 ea
Quick Connect Ferrules and Column Scales

Graphite Quick Connect ferrules w/ brass jackets
(not for use connecting to MS detector)
0.4 mm, for 0.25 mm ID columns
392538401 2/pk
392538402 2/pk
392538403 2/pk
450/430 Column insertion scale
392575001 1 ea
Fiber
SPME Fiber assortment 3/pk, 24ga
391896308 3/pk
Test Sample
SPME test sample, pk 5 ampules
391896700 5 ea
Fiber Holder
SPME fiber holder, CombiPAL/CP-8400/CP8410
392590210 1 ea
SPME Parts
Page: 442
User Manual 450-GC
Varian, Inc.
Replacement Parts
Injector Liners/Inserts
Insert
Type a
Description
1041
1061
1079 PTV
1093
1177
Split liner with fused silica wool
Laminar cup split liner
Split liner with frit
Baffle split liner
Splitless liner
Liner for direct injection on narrow bore columns, SPI
Liner for on-column 0.53 mm ID columns, SPI
SPI Glass liner with buffer
On-column injection liner
10
Splitless liner
11
Splitless liner
12
Gooseneck Split/Splitless liner
13
Gooseneck Split/Splitless liner
14
Gooseneck Split/Splitless with glass wool
15
Double Gooseneck Splitless liner
16
Inverted Cup liner.
17
Inverted cup with fused silica wool
18
Inverted cup liner packed with 10% OV-1 on Chromosorb

WHP
19
Straight liner with quartz wool
20
Gooseneck Split/Splitness liner
21
Straight Split/Splitless liner with glass wool
22
Splitless liner with glass wool
X
X
a Please refer to Liner/Insert Description on page 445

Varian, Inc.
User Manual 450-GC
Page: 443
Replacement Parts
23
Split liner packed with 10% OV-1 on Chromosorb WHP
Insert
Type a
Description
1041
1061
1079 PTV
1093
1177
24
Split/Splitless Liner
25
Liner for direct injection on Megabore 0,53 mm
26
Splitter insert with glass wool
27
Gooseneck splitter insert
28
Gooseneck splitter liner with frit
29
Splitless liner
30
Liner for SPME
31
Splitless insert
32
SPI glass liner with packed glass wool
33
Glass column guide for 3400, 3500, 3600
34
Glass column guide for 3700, 450-GC
35
Split/Splitless liner with glass wool
36
Split liner packed with 10% OV-101 on Chromosorb WHP

80/100
37
Splitless liner
38
39
Split/splitless insert with gooseneck
40
Split insert with fused silica wool
41
Split/Splitless Fast Focusliner
42
Split insert with Quartz wool
43
Split/Splitless Focusliner
44
45
Split/SplitlessTapered FocusLiner with restriction
46
Straight- through Liner

Page: 444
User Manual 450-GC
Varian, Inc.
Replacement Parts
47
Split/Splitless Tapered FocusLiner
Insert
Type a
Description
1041
1061
1079 PTV
48
49
50
Splitless Liner with Taper
51
Splitless Liner with slots
52
Packed Liner for Large-Volume Injection (LVI)
1093
1177
Liner/Insert Descriptions
Insert
Part Number Description
Type
Type
ID
OD
Length Volume Material Wool_Material Deactivated
Gooseneck
4 mm 6.3 mm 72 mm
1000
L
Glass
190010902 Laminar cup split liner
Inverted cup
4 mm 6.3 mm 72 mm
1000
L
Glass
yes
190010903 Split liner with frit
Gooseneck
4 mm 6.3 mm 72 mm
1000
L
Glass
Yes
190010904 Baffle split liner
Baffle
4 mm 6.3 mm 72 mm
1000
L
Glass
Yes
190010905 Splitless liner
Gooseneck
2 mm 6.3 mm 72 mm 250 L
Glass
Yes
190010906
SG092021
Split liner with fused silica wool
Liner for direct injection on narrow bore

columns, SPI
Quartz
Yes
Tapered
0.5 mm 5 mm
54 mm
10 L
Glass
Yes
190010907 Liner for on-column 0.53 mm ID columns, SPI
Tapered
0.8 mm 5 mm
54 mm
30 L
Glass
Yes
190010908 SPI Glass liner with buffer
Tapered
0.8 mm 4.6 mm 54 mm
30 L
Glass
Yes
391720300 On-column injection liner
On-column
10
Straight
2 mm 6.5 mm 78.5 mm 0.25 mL Glass
11
Straight
4 mm 6.5 mm 78.5 mm
12
392611926 Gooseneck Split/Splitless liner
Gooseneck
2 mm 6.5 mm 78.5 mm 250 L
13
392611927 Gooseneck Split/Splitless Liner
Gooseneck
4 mm 6.5 mm 78.5 mm
14
392611928 Gooseneck Split/Splitless with glass wool
Gooseneck
4 mm 6.5 mm 78.5 mm
Metal
1000
L
Yes
Glass
Yes
Glass
Yes
1000
L
Glass
Yes
1000
L
Glass
Glass
Yes

Varian, Inc.
User Manual 450-GC
Page: 445
Replacement Parts
15
392611929 Double Gooseneck Splitless liner
Gooseneck
Insert
Part Number Description
Type
Type
4 mm 6.5 mm 78.5 mm
ID
OD
1000
L
Glass
Yes
Length Volume Material Wool_Material Deactivated
16
392611931 Inverted Cup liner.
Inverted Cup
4 mm 6.3 mm 78.5 mm
1000
L
Glass
17
392611932 Inverted cup with fused silica wool
Inverted Cup
4 mm 6.3 mm 78.5 mm
1000
L
Glass
18
392611933
Inverted cup
4 mm 6.3 mm 78.5 mm
1000
L
Glass
19
392611934 Straight liner with quartz wool
Straight
4 mm 6.3 mm 78.5 mm
1000
L
Glass
Quartz
yes
20
392611936 Gooseneck Split/Splitness liner
Gooseneck
4 mm 6.5 mm 78.5 mm
1000
L
Glass
Glass
Yes
21
392611937 Straight Split/Splitless liner with glass wool
Straight
4 mm 6.4 mm 78.5 mm
1000
L
Glass
Glass
yes
22
392611938 Splitless liner with glass wool
Straight
2 mm 6.5 mm 78.5 mm 250 L
Glass
Glass
Yes
23
392611941
Gooseneck
4 mm 6.3 mm 72 mm
24
392611942 Split/Splitless Liner
Gooseneck
1 mm 6.3 mm 72 mm 225 L
25
392611943 Liner for direct injection on Megabore 0,53 mm Direct injection
1000
L
Glass
26
392611944 Splitter insert with glass wool
Straight
1000
L
Glass
27
392611945 Gooseneck splitter insert
Gooseneck
3.4 mm 5 mm
54 mm 500 L
Glass
Yes
28
392611946 Gooseneck splitter liner with frit
Gooseneck
3.4 mm 5 mm
54 mm 500 L
Glass
Yes
29
Gooseneck
54 mm 250 L
Glass
Yes
30
392611948 Liner for SPME
Straight
0.8 mm 5 mm
54 mm
30 L
Glass
Yes
31
392611949 Splitless insert
Straight
0.5 mm 5 mm
54 mm
15 L
Glass
Yes
32
392611950 SPI glass liner with packed glass wool
Tapered
0.8 mm 4.6 mm 54 mm
30 L
Glass
Yes
33
392611951 Glass column guide for 3400, 3500, 3600
34
392611952 Glass column guide for 3700, 450-GC
35
392611953 Split/Splitless liner with glass wool
36
392611954
Inverted cup liner packed with 10% OV-1 on

Chromosorb WHP
Split liner packed with 10% OV-1 on

Chromosorb WHP
Split liner packed with 10% OV-101 on

Chromosorb WHP 80/100
Straight
2 mm
5 mm
1000
L
Yes
Glass
Glass
54 mm 250 L
Glass
5 mm
54 mm
Glass
Yes
Glass
Siltek
Glass
Siltek
Straight
2 mm 6.2 mm 78.5 mm 250 L
38
RT207732145
5 pack
Straight
4 mm 6.5 mm 78.5 mm
1000
L
Glass
Yes
5 mm
RT207132145
Splitless liner
5 pack
User Manual 450-GC
Yes
Glass
0.8 mm 4.6 mm 18.3 mm
37
Page: 446
Yes
Yes
Glass
Straight
Fused Silica
Glass
6 mm 63.5 mm
2 mm
Yes
Yes
Varian, Inc.
Replacement Parts
39
RT207992145 Split/splitless insert with gooseneck
Insert
Part Number
Type
40
RT21079
PTV2265
41
Gooseneck
Description
Type
4 mm 6.2 mm 78.5 mm
ID
OD
1000
L
Glass
Siltek
Length Volume Material Wool Material Deactivated
Straight
SG092113
Split/Splitless Fast Focusliner
FocusLiner
42
SG092021
Split insert with Quartz wool
Gooseneck
4 mm 6.3 mm 72 mm
1000
L
Glass
Quartz
Yes
43
SG092022
Focusliner
4 mm 6.3 mm 72 mm
1000
L
Glass
Quartz
Yes
44
SG092025
Focus liner
4 mm 6.3 mm 72 mm
1000
L
Glass
Quartz
Yes
45
SG092028
Split/SplitlessTapered FocusLiner with

restriction
Focus liner
4 mm 6.3 mm 72 mm
1000
L
Glass
Quartz
Yes
46
SG092031
Straight- through Liner
Straight
0.5 mm 5 mm
54 mm
10 L
Glass
47
SG092036
Split/Splitless Tapered FocusLiner
FocusLiner
3.4 mm 5 mm
54 mm 500 L
Glass
Quartz
Yes
48
SG092037
FocusLiner
3.4 mm 5 mm
54 mm 500 L
Glass
Quartz
Yes
49
SG092038
Gooseneck
3.4 mm 5 mm
54 mm 500 L
Glass
Yes
50
SG092039
Splitless Liner with Taper
Tapered
2 mm
54 mm 170 L
Glass
Yes
51
SG092113
Splitless Liner with slots
Straight
2 mm 6.3 mm 72 mm 250 L
Glass
Yes
LVI Liner filled with deactivated Chromosorb

WAW 60 - 80 mesh
Gooseneck
52
CP14988
Varian, Inc.
4 mm 6.5 mm 78.5 mm
1000
L
Split insert with fused silica wool
2.3 mm 6.3 mm 72 mm 300 L
5 mm
3.4 mm 5 mm
User Manual 450-GC
54 mm 500 L
Glass
Quartz
Glass
Glass
Siltek
Yes
Yes
Quartz
Yes
Page: 447
Replacement Parts
1177 Injector
Parts and Supplies
Ceramic scoring wafer (for cutting fused silica columns)
0190015800
0394955100
Ferrule, no hole
2869459001
Septum pick
720000CP-8400
10/pk
Siltek Deactivated Restek Injector Liners
Siltek 4 mm ID fritted Injector insert for split

injections (must be used in combination with PFPD detector)
RT210462145 5/pk
Siltek 4 mm ID, unpacked, single gooseneck glass

Injector inserts for split/splitless injections
RT207992145
5/pk
Siltek 4 mm ID, unpacked, open glass Injector

inserts for split/splitless injections
RT207732145
5/pk
Siltek 4 mm ID, unpacked, open glass Injector

inserts for splitless injections
RT207132145
5/pk
392611931
5/pk
Injector Liner, packed W/10% OV-1 on Chromosorb-W

392611933
HP 4 MM ID, similar to HP # 18740-60840
5/pk
Injector Liner, packed with FS wool, 4 MM ID, similar to

392611932
HP # 18740-80190, MODIFIED
5/pk
Split Injector Liner, 4 MM ID, packed with FS wool,

similar to HP # 19251-60540
392611934
5/pk
Double gooseneck Splitless Injector Liner, 4 MM ID,

similar to HP # 5062-3587
392611929
5/pk
Deactivated Varian Injector Liners

Injector Liner unpacked, 4 mm ID, similar to HP #
18740-80190
Page: 448
User Manual 450-GC
Varian, Inc.
Replacement Parts
1177 Injector
Deactivated Varian Injector Liners
Gooseneck split/splitless Injector Liner, 2 MM ID,
modified 2 MM
392611926
5/pk
4 mm ID, wool plug, single gooseneck glass Injector

inserts
392611936
5/pk
Gooseneck splitless Injector liner, 4 MM ID, packed

with FS wool, similar to HP # 5181-3316
392611928
5/pk
4 mm ID, unpacked, single gooseneck glass Injector

inserts, similar to HP # 5181-3316
392611927
5/pk
4 mm ID, wool plug, open glass Injector inserts
392611937
5/pk
4 mm ID, unpacked, open glass Injector inserts, similar

392611925
to HP # S 18740-80220, 5181-8818
5/pk
2 mm ID, wool plug, open glass Injector inserts
392611938
5/pk
2 mm ID, unpacked, open glass Injector inserts, similar

392611924
to HP # S 18740-80220, 5181-8818
5/pk
SPME insert, 0.75 mm ID for SPME fiber injections
5/pk
392611998
Deactivated SGE Injector Liners (HP model 5890, 6890, 6850, 4890 GCS)
Varian, Inc.
SGE direct inlet Liner, 1.2 MM ID, Straight-Through
SG092016
5/pk
SGE split Injector liner 4 MM ID with quartz wool
SG092001
5/pk
User Manual 450-GC
Page: 449
Replacement Parts
1177 Injector
Deactivated SGE Injector Liners (HP model 5890, 6890, 6850, 4890 GCS)
No Picture available
SGE split inlet Liner, 4 MM ID, Straight-Through
SG092007
5/pk
SG092005
5/pk
SGE split/less 4 MM ID tapered focusliner inlet liner SG092003
5/pk
SGE split/less focusliner, 4mm ID
SG092002
5/pk
SGE split/splitless 2.3 MM fast tapered focusliner

inlet liner
SG092111
5/pk
SGE split/splitless inlet liner, 4 MM ID, double taper
SG092018
5/pk
SGE split/splitless inlet liner, 4 MM ID, recessed

gooseneck W/ Quartz wool
SG092010
5/pk
SGE split/splitless inlet liner, 4 MM ID, Single Taper
SG092017
5/pk
SGE split/splitless inlet liner, 4 MM ID, Single Taper W/

SG092019
Quartz wool
5/pk
SGE splitless inlet liner, 2 MM ID, recessed gooseneck SG092013
5/pk
SGE split/less 2.3 MM ID fast focusliner inlet liner
SGE splitless inlet liner, 2 MM ID, Straight-through,
Quartz
Page: 450
User Manual 450-GC
SG092004
5/pk
Varian, Inc.
Replacement Parts
1177 Injector
Septa
Insert
Seals
9.0 mm BTO Centerguide septa
CR298713
50/pk
9.0 mm Advanced Green 3 Centerguide septa
CR246713
50/pk
9.0 mm Marathon Centerguide septa
CR239778
25/pk
Viton O-ring for 6.3 and 6.5mm OD liners, 260 C max 8850103100
25/pk
Graphite O-ring 6.5 mm ID to fit HP Splitless 6.5 mm

OD Liners
392611930
10/pk
Graphite O-ring 6.5 mm ID, fits 6.5 mm OD Liners
392611940
10/pk
Graphite O-ring 6.3 mm ID, for HP Split 6.3 mm OD

Liners, similar to HP # 5180-4168
392611935
10/pk
1078/1079 PTV Injector

Parts and Supplies
Ceramic scoring wafer (for cutting fused silica columns)
0190015800
0394955100
Ferrule, no hole
2869459001
Septum pick
720000CP-8400
10/pk
SPME Mode Insert
Insert, 0.8 mm SPME for Fiber Injections
392611948
5/pk
Insert, tapered for column sealing with 0.53 mm ID

capillary columns
190010907
5/pk
Insert, high performance for column sealing with 0.32

or 0.25 mm capillary columns
190010906
5/pk
3.4 mm fritted Injector insert for enhanced mixing for

linear split performance
392611946
5/pk
On-Column Mode Inserts
Split Inserts
Varian, Inc.
User Manual 450-GC
Page: 451
Replacement Parts

Split Inserts
3.4 mm unpacked Injector insert
392611945
5/pk
3.4 mm packed w/10% OV101 on Chromosorb for full

range of capillary columns
392611954
5/pk
392611947
5/pk
2.0 mm packed insert with glass wool for split/splitless

392611953
injections
5/pk
0.5 mm open insert for trace analysis and thermolabile

392611949
compounds
5/pk
Splitless Mode Inserts
2.0 mm open insert to minimize dead volume
1078/1079 PTV Deactivated SGE Injector Liners
SGE LVI Large volume Injection inlet liner, sintered

glass
Page: 452
SG092245
5/pk
SGE Split/less 3.4 mm ID Tapered Focusliner inlet liner SG092036
5/pk
SGE Split/Splitless 3.4 mm ID Focusliner inlet liner
SG092037
5/pk
SGE Split/Splitless 3.4 mm ID inlet liner, single taper
SG092038
5/pk
SGE Splitless 2 mm ID inlet liner, single taper
SG092039
5/pk
User Manual 450-GC
Varian, Inc.
Replacement Parts

Split Inserts
Septa
SGE Straight-Thtough inlet liner, 0.5 mm ID
SG092031
5/pk
11.5 mm BTO Centerguide septa
CR298777
50/pk
11.5 mm Advanced Green 3 Centerguide septa
CR246725
50/pk
11.5 mm Marathon Centerguide septa
CR239787
25/pk
392534201
10/pk
Septa BTO, 9.5 mm
CR298705
50/pk
Septa Marathon, 9.5 mm
CR239188
25/pk
Septa, Advanced Green 3, 9.5 mm
CR246124
50/pk
1041 Insert for 0.53 mm ID columns
392543101
1060/1061 Flash Injector Liner, 0.53 mm ID Capillary

columns
392611943
5/pk
1060/1061 Flash Injector Liner, W/Glass wool, for

packed columns
392611944
5/pk
CP742552
1/pk
Insert Ferrule 1079 PTV graphite insert ferrule
1041/1061 Injector
Parts and Supplies
Septa
Inserts
1041 Stainless Steel Insert for Headspace injection
Packed Column Adapter Kits
Packed Column Adapter Kit for 1041, 1/8 SS columns
03-925588-91
Packed Column Adapter Kit for 1061, 1/8 SS columns
03-925588-92
Packed Column Adapter Kit for 1041& 1061, 1/4 glass columns
03-925586-91
Note that these kits contain Injector and detector adapters
Varian, Inc.
User Manual 450-GC
Page: 453
Replacement Parts
1093 Injector
Parts and Supplies
Septa
Column
Ferrule
7/16" (11.5MM) HT SEPTA,TEFLON FACED
00-997630-02 25/pk
BTO Centerguide septa, 11.5 mm
CR298777
50/pk
Marathon, Centerguide septa, 11.5 mm
CR239787
25/pk
Advance Green 3, Centerguide septa, 11.5 mm
CR246725
50/pk
Heater/Probe Harness, 120 Volt AC
391833400
Heater/Probe Harness, 240 Volt AC
391833401
Septum Support
391821100
Injector Switch Actuator
390820601
Union 1/8 W/Flow Restriction
3600004601
1/8 Swagelok brass plug
2824707101
Injector Nut W/ Cage
394966601
Polymide/Graphite 0.5mm ID
2869458101
10/pk
Polymide/Graphite 0.8mm ID
2869458200
10/pk
Graphite 0.5mm ID
SG072626
10/pk
Graphite 0.8mm ID
392611909
10/pk
SPI 0.5mm High Linearity direct injection liner for

0.25mm and 0.32 mm ID columns
190010906
5/pk
SPI High Linearity On-column injection liner for

0.53mm ID columns
190010907
5/pk
SPI Injector direct injection liner, 0.8mm ID, packed

Glass wool, injection volumes> 1 ql
392611950
5/pk
SG092027
5/pk
10/pk
Inserts
No Picture Available
0.5mm ID, SPI deactivated Injector liner
0.8mm ID, 0.25mm restriction SPI deactivated Injector
SG092030
Liner
0.8mm ID, 0.5mm restriction SPI deactivated Injector
Liner
Page: 454
User Manual 450-GC
SG092034
5/pk
5/pk
Varian, Inc.
Replacement Parts
Detectors
Flame Ionization Detector (FID)
Flame Tip Assembly (0.02 ID)
02-001938-00
Aluminum Crunch Washer (25)
15-003347-01
Thermionic Specific Detector

TSD Bead Probe
03-906074-00
TSD Bead Probe, preconditioned
03-906074-01
Electron Capture Detector (ECD)

ECD Cell with 63Ni Foil
02-001972-01
ECD Wrench
72-000081-00
Thermal Conductivity Detector (TCD)

TCD Make-up Gas Option
03-925605-01
Pulsed Flame Photometric Detector (PFPD)

Aluminum Crunch Washer
15-003347-00
Combustor, Quartz (2mm ID)
03-925176-00
Combustor, Quartz (3 mm ID)
03-925177-00
Filter Assembly, Sulfur
03-925151-01
Filter Assembly, Phosphorus
03-925151-02
Igniter Assembly
03-925160-00
Combustor support, 2 mm
03-925178-00
Combustor support, 3 mm
03-925179-01
Combustor support seal
03-925138-00
Varian, Inc.
User Manual 450-GC
Page: 455
Replacement Parts
Page: 456
User Manual 450-GC
Varian, Inc.
Technical Tips
TECHNICAL TIPS
This section will give technical tips regarding common questions like:
1. Chromatographic Interpretations, on page 458.
2. To Bleed not to Bleed .. that is the question 1, on page 461.
3. Choosing the right GC Injection Technique 2, on page 466.
4. GC line Labyrinth How to choose the right Injector Insert 3, on page 472.
1 Source Technical helpdesk Europe, Middelburg, The Netherlands

Varian, Inc.
User Manual 450-GC
Page: 457
Technical Tips
CHROMATOGRAPHIC INTERPRETATIONS
The troubleshooting procedures outlined in this section are structured to
accommodate deviations from known responses of a standard sample,
including peak shapes, peak areas, retention times, baseline characteristics,
etc.
In these cases, the general characteristics of the chromatogram are well known
and even slight deviations can be discerned.
A vast majority of gas chromatographic malfunctions will be indicated by one or
more of the following symptoms; inspect the chromatogram for all of the
symptoms:
Change in peak size (peaks of different area, or height than expected).

Change in retention times.
Change in baseline stability.
Asymmetrical peak shapes (non-Gaussian, skewed, etc.).
Change from expected peaks.
For overall troubleshooting of the capillary system based on the appearance of

the chromatogram, refer to Table Capillary Chromatographic Interpretations.
If a problem exists which cannot be identified and/or corrected, call your
nearest Varian Service Center for assistance.
Symptom
Cause
Remedy
Multiple peaks from a single

compound
Injection is too large.

Initial temperature is too low.
Tailing
Degraded column or sample

adsorption.
Frit may be clogged.
Reduce the size of the

injection.
Initial temperature should
be no more than 20C
below the solvent boiling
point for samples greater
than or equal to 1.0 mL.
Replace or recondition
column.
Contaminated insert.
Excess dead volume.
Injector not heating correctly.
Peak broadening, poor resolution Degraded column.

Wrong carrier gas flow.
Page: 458
User Manual 450-GC
Replace purge frit or use

needle valve.
Replace glass insert.
Recheck Injector
assembly and column
connections.
Check make-up gas flow.
Check Injector
heating/cooling functions.
Replace or recondition
column.
Varian, Inc.
Technical Tips
Symptom
Cause
Remedy
Check carrier gas flow.
Ghost peaks during temperature

programming, no injection made
Contaminated Injector.
Replace or clean Injector

insert.
Bake out Injector per
Section 4.
Leading peak
Overloaded column.
Decrease sample size or

increase dilution; use
column with thicker film.
Check column
connections and Injector
insert for obstructions.
Lower initial Injector
temperature.
Reseat column to glass
insert. See Section 3.
Decrease column
temperature.
Check for leaks (Section
4, paragraph 4.2).
Repair or replace syringe.
Replace or repair column.
Check or replace septum
or Injector.
Reduce maximum
temperature
Use column with
appropriate coating
thickness for sample. For
relatively non-volatile
compounds that require a
high retention
temperature, choose a
0.1 coating thickness.
Check gas filters. Correct
all leaks, checking for the
following:
(a)make-up gas line union
(b)column-to-detector
connection
(c)detector insert-todetector crossover
connection
(d)detector crossover-to-
Carrier gas flow restricted.
Long solvent peak tail
Injector temperature too high.

Injector leakage.
Column temperature too high.
No sample peak or peak too

small
Leak at column inlet.

Syringe is leaking.
Broken column.
Injector is leaking.
Rising baseline when

temperature programming
Column temperature limit

is exceeded.
Contamination.
Varian, Inc.
User Manual 450-GC
Page: 459
Technical Tips
Symptom
Cause
Instrument problem.
High boiling compounds, C60

through C80, not eluting
Wrong flame tip.
Syringe hits insert
Glass insert installed upside

down (wrong end facing up).
Page: 460
User Manual 450-GC
Remedy
detector body connection
Condition the column or
bake out the column as
described in Section 4. In
badly contaminated
systems, it may be
necessary to lift the
detector crossover from
the ion oven, then heat
the lines and crossover
with a flame while purging
with an inert gas.
Install an uncoated test
column and repeat the
Change to ceramic flame
tip,
P/N 03-918351-00.
Reverse glass insert.
Varian, Inc.
Technical Tips
TO BLEED OR NOT TO BLEED THAT IS THE QUESTION

As GC and capillary column manufacturer Varian is regularly confronted with
customer queries with respect to rising baselines and baseline instability. These
effects are often attributed to column failures and unacceptable column bleed is
the diagnosis. But is this really the case? Here follows a short guide into more
effective troubleshooting on the baseline.
A rising baseline is part of many temperature-programmed analyses in gas
chromatography. The major factors contributing to this rise are:
1.
2.
3.
4.
Stationary phase bleed from the column.

Contamination in the Injector system.
Contamination of the detector system.
Carrier gas impurities.
Both the column and the Injector/detector system can play a role in baseline
rises and it is important to distinguish between the 2 sources.
Starting the troubleshooting exercise by immediately disconnecting the column
from Injector and/or detector can mean an unstable system for at least a couple
hours. It can be more effective to have a closer look at the baseline itself first.
The baseline below 250 C

Improvements in column technology and stationary phase synthesis during the
last few years have resulted in highly temperature stable capillary columns.
Examples of these are the Varian Factor Four column range. These columns
only show some measurable bleed levels close to their maximum operating
temperature. This maximum temperature is often around 325 C. The bleed
level of a capillary column roughly doubles with every 14 C and it means that
already at oven temperatures 75 C below the maximum temperature its bleed
level is virtually zero. Therefore, any significant baseline rise starting before 250
C can safely be attributed to system contamination from medium to high
molecular weight residues. Most frequently these are originating from a
contaminated Injector. This contamination may use the column as a transport
device but the column is not the primary source. Major air leakage however,
may oxidize the liquid phase at temperatures lower than 250 C and high
column bleed level can results of this.
Varian, Inc.
User Manual 450-GC
Page: 461
Technical Tips
Injector contamination
Unstable and noisy baselines, which include ghost peaks during a blank
analysis run, are hardly ever caused by column bleed.
Clear distinctive peaks eluting during such a blank analysis run are an
indication again of Injector contamination (figure 1).
Higher molecular weight residues inside the Injector are continuously being
introduced on to the column, trapped there at lower oven temperatures and
eluted again at higher temperatures. Injector contamination can be confirmed
by lowering the Injector temperature to e.g. 100 C. Evaporation from the
Injector of the higher molecular residues is significantly reduced at these lower
temperatures. The overall bleed level should drop and the majority of the ghost
peaks should disappear. In case of a split/splitless injection Injector
contamination can also be confirmed by extending the splitless time period
considerably. A contaminated Injector will expose itself by an increased bleed
level and/or higher ghost peaks. If the Injector is contributing to the bleed level
maintenance should be performed. In particular replace the septum, liner and
glass wool. Confirm the cleanliness of the Injector by performing a blank
injection.
If lowering the Injector temperature has little effect on the total bleed level the
focus of attention should be directed towards the column or to the purity of the
carrier gas.
Page: 462
User Manual 450-GC
Varian, Inc.
Technical Tips
The Column
Mass spectra taken from the bleed can be of great help in determining its
source. The main bleed products from all siloxane-based columns are some
smaller cyclic siloxane fragments formed by degradation of the liquid phase.
These fragments have m/z ions of 207, 281 and 341 (figure 2). However, the
presence of these ions in the spectrum is no confirmation of column bleed. Also
the septum is made of almost 100 % pure polydimethylsiloxane just like the
liquid phase of the capillary column. The total siloxane amount of a septum can
be more than a factor 40 of that present in a capillary column. Torn away pieces
of septum inside the liner or septum bleed can therefore be responsible for this
typical mass spectrum. In cases where the mass spectra of the bleed is
dominated by other m/z ions than 207 and 281 the cause of the bleed is most
likely Injector contamination due to sample residues. Degradation of the liquid
phase and formation of bleed products is often the result of low ppm level
presence of oxygen and moisture in the carrier gas. It is therefore imperative to
install high quality gas filters close to the GC.
Bleed formation from the column is a continuous process and usually exhibits
itself as a slow steady climb of the baseline. Exceptions to this general rule are
the older type cyanopropyl containing liquid phases. These columns may form a
wavy, sinusoid like, rising baseline close to their maximum operating
temperature.
Varian, Inc.
User Manual 450-GC
Page: 463
Technical Tips
Phase degradation at these temperatures is creating bleed products and they

are trapped on the column during the rapid cool-down of the oven at the end of
the analysis. These relatively small, low molecular weight degradation products
are subsequently eluted during the next analyses. It can sometimes be difficult
to distinguish this bleed pattern from a contaminated Injector induced bleed.
Lowering the Injector temperature will not reduce this type of bleed
The problem can be partially solved by a more controlled and slower cool down
of the oven. Recent implementation of Varians FactorFour technology in the
cyano-type phases like the VF-1701ms and VF-624ms have effectively
eliminated these problems al together so that the column bleed patterns and
levels are like any other MS grade column. Wave like baselines patterns, which
already begin at lower temperatures, can be the result of a poorly conditioned
column but can also be related to unstable column flows or impurities in the
carrier gas or detector gases.
Page: 464
User Manual 450-GC
Varian, Inc.
Technical Tips
Gas Impurities
Impurities in either the carrier gas or detector gases can cause unstable
baselines.
Figure 4 shows the effect on the baseline stability due to the presence of some
hydrocarbon impurities in the hydrogen gas flow for an FID. A noisy baseline
caused by gas flow impurities is independent of oven temperatures and visible
throughout the entire temperature program.
The installation of a good quality gas purifying system like the Varian GasClean filters will maintain a supply of high quality gasses to both the column
and detector. Overall baseline stability will improve. If positioned close enough
to the GC such a system will guarantee oxygen, moisture and hydrocarbon free
gas supply regardless of initial gas bottle quality or the possible presence of
leakage anywhere in the gas supply system.
Varian, Inc.
User Manual 450-GC
Page: 465
Technical Tips
CHOOSING THE RIGHT GC INJECTION TECHNIQUE

A vast number of injection techniques are being used in gas chromatography
today. Some have been around since the early days of GC while the popularity
of others is sometimes of more recent date. This article attempts to briefly
characterize the most commonly used techniques, their applications and their
limitations.
The analysis in GC starts with the introduction of the sample onto the column. It
is also by far the most critical step in the entire analysis. The liquid sample is
vaporized either inside the column itself or in a vaporization chamber positioned
just in front of the column.
The injection system should fulfill the following requirements:
The injected amount should not overload the column.
The injection bandwidth should be small compared to the band broadening

effects in the capillary column.
Other requirements, which could be applied, are:
The column should be able to achieve its optimum separation efficiency.
Sample composition should remain intact. No discrimination should occur

on basis of boiling point, polarity, concentration or thermal stability.
Applicable to trace analysis as well as high concentration samples.
The injected amount should be reproducible.

No injection technique will meet all of the above demands. Some requirements
will have to be sacrificed in order to meet the others. The detection of traces
and higher concentrations both at the same time is often difficult to combine
within one single injection technique. The choice of injection technique is often
determined by the concentration levels, which have to be reached.
Direct Injection
Split Injection
Splitless Injection
Cool on-column
Programmed Temperature Vaporizer (PTV)
Page: 466
User Manual 450-GC
Varian, Inc.
Technical Tips
Direct Injection
Description
Sample is vaporized in the hot insert. The entire sample enters the
column.
Volume(s)
0.1 L 1 L
Concentration Range
1 ppm - %-levels.
Application
Applicable to packed and 0.53 mm ID capillary columns

No refocusing on the column is needed.
Direct injection is the most commonly used injection technique for packed
columns and 0.53 mm ID columns. Its major advantages are its ease of use
and the wide concentration range that it can cover. It is especially suitable for
the lower concentrations in the ppm range, which are below the scope of the
split injection. Higher gas flow rates are needed for an efficient and quick
sample transfer from the Injector liner to the column. The minimum gas flow for
direct injection is about 5 mL/min. Direct injection can therefore only be applied
to columns, which can cater for higher column flow rates such as, packed
columns or 0.53 mm ID columns. These columns can also handle the higher
concentration levels because of their increased sample capacity. Direct
injection will produce poor peak shapes if too large injection volumes (> 1 L)
are applied. Discrimination effects are low compared to split injections. Direct
injection is sometimes confused with the splitless type injection described
further below. The Varian Injector models 1040/1041 and 1060/1061 are
designed for various types of direct injection.
Split Injection
Description
Sample is vaporized in the hot insert. Only a fraction of sample

enters the column. The majority is vented of through the split vent.
Volume(s)
0.1L 1 L
Concentration Range
50 ppm - %-level
Remark
Applicable to all capillary columns.

Usually no refocusing on the column is needed.
Beyond doubt the most widely used injection technique for capillary columns.
This is despite its tendency for discrimination of compounds with higher boiling
points. The reproducibility of the injection is strongly dependent on liner
geometry and heat capacity. (See also the Tech Tip: the jungle of injection
liners, e-inspirations, No. 3, September 2004). Sample discrimination during
the evaporation from the syringe also occurs due to differences in component
volatility. The difference in sample capacity of the various capillary columns
Varian, Inc.
User Manual 450-GC
Page: 467
Technical Tips
(varying internal diameters and film thickness) can easily be addressed by

changing the split flow. The relatively high split flow takes care of a quick and
efficient sample introduction onto the column. Split injections can exploit the full
separation power of the capillary column because of this quick sample
introduction. The following table gives some general guidelines, which splitflows should be applied to which column diameter. Split flows and split ratios
are related to column sample capacity and the minimum flow needed in the
Injector to minimize band-broadening effects.
Column ID [m]
Split ratio
Minimum split flow [mL/min]
530
1:5 to 1:15
15
320
1:20 to 1:250
25
250
1:50 to 1:250
40
150
1:150 to 1:500
75
100
> 1:500
150
The suggested minimum split ratios and split flows can result in band
broadening inside the Injector liner and therefore loss of separation efficiency is
likely.
The 1177 Injector model is the most recent split/splitless Injector of Varian.
Splitless Injection
Description
Sample evaporates in the hot Injector. The majority of the sample

enters the column during the first 1 2 min of the analysis.
Volume(s)
0.5 L 2 L
Concentration Range
0.5 ppm 50 ppm
Remark
Refocusing on the column needs to be supported by retention gaps

and low oven temperatures.
The most widely used technique for low ppm level samples. Splitless is often
confused with direct injection. Sample is being introduced on the column during
the entire splitless time. Due to this 1 2 min period there is a large initial
injection bandwidth and refocusing of the analytes on the column is essential in
order to obtain good symmetrical narrow peak shapes. This is done in 2 ways:
1. Cold trapping. The large temperature drop between Injector (250 C) and a
low initial oven temperature (50 C) effectively reduces the mobility of
higher boiling compounds to virtually zero. These compounds freeze in a
narrow band and only start to migrate again during the temperature
program. This cold trapping effect combines both focusing due to thermal
condensation as well as focusing as a result of a strong retention in the
columns stationary phase.
Page: 468
User Manual 450-GC
Varian, Inc.
Technical Tips
2. Solvent focusing. Reconcentration of lower boiling components (close to

the boiling point of the solvent) takes place by the solvent effect. Low oven
temperatures will allow the solvent to condense in the column together with
the low boiling sample components. The liquid film formed by the solvent
will start to evaporate and the sample components will concentrate in a
continuously smaller liquid film, resulting in a narrow band of concentrated
sample components. Whether this process really takes place as described
here is still a point of discussion among chromatographers. Fact is that both
choices of solvent and initial oven temperatures are important in obtaining
narrow peak shapes. The table below provides some general guidelines.
Solvent
Boiling Point
[C]
Suggested Initial Oven Temperature

[C]
n-Pentane
36
10 to ambient
Dichloromethane
36
10 to ambient
Carbon disulfide
40
10 to ambient
Chloroform
46
10 to ambient
Methanol
61
25
n-Hexane
65
35
Ethyl acetate
69
40
Acetonitrile
77
45
n-Heptane
82
50
Isooctane
98
70
Column flow and the volume of the liner determine the speed and effectiveness
of the sample transfer from Injector to column. Very low column flows prevent
the use of splitless and it is mainly for this reason that 100 m are not suited of
splitless type of injections. 150 m columns can be used but only if the splitless
time period is long enough and the liner volume limited to 250 L to permit
adequate sample transfer.
Splitless is not very suitable for samples where the components of interest elute
closely to the solvent either in front or behind. Insufficient focusing of the
analytes will produce poor peak shapes. In those cases a direct injection on a
0.53 mm ID column is often preferable.
The 1177 Injector model is the most recent split/splitless Injector of Varian.
Varian, Inc.
User Manual 450-GC
Page: 469
Technical Tips
Cool on-column
Description
Sample passes from the syringe into the column. The column is kept
cool during injection and is subsequently heated. The Injector is kept
cool during sample introduction.
Volume(s)
0.1 L 2 L
Concentration Range
0.25 ppm 50 ppm
Remark

Cool on-column is perhaps the most ideal injection technique. It eliminates
inlet-related discrimination and alteration and combines this with a high
analytical precision. Syringe discrimination, as experienced with split and
splitless, is absent. Components eluting just in front of the solvent however are
difficult to focus and therefore difficult to determine. Cool on column follows
closely the splitless injection type with respect to refocusing aspects like oven
temperatures and the use of retention gaps. The market acceptance of the cool
on-column Injector has always been rather limited. This is mainly due to the
instrumental difficulties during the early days of its introduction. Its competitor
splitless is far easier to automate and this is one of the reasons for its wide
acceptance. Automated on-column Injectors require a 0.53 mm ID piece of
deactivated fused silica or retention gap as inlet piece because of the gauge 26
syringes used in auto samplers. Although not a cold on-column Injector in the
true sense, the Varian 1093 SPI Injector covers the same application range
and provides similar results.
Programmed Temperature Vaporizer (PTV)

Description
Sample passes as a liquid from the syringe into a cooled inlet. The
sample is subsequently heated to vaporize the sample. Split or
splitless injection can be applied.
Volume(s)
0.1 L 250 L
Concentration Range
1 ppb 50 ppm
Remark

The PTV Injector can arguably be considered as the most universal of Injector,
capable of handling a wide variety of sample types, concentrations and
volumes. In essence, it is designed as a split/splitless Injector that can be
rapidly heated (and cooled. The syringe introduces the sample in it liquid state
into a cold Injector insert. Discrimination of the sample compounds by additional
evaporation of the more volatile constituents is absent. Evaporation of
Page: 470
User Manual 450-GC
Varian, Inc.
Technical Tips
components starts as the insert is being heated. The PTV can operate in
various modes:
Cold Split Injection
is comparable with a split injection but with a cold transfer from syringe to
insert. This provides less discrimination effects and therefore more accurate
results. Refocusing using retention gaps and low oven temperatures may be
necessary for lower boiling compounds.
Cold Splitless Injection
is similar to hot splitless. It has the same advantages as cold split with
respect to the cold transfer from the syringe. The classic hot splitless technique
can result in thermal degradation due to the long residence time of components
in the hot insert. The PTV in cold splitless mode also avoids this phenomenon.
Refocusing using retention gaps and low oven temperatures may be necessary
for lower boiling compounds.
Solvent Venting
permits the injection of large sample volumes (250 L). It enables detection
limits in the ppb range. The majority of the solvent is removed through the split
vent. The components are retained in the liner by cold trapping, aided in some
cases by packed supports. At the end of the vent period the split vent is closed
and the insert is rapidly heated. This technique requires a slow sample
introduction in order to avoid overloading the insert. Lower boiling compounds
will unavoidably be partly vented of together with the solvent depending on
insert temperatures, type of packed support and vent times. In general, light
boiling solvents are preferred for better results. Some column refocusing on the
column supported by retention gaps and low initial oven temperatures is
needed.
The Varian 1079 PTV Injector can perform all of these modes.
Varian, Inc.
User Manual 450-GC
Page: 471
Technical Tips
GC LINER LABYRINTH - HOW TO CHOOSE THE RIGHT INJECTOR INSERT
Injections and vaporization in gas chromatography are influenced by a number

of variables. The liner always plays a significant role. The most important ones
are liner design and volume, sample composition, Injector heat capacity, heat
transfer and adsorption effects. These factors together with the type of injection
determine for a large extent the choice of liner.
Liner Types
Three major types of injection based on flash vaporization of the sample can be
distinguished:
1. Direct injection
After flash vaporization the entire sample is transferred to the column. The
sample transfer speed in the Injector is determined by column flow and
volume of the Injector liner. This injection type is most commonly applied for
0.53 mm ID columns or packed columns. Injection volumes usually do not
exceed 1 L. This maximum in injection volume is related to the internal
volume of the liner.
2. Split injection
After flash vaporization the sample is divided into 2 streams. One directed
towards the column, the other to the split vent. Here, the sample transfer
speed in the Injector is mainly determined by the flow of the split vent and
the liner volume. The column flow plays an insignificant role. A high transfer
speed of the sample is critical for the quick introduction of the compounds
into the capillary column maintaining the columns separation efficiency Split
injections are used for all capillary columns with IDs ranging from 100 m to
530 m. The maximum injection volume for split injections is about 1 L.
Page: 472
User Manual 450-GC
Varian, Inc.
Technical Tips
3. Split/Splitless
During the initial splitless period the vaporized sample is transferred to the
column. The capillary column flow and the liner volume determine the speed
and efficiency of this process. Larger injection volumes are possible for
splitless type injections; volumes up to 5 L are not uncommon. These large
injection volumes can never be injected at once because of possible liner
overload but must be careful introduced at a rate of about 1 L/sec.
Liner volume
The sample gas volume, which at one time resides in the Injector, should in all
cases be smaller than the internal volume of the liner. If not, the liner is
overloaded and back flash of the sample into various (metal) parts of the
Injector may occur. This phenomenon will cause poor injection profiles, bad
peak shapes, adsorption and possible sample carry over. Many liners used for
direct and split injection have dimensions of about 80 mm x 4 mm resulting in
an internal volume of ca. 1mL. The effective volume available for the sample is
however significantly lower as part of the liner volume will always be filled with
carrier gas. The list below indicates the solvent expansion volume per L at
250 C and 50 kPa
Methanol
0.65 mL
n-hexane
0.2 mL
Isopropanol
0.34 mL
Water
1.46 mL
Dichloromethane
0.41 mL
It is clear from the above that water and methanol in particular quickly can
cause liner overload and some care must taken if these solvents are used. For
these solvents smaller injection volumes than 1 L are to be recommended.
Injector heat capacity

The efficient and quick evaporation of the sample is influenced by the following
factors:
Varian, Inc.
sample volume
type of solvent and sample components
Injector and liner geometry and design
presence of quartz wool or other liner fillings
User Manual 450-GC
Page: 473
Technical Tips
The last three determine the heat capacity of the Injector and its ability for heat
transfer to the sample. The below list compares the amount of energy needed for
evaporation of methanol and water relative to cyclohexane.
Water
5.22
Methanol
3.29
Cyclohexane
1.00
Solvents like methanol and water require much more energy than other
common solvents for their evaporation therefore they need a larger heat
capacity and better heat transfer system for a quick evaporation.
This can be accomplished by using higher Injector temperatures (>275 C) and
larger liner surface areas. Glass or quartz wool is often used to increase the
Injectors heat transfer capacity. The evaporation of higher boiling compounds
also requires more energy and also in those cases quartz wool is often used.
Besides benefits glass or quartz wool also has a few disadvantages. The wool
can become adsorptive especially if some fibers are broken or when it has
become dirty. It should be exchanged at a regular basis to prevent
chromatographic problems
Discrimination effects
The main aim and challenge of injections is to maintain sample integrity and
sample composition during its transition from the liquid to the gaseous state and
also during the sample transfer from Injector to the column. The evaporation
process of low boiling compounds is always quicker than that of high molecular
weight ones. This difference accounts for the often-mentioned discrimination
effects caused by injections. In general, the quicker and more complete the
evaporation of the sample, the less discrimination effects will be observed.
Higher Injector temperatures, special liner design and quartz wool will help to
minimize these effects. Inconsistent discrimination profiles will result in poorer
repeatability.
Page: 474
User Manual 450-GC
Varian, Inc.
Technical Tips
Liners for splitless injections

Straight liner
These are low cost liners for samples with a narrow boiling point range
and little risk of thermal decomposition. Can be packed with quartz
wool to aid evaporation, limit discrimination and trap non-volatile
materials. Do not use for high boiling samples. Comes usually in 2 or 4
mm ID. Use the 4 mm version for sample volumes > 2 L to prevent
liner overload.
Gooseneck
Minimizes breakdown of active compounds and improves the splitless

efficiency. The gooseneck prevents the sample from reaching metal
Injector parts, which could cause decomposition of sensitive
compounds. The gooseneck is positioned at the top of the Injector. It is
generally regarded as the best splitless liner.
Gooseneck with wool
The single gooseneck can be easily packed with quartz or glass wool to
minimize discrimination. Wool is also a risk as it can become active and
adsorptive due to the trapping of non-volatile residues. Replace it at
regular intervals.
Double Gooseneck
The 2 goosenecks isolate the sample vaporization cloud from any

metal Injector parts. The risk of catalytic breakdown is reduced. This
type of liner can not packed with glass wool.
Varian, Inc.
User Manual 450-GC
Page: 475
Technical Tips
Recessed Gooseneck
This model has the same advantages as the other goosenecks but in
addition it can be packed with glass wool at the top. It can also be used
for dual column analysis.
Liners for split injections

Frit Splitter
The ceramic frit will prevent dirt and non-volatiles from reaching the
column. The frit can become active. The gooseneck prevents back
flash.
Inverted -or Laminar Cup Splitter
The cup will promote evaporation and mixing of the sample with the
carrier gas. It is the best splitter for higher molecular weight
compounds. Slightly larger injection volumes are possible because the
cup will hold the sample liquid until it vaporizes. It is difficult to clean
and is relatively expensive.
Baffle Splitter
The baffle creates a turbulent flow, which results in more reproducible

injections. Not well suited for higher boiling compounds because of
incomplete vaporization and thus subject to discrimination.
Page: 476
User Manual 450-GC
Varian, Inc.
Technical Tips
Liners for direct injections

Straight tube
This type of liner is more suited for packed columns than it is for 0.53
mm ID columns. The wide-bore column should be positioned at the
bottom of the liner just piercing through the ferrule. This will minimize
the effects of possible dead volume during injections although Injector
parts, which are swept poorly with carrier gas will result in poor injection
profiles.
Gooseneck
This is a different type of gooseneck liner where the gooseneck holds

the wide-bore column in position. This design effectively eliminates any
dead volume in the Injector and provides the best possible injection
profile for wide-bore columns. In reversed position it can also be used
for on-column injections on 0.53 mm columns.
Varian, Inc.
User Manual 450-GC
Page: 477
Technical Tips
Page: 478
User Manual 450-GC
Varian, Inc.
Appendix A: Error Codes
APPENDIX A: ERROR CODES

Code
8
Error Description
Coolant timed out
Error level
Event
Cause Condition(s)
Column oven standby

EFC21 (gas saver)
450-GC action
Error Led on for all
errors
Notification Message
Action needed
Activate method, clear
timeout
FID Flame out
15
Front FID Flameout
Alert
16
Middle FID Flameout
Alert
17
Back FID Flameout
Alert
FID signal is < than given

threshold
No gas supply, flow 0.0 mL/min
threshold
threshold
Auto-re-ignite
Auto-re-ignite
Auto-re-ignite
Ignite FID flame, check

EFC flow (gas supply), set
FID gasflows
FID gasflows
FID gasflows
TCD Air Leak

18
Front TCD Air Leak
Event
Air Leak
TCD Power off,

Electronics off
Check for TCD air-leak
19
Middle TCD Air Leak
Event
Air Leak
TCD Power off,

Electronics off
20
Back TCD Air Leak
Event
Air Leak
TCD Power off,

Electronics off
Injector EFC Flow Out of Range
35
Front EFC Flow Out of Range
Alert/Error w
Flow is above max+10% or below 5kPa for more then 10 seconds
Activated Safety
Method
Check EFC flows (gas

supply)
36
Middle EFC Flow Out of Range
Alert/Errora
Activated Safety
Method

supply)
37
Back EFC Flow Out of Range
Alert/Errora
Activated Safety
Method

supply)
Alert/Errora
Pressure is above max+10% or

below -5kPa for more then 10
seconds
Injector EFC Pressure Out of Range

38
Front EFC Pressure Out of Range
w If the used gas is Hydrogen (H ) the Error level is Error, in all other cases an Alert is given.
2
Varian, Inc.
User Manual 450-GC
Page: 479

39
Middle EFC Pressure Out of Range
Alert/Errora
40
Back EFC Pressure Out of Range
Alert/Error x

seconds
seconds
Injector EFC Flow ready time out

41
Front EFC Flow Ready Time Out
Alert/Errora
Unit not ready for 10 minutes
Activated Safety
Method
42
Middle EFC Flow Ready Time Out
Alert/Errora
Activated Safety
Method
43
Back EFC Flow Ready Time Out
Alert/Errora
Activated Safety
Method
Check gas supply, set

desired pressure, check
EFC device, reboot GC
Injector EFC Pressure ready time out

44
Front EFC Pressure Ready Time Out
Alert/Errora
Activated Safety
Method
45
Middle EFC Pressure Ready Time Out
Alert/Errora
Activated Safety
Method
46
Back EFC Pressure Ready Time Out
Alert/Errora
Activated Safety
Method
PFPD Board Failure

Electronics off (all)
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
50
Front PFPD Board Failure
Alert
Defect PFDP board
Replace PFPD board
51
Middle PFPD Board Failure
Alert
Defect PFDP board
52
Back PFPD Board Failure
Alert
Defect PFDP board
53
Becoming Not Ready (during run)
Event
54
Becoming Ready (during run)
Event
Event
Replace PFPD board

Replace PFPD board
IOC Failure
55
IOC Bad Addre Chan
x If the used gas is Hydrogen (H ) the Error level is Error, in all other cases an Alert is given.
2
Page: 480
User Manual 450-GC
Varian, Inc.

56
IOC Bad Cmd
Event
57
IOC Stepper in Motion
Event
58
IOC Bad Parameter
Event
59
IOC Run mode error
Event
60
IOC no Detector
Event
61
IOC Command not Allowed
Event
62
IOC_EFC_BUFFER_OVERFLOW, Unit rebooted
Event
Caused by too many request

requested by IOC to EFC Interface
print.
GC reboot the interface

print firmware
63
IOC_EFC_COMMUNICATION_ERROR, Unit
Rebooted
Event
Communication between EFC

Interface Print and EFC broken.
GC reboot the interface

print firmware
Zone Open Sensor (zone)

67
Column Oven Open Sensor
Error
Column Oven sensor not in use, mis

used
68
Zone 1 Open Sensor
Error
Zone 1 sensor not in use, mis used
69
Zone 2 Open Sensor
Error
70
Zone 3 Open Sensor
Error
71
Zone 4 Open Sensor
Error
72
Zone 5 Open Sensor
Error
73
Zone 6 Open Sensor
Error

H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
Check Column Oven zone

Check zone (1)
Check zone (2)
Check zone (3)
Check zone (4)
Check zone (5)
Check zone (6)
Shorted Sensor (zone)

74
Column Oven Shorted Sensor
Error
Shorted sensor. Defect Sensor
75
Zone 1 Shorted Sensor
Error
Varian, Inc.
User Manual 450-GC

H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min

Check zone (1)
Page: 481

76
Error
77
Error
78
Error
79
Error
80
Error

H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
Check zone (2)

Check zone (3)
Check zone (4)
Check zone (5)
Check zone (6)
Thermal Runaway (zone)

81
Column Oven Thermal Runaway
Error
82
Zone 1 Thermal Runaway
Error
83
Error
84
Error
85
Error
86
Error
87
Error

H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min

Check zone (1)
Check zone (2)
Check zone (3)
Check zone (4)
Check zone (5)
Check zone (6)
Max Temper Exceeded (zone)

88
Column Oven Max Temper Exceeded
Error
Defect Sensor
89
Zone 1 Max Temper Exceeded
Error
Defect Sensor
90
Error
Defect Sensor
91
Error
Defect Sensor
Page: 482
User Manual 450-GC

H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min

Check zone (1)
Check zone (2)
Check zone (3)
Varian, Inc.

92
Error
Defect Sensor
93
Error
Defect Sensor
94
Error
Defect Sensor
Turn device off. Temperature below

-10 C, only for non callable devices

H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
Check zone (4)

Check zone (5)
Check zone (6)
Min Temper Exceeded (zone)

95
Column Oven Min Temper Exceeded
Error
96
Zone 1 Min Temper Exceeded
Error

97
Error

98
Error

99
Error

100
Error

101
Error


H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min

Check zone (1)
Check zone (2)
Check zone (3)
Check zone (4)
Check zone (5)
Check zone (6)
Too Slow Response (zone)

109
Column Oven too slow response
Error
110
Zone 1 too slow response
Error
111
Error
112
Error
113
Error
114
Error
Varian, Inc.
Sensor not used (wrong used),

mismatch heated device. 230 V GC
is using 110 V heaters
User Manual 450-GC

H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min

Check zone (1)
Check zone (2)
Check zone (3)
Check zone (4)
Check zone (5)
Page: 483

115
Error


H2 flow set to 0.0
mL/min


H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
Check zone (6)
Too Fast Response (zone)

116
Column Oven too fast response
Error
117
Zone 1 too fast response
Error
118
Error
119
Error
120
Error
121
Error
122
Error

Check zone (1)
Check zone (2)
Check zone (3)
Check zone (4)
Check zone (5)
Check zone (6)
Fan or Heater
123
No Fan or Heater detected
Error
Hardware error
124
Watch Dog Heater activated
Error
Hardware error
TCD no Air Leak (position)

230
Front TCD no Air leak
Event
When error (18) is solved within 4

minutes after error (18) appears
231
Middle TCD no Air leak
Event

232
Rear TCD no Air leak
Event

TCD Air Leak fault (position)

233
Front TCD Air leak fault
Alert
4 minutes after error (18) where

there has been no No Air Leak
Turn Electronics and

power off
Find source and

repair/replace hardware
234
Middle TCD Air leak fault
Alert


power off
Find source and

Page: 484
User Manual 450-GC
Varian, Inc.

235
Rear TCD Air leak fault
Alert


power off
Find source and

Max Setup Temper Exceeded (position)

247
Column Oven Max Setup Temper Exceeded
Error
Defect Sensor. Temperature is

10 C above set temperature limit
248
Zone 1 Max Setup temper Exceeded
Error

249
Error

250
Error

251
Error

252
Error

253
Error


H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min

Check zone (1)
Check zone (2)
Check zone (3)
Check zone (4)
Check zone (5)
Check zone (6)
Detector EFC Flow out of range

304
Front DFC Chan1 out of range
Alert/Error y
Flow is above max +10 % or below 5 mL/min for more then 10 sec.
Activate Safety Method
Turn off/on flow, check

source (gas-supply)
305
Alert/Errora

source (gas-supply)
306
Alert/Errora

source (gas-supply)
307
Middle DFC Chan1 out of range
Alert/Errora

source (gas-supply)
308
Alert/Errora

source (gas-supply)
309
Alert/Errora

source (gas-supply)
310
Rear DFC Chan1 out of range
Alert/Errora

source (gas-supply)
311
Alert/Errora

source (gas-supply)
312
Alert/Errora

source (gas-supply)
y If the used gas is Hydrogen (H ) the Error level is Error, in all other cases an Alert is given.
2
Varian, Inc.
User Manual 450-GC
Page: 485
313
Front EFC Channel 1, flow ready time out
Alert/Errora
314
Alert/Error z
315
Alert/Errora
316
Middle EFC Channel 1, flow ready time out
Alert/Errora
317
Alert/Errora
318
Alert/Errora
319
Rear EFC Channel 1, flow ready time out
Alert/Errora
320
Alert/Errora
321
Alert/Errora
Auto Sampler (AS)

370
Sampler old firmware
Event
Syringe stepper motor firmware old
371
Sampler Faulted
Alert
Mismatch AutoSampler
Cable in SID2, check

power switch, jumpers on
AS, Reboot GC
372
Sampler Communication error
Alert
No communication AS
Check cables, reboot GC
373
Sampler Tower error
Alert
No response AS-tower. Start AS

when AS is turned off
374
Sampler Carrousel error
Alert
Block carrousel when its turning
375
Sampler Syringe Sled error
Alert
Block syringe when its turning
376
Sampler Plunger error
Alert
Hall sensor unplugged Switched to

SPME mode during syringe use
Recalibrate AS, reboot GC
377
Sampler Syringe Missing
Alert
No Syringe available
Place Syringe
378
Sampler Vail Missing
Alert
No Vial available
Vial detect should be turned on
Place Vial in position
z If the used gas is Hydrogen (H ) the Error level is Error, in all other cases an Alert is given.
2
Page: 486
User Manual 450-GC
Varian, Inc.

(setup)
379
Sampler Dual Dup Mode Delay Expired
Alert
Delay between runs has expired

before the second injection. This
error will only appear in dual-/ or
duplicate mode
380
Sampler Run not started after Inj
Alert
Run did not start injection. Contact

switch on Injector broken?
Notification Message?
restart
381
Sampler Syringe volume exceeded
Alert
Total Injection volume exceeds

syringe volume
Check error source
383
Sampler Tower sensor not found
Alert
Unplugged sensor: sense tower
Check source, solve error
384
Sampler Carrousel sensor not found
Alert
Carrousel not in place
385
Sampler Syringe sled sensor not found
Alert
Unplugged sensor: sled sensor
386
Sampler Plunger sensor not found
Alert
387
Sampler Plunger Strokes exceed limit
Alert
Plunger strokes exceed limit
Reset plunger stroke

counter
Remove time out, restart

seq.
Gas saver timeout expired (position)

388
Front Gas saver timeout exceeded
Event
Gas saver timeout exceeded
Activate standby
method
Activated method, remove

time out
389
Middle saver timeout exceeded
Event
Activate standby
method

time out
390
Rear saver timeout exceeded
Event
Activate standby
method

time out
391
Run ended before second injection
Alert
Stopped
Check cause, solve, restart

automation?
Miscellaneous
412
Unavailable operation nonautom
Alert
Running, remote with Galaxie
Check cause, solve, restart

automation?
413
IOP_COMMUNICATION_FAILURE_AT_STARTUP_e
Error
IOP Communication Failure at

startup
Replace/fix IOP
425
IOP_SKIPS_ADC_READING_e
Error
IOP too busy (might be due to EFC)

and therefore skips ADC reading
Alert
Set Injection to 60 L/se (with

testclient) using a 10 L syringe
Auto Sampler (AS)

414
Sampler Max Plunger speed exceeded
Varian, Inc.
User Manual 450-GC

H2 flow set to 0.0
mL/min
Down load method, reset

plunger speed
Page: 487

416
Sampler Tray is missing
Alert
Only on 8410 sampler
Place tray in position
418
Sampler Vial is unreachable
Alert
Only on 8410 sampler, tray has

been turned vial becomes
unreachable for the tower
Calibrate AS, place vial,

solve error
423
Sampler Vial sensor bad
Alert
Defective sensor
424
Sampler Column standby timeout expired
Event
Standby timeout expired
426
Sampler Plunger stuck on sensor
Alert
(errors not reproducible)
427
Sampler Syringe stuck on sensor
Alert
428
Sampler Tower stuck on sensor
Alert
429
Sampler Carrousel stuck on sensor
Alert
434
Sampler EDS Checksum is bad
Alert
436
IOP Communication failure
Error
IOP Communication failure
437
Battery voltage out of range
Event
439
PGA Calib Failed
440

H2 flow set to 0.0
mL/min
Activate method, reset
time out
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
H2 flow set to 0.0
mL/min
Replace vial sensor

Activate method, reset time
out
-
Replace/fix IOP
Battery voltage < 2V or > 4V

error
Error
IOPSH (measuring system)
Recalibrate PGA
Temp Calib Failed
Error
Recalibrate temp
442
Press out of tolerance
Error
Ambient pressure < 15kPa or >

115pKa error
443
Boardtemp out of tolerance
Error
Currently in use, only logged
GC main board
Check power supply

requirements/ replace main
board electronics
Out of Tolerance (red_id)

444 to 465 Refvolt out of Tolerance
(all voltages on mainboard, part of
measuring system)
Hazardous by default, basis of all
measurement in system
444
P10V ref out of tolerance
Error
445
AIN10V out of tolerance
Error
446
P5V ref out of tolerance
Error
447
P2V5 ref out of tolerance
Error
Page: 488
User Manual 450-GC
Varian, Inc.

448
P24V Prim out of tolerance
Error
449
P24V Sec out of tolerance
Error
450
N24V out of tolerance
Error
451
P5V D out of tolerance
Error
452
P5V out of tolerance
Error
453
Error
454
P15V out of tolerance
Error
455
Error
456
P5V DAC out of tolerance
Error
457
VREF1 out of tolerance
Error
458
VREF0 out of tolerance
Error
Out of Tolerance (cts_id)

459
CTS1 out of tolerance
Error
460
Error
461
Error
462
Error
463
Error
464
Error
465
Tref out of tolerance
Error
466
Step motor moving
Error

H2 flow set to 0.0
mL/min
Option Board Errors

Varian, Inc.
User Manual 450-GC
Page: 489

482
Analogoutput buffer underrun
Alert
Buffer underrun
483
Analogoutput buffer overflow
Alert
Buffer overrun
484
Analogoutput communication error
Alert
485
Optionboard external events error
Alert
Page: 490
User Manual 450-GC
Varian, Inc.
Appendix B: Public Statement
APPENDIX B: PUBLIC STATEMENT

This public statement is required for the GPL/LGPL licensed software used in
this Gas Chromatograph.
GNU General Public License is a free, copy left license for software and other
kinds of works.
The 450-GC is using version 2.6.18 of the Linux kernel (provide by Montavista
Pro 5.0).
For more details about used GPL/LGPL packages look in the document
License included on the CD (CP501414) which is included with the 450-GC.
Varian, Inc.
User Manual 450-GC
Page: 491

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Read Before Operating

Important Tips Regarding 450-GC Operation

If a potentially hazardous Error is detected, such as a thermal runaway, the

User Manual 450-GC

VARIAN ANALYTICAL INSTRUMENT WARRANTY

LIMITATION OF REMEDIES AND LIABILITY

User Manual 450-GC

User Manual 450-GC

Information to aid you in

Alerts you to situations that

Alerts you to potentially

The potential for explosion may exist because of type of

Ionizing radiation source is present. Follow manual

Keep hands and fingers away.

User Manual 450-GC

GENERAL SAFETY PRECAUTIONS

Store organic solvents in fireproof, vented and clearly labeled cabinets so

Do not accumulate waste solvents. Dispose of such materials through a

User Manual 450-GC

COMPRESSED GAS CYLINDERS

Store and handle compressed gases carefully and in strict adherence to

Secure cylinders to an immovable structure or wall.

Store and move cylinders in an upright, vertical position. Before transport,

Store cylinders in a well-ventilated area away from heat, direct sunshine,

Mark cylinders clearly so there is no doubt as to their contents.

Use only approved regulators and connections.

User Manual 450-GC

Use only fireproof ducting.

Install a blower at the duct outlet.

Check periodically for proper operation of the duct.

Radioactive Source Detectors

User Manual 450-GC

SPARE PARTS AVAILABILITY

Varian provides a variety of

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User Manual 450-GC

User Manual 450-GC

User Manual 450-GC

General laboratory precautions........................................................................................ 9

User Manual 450-GC

User Manual 450-GC

External Sample Introduction Systems............................................................................. 101

User Manual 450-GC

Column Installation in Detector .................................................................................... 160

User Manual 450-GC

Temperature Ramped Splitless Injection ..................................................................... 191

User Manual 450-GC

Condition the Column................................................................................................... 224

User Manual 450-GC

Two trap sizes available ................................................................................................... 253

User Manual 450-GC

PULSED DISCHARGE HELIUM IONIZATION DETECTOR (PDHID)..................................... 295

User Manual 450-GC

ELECTRON CAPTURE DETECTOR (ECD) ............................................................................ 329

User Manual 450-GC

Adjust the Gas Flow Rates ............................................................................................... 365

User Manual 450-GC

Emission Wavelengths ..................................................................................................... 405