Trace 1110 SOP 2013 Rev 0.2013

Thermo Fisher Scientific
TRACE 1110
Standard Operating Procedures
PN 827S07134, Revision 0- 2013
TRACE™ GC 1110 - Standard Operating Procedures
September 2013 Edition
© 2013 Thermo Fisher Scientific. All rights reserved.
Printed in India
Published by Thermo Fisher Scientific India Pvt. Ltd.

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Printing History: First Edition, released July 2013.
Disclaimer
Technical Information contained in this publication is for reference
purposes only and is subject to change without notice. Every effort
has been made to supply complete and accurate information;
however, Thermo Fisher Scientific assumes no responsibility and will
not be liable for any errors, omissions, damage, or loss that might
result from any use of this manual or the information contained
therein (even if this information is properly followed and problems
still arise).
This publication is not part of the Agreement of Sale between

Thermo Fisher Scientific and the purchaser of a TRACE™ GC 1110
system. In the event of any conflict between the provisions of this
document and those contained in Thermo Fisher Scientifics’ Terms
and Conditions, the provisions of the Terms and Conditions shall
govern.
Reference to System Configurations and Specifications supersede all

previous information and are subject to change without notice.
Trademarks
TRACE™ GC is a trademark of Thermo Fisher Scientific Inc., and its
subsidiaries. Other brand and product names may be trademarks or
registered trademarks of their respective companies.
Contents
Chapter 1 About This Manual ........................................................................... 1

Conventions Used in This Manual................................................... 1
Informational Symbols .................................................................... 2
Abbreviations for Injectors and Detectors ....................................... 2
Safety Information ........................................................................... 3
Using the TRACE GC 1110 Document Set..................................... 3
SOPs Overview ................................................................................ 4
Chapter 2 General Overview ............................................................................ 1

Scope ................................................................................................ 1
Parts Referenced .............................................................................. 2
Getting Started ................................................................................. 2
Column Conditioning ...................................................................... 3
Operating Procedure ........................................................................ 4
Chapter 3 Checkout Using FID with PKD Injector......................................... 1

Scope ................................................................................................ 1
Recommended Initial Operations .................................................... 2
Analytical Conditions Required for Packed Injector ....................... 3
Chapter 4 Checkout Using FID with S/SL Injector ......................................... 1

Scope ................................................................................................ 1
Analytical Conditions Required for Splitless Injection ................... 2
Chapter 5 Checkout Using FID with PTV Injector ......................................... 1

Scope ................................................................................................ 1
Analytical Conditions Required for PTV Injection ......................... 2
Thermo Fisher Scientific Trace 1110 SOP Guide i

Contents
Checkout Using TCD with PKD Injector ....................................... 1

Chapter 6 Scope ................................................................................................ 1
Analytical Conditions Required for Packed Injector ....................... 2
Chapter 7 Checkout Using TCD with S/SL Injector ....................................... 1

Scope ................................................................................................ 1
TCD-S/SL Injector Analytical Conditions...................................... 2
Chapter 8 Checkout Using ECD with S/SL Injector ....................................... 1

Scope ................................................................................................ 1
Chapter 9 Checkout Using NPD with S/SL Injector........................................ 1

Scope ................................................................................................ 1
Chapter 10 Checkout Using FPD with S/SL Injector ( Sulphur mode) ........... 1
Scope ................................................................................................ 1
Checkout Using FPD with S/SL Injector (Phosphorus mode)......... 5
ii Trace 1110 User Guide Thermo Fisher Scientific

Chapter 1
About This Manual
Conventions The following symbols and typographical conventions are used

throughout this manual.
Used in This
• Bold : Bold text indicates names of windows, menus, dialog
Manual
boxes, buttons, and fields.
• Italic : Italic indicates cross references, first references to
important terms defined in the glossary, and special emphasis.
• Monospace : Monospace, or Courier, indicates filenames and
filepaths, or to indicate text the user should enter with the
keyboard.
• MonospaceBol : Monospace Bold indicates messages or prompts
displayed on the computer screen or on a digital display.
• » : This symbol illustrates menu paths to select, such as
File»Open….
• KEY NAME : Bold, uppercase sans serif font indicates the name
of a key on a keyboard or keypad, such as ENTER.
• CAUTION : This symbol alerts you to an action or procedure
that, if performed improperly, could damage the instrument.
• NOTE : This symbol alerts you to important information related
to the text in the previous paragraph.
Thermo Fisher Scientific Trace 1110 SOP Guide 1

About This Manual
Informational Symbols
Informational Informational symbols used in this manual and their meaning:
Symbols
Warning pertaining to a possible safety hazard or instrument damage.
Some important information is given, which can be noted down
Warning pertaining to a possible explosion hazard.
Hot surface. Avoid contact. Surfaces are hot and may cause personal
injury if touched.
Abbreviations for Table 1.1

Injector Abbreviation
Injectors and Split/splitless Injector S/SL
Detectors Packed Column Injector PKD
Programmable Temperature Vaporizing Injector PTV
Table 1.2
Detector Abbreviation
Flame Ionization Detector FID
Electron Capture Detector ECD
Nitrogen Phosphorus Detector NPD
Flame Photometric Detector FPD
Thermal Conductivity Detector TCD
2 Trace 1110 SOP Guide Thermo Fisher Scientific

About This Manual
Safety Information
Safety
Information Precaution for Gases
Before using gases, carefully read the indications of hazard and the
warning reported in the Safety sheet supplied by the manufacturer
with reference to the relevant CAS number (Chemical Abstract
Service).
WARNING! : Hydrogen is a harmful gas that mixed with air may

give rise to an recourse to special precautions due to the risk
involved.
Precaution for the Electron Capture Detector
WARNING! : The Electron Capture Detector (ECD) contains a 63Ni

beta-emitting radioactive source of 370 MBq (10 mCi). For no reason
should the detector be opened or handled by the operator. Any
maintenance or service operations involving even partial
disassembling of the instrument must be performed ONLY by
qualified personnel at the laboratory expressly authorized by Thermo
Fisher Scientific and specially licensed to handle radioactive material
Using the TRACE The TRACE GC Ultra Document Set (CD-Rom PN 828S08030)
includes all manuals in electronic format, and serves as your library
GC 1110
for information about the TRACE GC 1110 hardware and software.
Document Set
The TRACE GC 1110 Document Set as paper copy is also available
Furthermore, Thermo Fisher Scientific part numbers (PN) for the
paper copy manuals are provided for each book title.
Preinstallation Manual : (PN 827S07132) this manual and diskette

describes how to set up a workspace for the TRACE GC 1110 and
how to connect the TRACE GC 1110 to the gas supplies and
peripheral devices.
Operating Manual : (PN 827S07130) this manual provides

descriptions of the TRACE GC 1110 hardware and software and
instructions for their use.
Service Manual : (PN 827S07133) this manual contains instructions

for diagnosing and resolving operational problems.

About This Manual
SOPs Overview
Standard Operating Procedures : (PN 827S07134) this manual

contains instructions, operating sequences, and test criteria for final
testing of the TRACE GC 1110.
Spare Parts Catalog : (PN 827S07133) this catalog contains a list of

spare parts for the TRACE GC 1110
The SOPs Overview section contains a general description of the

SOPs Overview Standard Operating Procedures.
Chapter 2 General Overview contains a guideline to apply correctly

the SOPs.

Chapter 2
General Overview
Chapter at a Glance…
• Scope
• Parts Referenced
• Getting Started
Operating Procedures
• Test Column Conditioning
Scope The Standard Operating Procedures (SOP) described in this book are
a series of instructions, operations and test criteria derived from our
quality policy procedures used for final testing of the TRACE GC
1110. The SOPs have been developed to test and verify instrument
complete analytical performance after the installation has been
completed. This will help you as a guideline, to check if your TRACE
GC 1110 continues to perform according to the original checkout
testing specifications carried out in the factory premises. However,
these tests alone cannot define if the instrument is not performing
according to the original specifications. The checkout is carried out
injecting a standard solution into a test column under analytical
conditions set according to the injector(s) and detector(s) hardware
provided with the GC. Before starting the test checkout, refer to the
Parts Referenced and the Analytical Condition required.
For specific operating or maintenance questions, please refer to

the following manuals:
• TRACE GC 1110 Operating Manual PN 827S07130
• TRACE GC 1110 Service Manual PN 827S07133
• TRACE GC Ultra Pre installation Manual PN 827S07132

General Overview
Parts Referenced
Parts Referenced Table 2.1 The SOPs require the following parts:
Part Description Part

Number
Test Column Fused Silica Capillary Column TR-5; 7 m
long; 0.32 mm ID; 0.25 µm film thickness. 637260E11
Graphite ferrule for 0.32 mm ID column 3P
Syringes Standard 5 or 10 µl size; with 50 mm needle 523860920
length or
523860926
Test Mixtures Test Mixture for FID checkout 102973441
Test Mixture for ECD checkout 102973442
Test Mixture for NPD checkout 102973443
Test Mixture for FPD checkout 102973444
Test Mixture for TCD checkout (SSL) 102973445
Test Mixture for TCD checkout (Packed) 102973446
Gases Gas Chromatographic-grade purity
Carrier Gas = Helium
Fuel Gases = Hydrogen - Air
Make-up Gas = Nitrogen
Data Chrom-Card Iris 32
Acquisition
Note : under un avoidable circumstances Nitrogen can be used as a

Carrier gas in place of Helium and can be replaced in all the test
procedure in this manual..
Getting Started Before starting checkout, perform the following preliminary

operations sequentially:
1. Gas Supply Connections : Connect the gas supplies following

the instructions reported in Chapter 2 of the TRACE GC 1110
Operating Manual.
2. Data Handling Connections : Connect your data handling

following the instructions reported in Chapter 5 of the TRACE
GC 1110 Operating Manual.

General Overview
Column Conditioning
3. Column Installation : Install the test column according to the

injector installed in your GC following the Operating Sequences
reported in Chapter 5 “Column installation information” of the
TRACE GC 1110 Operating Manual.
• Preparing a Capillary Column

• Connecting a Capillary Column to a Split/Splitless Injector
• Connecting a Packed Column to packed Injector
• Connect a Capillary Column to an Programmable
Temperature Vaporizing Injector
4. Glass Liner and Septum Installation : Install the glass liner

following the Operating Sequences “Install a Liner and Septum”
reported in the TRACE GC Ultra Operating Manual.
• Chapter 6: Split/Splitless Injector

• Chapter 10: Packed Column Injector
• Chapter 12: Programmable Temperature Vaporizing Injector
Column CAUTION !
When performing column conditioning, the column should be
Conditioning
connected only to the injector leaving the column outlet
disconnected to avoid the possibility of contamination of the
detector base body.
Column conditioning consists of passing a flow of carrier gas through

the column and heating it to a temperature of 20-50 °C above the
maximum temperature that will be used for running the analysis.
Refer to Table 1-2 for the parameter setting and to the Operating
Procedure “Test Column Conditioning” on page 31, to perform the
operation.
Detector Connections This operation should be carried out at the end

of the column conditioning. Connect the test column to the detector
following the Operating Sequences reported in Chapter 5 “Column
installation informations” of the TRACE GC 1110 Operating
Manual.

General Overview
Operating Procedure
• Connecting a Capillary Column to an FID, FPD or NPD

Detector
• Connecting a Capillary Column to an ECD Detector
• Connecting a Capillary Column to a TCD Detector
Operating
Table 2.2 Test Column Conditioning
Procedure Parameter Setting
Gases Carrier Gas: Helium or Nitrogen
Control Mode : Constant Flow
Injector Mode: Splitless
Column Flow = 3.40 ml/min (for Capillary column )
Column Flow = 20.0 ml/min (for Packed column )
Oven Initial Temperature = 50 °C
Program Initial Time = 1 min.
Ramp 1 = 10 °C/min.
Final Temperature = 250 °C
Final Time = 30 min.
Injector Temperature = according to the injector in use
Before beginning, press CONFIG to verify the GC configuration:

1. Use INJ menu and set the Flow and temperature value for the
required test
2. Use OVEN menu to display the Column Oven parameters. Set the
oven temperature and the Oven Program required.
3. Use Det menu to Set the required temperature and flow set point.
4. Use similar program for packed column conditioning with a column
flow of 20 ml/min for conditioning ( it should be less than working
flow)

Chapter 3
Checkout Using FID with PKD
Injector
• Scope
• Analytical Conditions required for packed Injection
• Recommended Initial Operations
• FID-PKD Checkout
Scope Use the following procedure to verify proper FID operation with the
Packed column Injector.
Parts Referenced Table 3.1 : FID-Packed Injector Parts Referenced
Part Description Part number

Test Column Packed Column 4 ft long 6372A4511
1/8’’ OD; 5% SE-30 on Chw-HP
Septum Standard septum for Packed injector L99838901
Syringes Standard 5 or 10 µl size; with 50 mm 523860920
needle length OR
523860926
Test Mixture Three components in n-Hexane:
Component Concentration
Dodecane : 200 µg/ml 102973445
Tetradecane : 200 µg/ml
Hexadecane : 200 µg/ml
Gases Chromatographic-grade purity
Data Acquisition Chrom-Card, Iris-32

Checkout Using FID with PKD Injector
Recommended Initial Operations
Recommended Before starting the checkout, the following operations should be

carried out:
Initial Operations
1. Connect/ensure proper gases are connected to your GC.
2. Replace the septum. A new septum should be installed properly in
your injector.
3. Connect the test packed column to your GC.
4. Measure suggested flow of carrier gas for column and other gases.
5. Connect your data handling. Verify that your data handling is
properly connected to your GC system.
Operating
Procedure FID- Packed Injector Checkout

required test.
2. Use OVEN menu to display the Column Oven parameters. Set
the oven temperature and the Oven Program required.
3. Use Det. menu to Set the required temperature and flow set point.
4. Activate your Data System and set the parameters required for the
checkout.
5. In the FID Detector Menu , scroll to SIGNAL and press mV
value followed by ENTER for Auto zero
6. Perform a blank analysis injecting pure hexane and press START
on the GC to begin the checkout run.
7. Inject the test mixture and press START on the GC to begin the
checkout run. The resulting chromatogram should look like the
one shown in Figure 2.1.
8. The following acceptance criteria indicates successful completion
of Packed-FID checkout according to the data handling in use.
9. If these criteria are not met, repeat the test.

Analytical Conditions Required for Packed Injector
Analytical Table 3.2
Conditions Parameters Setting

Injector Inj Temperature = 230 °C
Required for (Packed) Control Mode : Constant Flow
Packed Injector Carrier Gas: Helium or Nitrogen
Inlet Press = 30.0 ml/min (Constant Flow )
Oven Program Initial Temperature = 80 °C
Initial Time = 1 minute
Ramp 1 = 20 °C/minute
Final Time = 1 minute
Max Temperature = 300 °C
Injection Mode On column
Detector Det Temperature = 250 °C
Detector Range = 10^1
Hydrogen = 45 ml/min
Air = 300 ml/min
Injected Volume 1 µl + needle of Test Mixture
Aquisition Chrom-Card, Frequency = 10 Hz
Frequency

Fig. 3.1
Passing Crieteria : Area of Each Peak should be greater than

30,00,000 counts (uV) on Chromcard data acquisition system @ 10
Hz
While on Iris-32 Area of Each Peak should be greater than 300.000

counts (mV).
@ with Sample qty of Injection 1.0 microlitre

Chapter 4
Checkout Using FID with S/SL
Injector
• Scope
• Analytical Conditions Required for splitless injection
• FID-S/SL Checkout for splitless injection.
Split/ Splitless Injector.
Parts Referenced Table 4.1 : FID-S/SL Parts Referenced

Number
Test Fused Silica Capillary Column TR- 637260E113P
Column 5; 7 mt long 0.32 mm ID; 0.25 µm
film thickness.
Septum Standard septum for S/SL injector L99838901
needle length OR
523860926
Test Three components in n-Hexane:
Mixture Component Concentration
Data Chrom-Card, Iris-32 ,Computing-
Acquisition Integrator

Checkout Using FID with S/SL Injector
Analytical Conditions Required for Splitless Injection
Table 4.2 : FID-S/SL Analytical Conditions

Analytical
Required for
(Capillary ) Control Mode : Constant Flow
Splitless Injection Carrier Gas: Helium or Nitrogen
Split Operating Mode = Splitless
Splitless Time = 0.4 minutes
Split Flow = 60 ml/min
Septum Purge = 2 ml/min
Air = 300 ml/min
Make-up Gas: Nitrogen = 20 ml/min
Aquisition Frequency Chrom-Card, Frequency = 10 Hz

Recommended
Initial Operations Before starting the checkout, the following operations should be
carried out:
1. Check up the Splitless glass liner(208262940) installed in your
injector , it should be clean and free from any deposits or septum
particles if required clean it or replace with new one, with the
appropriate liner seal(208826974).
2. Replace the septum A new septum should be installed properly in
your injector.
3. Connect the required gas lines, Verify the required gas supplies
are properly connected to your GC.
4. Install the test column. The column currently installed should be
carefully removed and replaced with the required test column and
Perform Column Leak Test.
Operating
Procedure FID-S/SL Checkout in Splitless Mode

1. Use INJ menu and set the pressure value to have the required
carrier gas flow rate .
2. Use OVEN menu to display the Column Oven Control Table. Set
3. Use Split menu to display the appropriate Split/Splitless Control
Table.
checkout.
10. In the FID Detector Signal Control , scroll to SIGNAL and press
mV value followed by ENTER for Auto zero
one shown in Figure 4.1

Operating Procedure
Fig. 4.1
8. The following acceptance criteria indicate successful completion

of FID-S/SL checkout according to the data handling in use.
FID-S/SL Acceptance Criteria

Hz

counts (mV).

Chapter 5
Checkout Using FID with PTV
Injector
• Scope
• Analytical Conditions Required for PTV injection
• FID-PTV Checkout for PTV injection
PTV Injector.
Parts Referenced Table 5.1 : FID-PTV Parts Referenced

Number
Test Column Fused Silica Capillary Column 637260E113P
TR-5; 7 mt long
0.32 mm ID; 0.25 µm film
thickness.
Syringes 523860920
Standard 5 or 10 µl size; with 50 mm
needle length OR
523860926
Test Mixture Three components in n-Hexane:

Checkout Using FID with PTV Injector
Analytical Conditions Required for PTV Injection
Analytical Table 5.2 : FID-S/SL Analytical Conditions

Required for PTV
(PTV ) Control Mode : Constant Flow
Injection Carrier Gas: Helium or Nitrogen
Air = 300 ml/min
Frequency


carried out:
Initial Operations
1. Check up the PTV liner (208262928). The PTV liner installed in
your injector should be clean and free from any deposits or
septum particles ,if required clean it or replace with new one ,
with the appropriate liner seal.
your injector.
3. Connect the required gas lines, Verify the required gas supplies
carefully removed and replaced with the required test column and
Perform Column Leak Test.
Operating
Procedure FID-S/SL Checkout in PTV Mode

carrier gas flow rate.
3. Use Split menu to display the appropriate PTV parameters.
checkout.
6. In the FID Detector menu , scroll to SIGNAL and for press mV
value followed by ENTER key for Auto zero.

Operating Procedure
9. The following acceptance criteria indicate successful

completion of FID-PTV checkout according to the data
handling in use.
Fig. 5.1.
FID-PTV Acceptance Criteria

Hz

counts (mV).

Chapter 6
Checkout Using TCD with PKD
Injector
• Scope
• Analytical Conditions Required for TCD with PKD injection
• TCD-PKD Checkout for PKD injection
Scope Use the following procedure to verify proper TCD operation with the
Parts Referenced Table 6.1 : TCD-Packed Injector Parts Referenced
Part Description Part Number

Test Packed Column 4 ft long 6372A4511
Column 1/8’’ OD; 5% SE-30 on Chw-HP
Syringes Standard 5 or 10 µl size; with 523860920
50 mm needle length OR
523860926
Dodecane : 2000 µg/ml 102973446
Tetradecane : 2000µg/ml

Checkout Using TCD with PKD Injector
Table 6.2 TCD-Packed Injector Analytical Conditions

Analytical
Gases Carrier Gas (Helium) = 30 ml/min
Required for
Reference gas(He) = 30 ml/min
Packed Injector Make up gas(He) = 0.0 ml/min
Oven Program Initial Temperature = 80 °C ,
Final Temperature = 200 °C,
Injector Operating Mode = On-column
Temperature = 230 °C
Detector Base Temperature = 250 °C
Bridge Voltage =8.5 V
Bridge Current = 100 mA
Polarity = +
Detector Signal Range = 101
Analog Signal Iris-32 Data Acquisition system or any
Output other standalone CDS
Digital Signal Chrom-Card, Frequency = 10 Hz
Output
Recommended
Before starting the checkout, the following operations should be
Initial Operations
carried out:
your injector.
3. Connect the required packed column to your GC.
4. Measure suggested flow of carrier gas for column, reference and
Make up gases.

Operating Procedure
Operating
Procedure TCD- Packed Injector Checkout
required test.
2. Use OVEN menu to display the Column Oven Control Table.
Set the oven temperature and the Oven Program required.
4. Activate your Data System and set the parameters required for
the checkout.
5. In the TCD Detector menu, scroll to SIGNAL and press mV
value followed by ENTER for Auto zero
one shown in
Fig. 6.1

Operating Procedure
8. The following acceptance criteria indicate successful completion

of Packed-TCD checkout according to the data handling in use.
TCD-PKD Acceptance Criteria
Passing Crieteria : Area of Each Peak should be greater than 20,000

counts (uV) on Chromcard data acquisition system @ 10 Hz

counts (mV).

Chapter 7
Checkout Using TCD with S/SL
Injector
• Scope
• Analytical Conditions Required for TCD with splitless
injection
• TCD-S/SL Checkout for splitless injection
Scope Use the following procedure to verify proper TCD operation with the
Table 7.1 : TCD-S/SL Injector Parts Referenced

Test Fused Silica Capillary Column 637260E113P
Column TR-5; 7 mt long x0.32 mm ID; 0.25
µm film thickness.
needle length OR
523860926
Dodecane : 200µg/ml 102973445

Checkout Using TCD with S/SL Injector
TCD-S/SL Injector Analytical Conditions
Table 7.2 : TCD-S/SL Injector Analytical Conditions

TCD-S/SL Injector
Analytical Parameters Setting
Gases Carrier Gas (Helium) = 3.00 ml/min (Flow
Conditions mode)
Reference gas(He) = 30 ml/min
Make up gas(He) = 27.0 ml/min
Oven Program Initial Temperature = 60 °C ,Initial Time = 1
minute
Final Temperature = 200 °C,Final Time = 1
minute
Injector Operating Mode = Splitless
Split Flow = 60 ml/min ,
Bridge Voltage =8.0 V
Bridge Current = 100 mA
Detector Signal Range = 100
Polarity = +
Analog Signal Iris-32 Data Acquisition system or any
Output other standalone CDS
Digital Signal Chrom-Card, Frequency = 10 Hz
Output

carried out:
Initial Operations
your injector.
3. Connect the required Capillary column to your GC.
4. Measure suggested flow of carrier gas for column and other gases.
Operating
Procedure TCD-S/SL Checkout in Splitless Mode

Operating Procedure

Table.
checkout.
11. In the TCD Detector menu scroll to SIGNAL and press mV value
followed by ENTER for Auto zero
8. The following acceptance criteria indicate successful

completion of TCD-S/SL checkout according to the data
handling in use.

Operating Procedure
Fig. 7.1
TCD-S/SL Acceptance Criteria

20,000 counts (uV) on Chromcard data acquisition system @ 10 Hz

counts (mV).

Chapter 8
Checkout Using ECD with S/SL
Injector
• Scope
• Analytical Conditions Required for TCD with S/SL injection
• TCD-S/SL Checkout for S/SL injection
Scope Use the following procedure to verify proper ECD operation with the
Table 8.1 : ECD-S/SL Parts Referenced

TR-5; 7 mt long 0.32 mm ID;
0.25 µm film thickness.
Septum Standard septum for S/SL L99838901
injector
Syringes 523860920 OR
Standard 5 or 10 µl size; with 50 mm
needle length 523860926
Test Mixture ECD test Mixture in Iso-octane 102973442

Lindane : 0.033 µg/ml

Checkout Using ECD with S/SL Injector
Analytical Table 8.2 : ECD-S/SL Analytical Conditions

Required for
Splitless Injection Carrier Gas: Nitrogen
ECD Cell Temperature = 300 °C
Reference Current = 0.5 nA
Frequency

carried out:
Initial Operations
1. Ensure The splitless glass liner (P/N208262940) installed in your
injector with the appropriate liner seal.(P/N 208826974)
2. Replace the septum A new septum should be installed properly
in your injector.
3. Connect the required gas lines Verify the required gas supplies
carefully removed and replaced with the required test column.
5. Perform Column Leak Test.
6. Connect your data handling .Verify that your data handling is

Operating Procedure
Operating ECD-S/SL Checkout in Splitless Mode

Procedure

Table.
4. Use Det menu to Set the required temperature and flow setpoint.
checkout.
6. In the ECD Detector menu scroll to SIGNAL and press mV value

followed by ENTER for Auto zero.
7. Perform a blank analysis injecting pure iso-octane and press

START on the GC to begin the checkout run.

Fig 8.1
Passing Crieteria : Area of Lindane Peak should be greater than

50,00,000 counts (uV) on Chrom-card data acquisition system @ 10
Hz
While on Iris-32 Area of Lindane Peak should be greater than 500

counts (mV).
If these criteria are not met, repeat the test.

Chapter 9
Checkout Using NPD with S/SL
Injector
• Scope
• Analytical Conditions Required for TCD with S/SL injection
• NPD-S/SL Checkout for S/SL injection
Scope Use the following procedure to verify proper NPD operation with the
Table 9.1 : NPD-S/SL Parts Referenced

TR-5; 7 mt long
0.32 mm ID; 0.25 µm film
thickness.
Septum Standard septum for S/SL L99838901
injector
523860926
Test Mixture Azobenzene : 1 µg/ml
Methyl parathion : 1 µg/ml 102973443
Octadecane : 10000 µg/ml
in Hexane

Checkout Using NPD with S/SL Injector
Table 9.2 : NPD-S/SL Analytical Conditions

Analytical
Required for Injector Inj Temperature = 230 °C
Splitless Injection (Capillary ) Control Mode : Constant Flow
Carrier Gas: Nitrogen
Hydrogen = 4.5 ml/min
Air = 60 ml/min
NPD Supply Bias Voltage = 5.0 volt
NPD Source Current = 3.10 Amp (dial set 3.10)

Frequency


carried out:
Initial Operations
Ensure The splitless glass liner (P/N208262940) installed in your
7. Replace the septum A new septum should be installed properly

in your injector.
8. Connect the required gas lines Verify the required gas supplies
Operating
Procedure NPD-S/SL Checkout in Splitless Mode
Table.
Activate your Data System and set the parameters required for the
checkout.
12. In the NPD Detector menu , scroll to SIGNAL and press mV
value followed by ENTER for Auto zero.

Operating Procedure
Fig. 9.1
Passing Crieteria : Area of 1 ppm Azobenzene Peak should be

greater than 30,000 counts (uV) on Chrom-card data acquisition
system @ 10 Hz
While on Iris-32 Area of Azobenzene Peak should be greater than 30

counts (mV).
Area of 1 ppm Methyl Parathion Peak should be greater than

40,00,000 counts (uV) on Chrom-card data acquisition system @ 10
Hz
While on Iris-32 Area of Methyl Parathion Peak should be greater

than 400 counts (mV).
Selectivity :
Azobenzene to Octadecane should be > 2000 : 1
Methyl Parathion to Octadecane should be > 20000 : 1

Chapter 10
Checkout Using FPD with S/SL
Injector ( Sulphur mode)
• Scope
• Analytical Conditions Required for FPD with S/SL injection
• FPD-S/SL Checkout for S/SL injection
Scope Use the following procedure to verify proper FPD operation with the
Table 10.1 : FPD-S/SL Parts Referenced

Number
Test Fused Silica Capillary Column
Column TR-5; 7 mt long 0.32 mm ID; 0.25 µm 637260E113
film thickness. P
Standard septum for S/SL injector L99838901
523860926
Test Methyl parathion : 10 µg/ml 102973444
Mixture in Hexane
S- Filter FPD with Sulphur filter ( 393 nm) 525249984
P- Filter FPD with Phosphorous filter ( 526 nm) 525249985
Table 10.2 : FPD-S/SL Analytical Conditions ( S-mode)

Checkout Using FPD with S/SL Injector ( Sulphur mode)
Parameters Setting
Air-1 = 60 ml/min
Air-2 =160 ml/min
FPD Supply PMTVoltage = 500-600 volt
FPD PMT voltage = 5.50 (dial set approx,550 V)
Frequency

carried out:
Initial Operations

Operating Procedure
1. Ensure The splitless glass liner (P/N208262940) installed in your

2. Replace the septum. A new septum should be installed properly
in your injector.
3. Connect the required gas line Verify the required gas supplies
4. Install the test column.The column currently installed should be
Operating
FPD-S/SL Checkout in Splitless Mode
Procedure
Table.
4. Use Det menu to Set the required temperature and flow setpoint.
checkout.
6. In the FPD Detector menu scroll to SIGNAL and press mV value
followed by ENTER for Auto zero.
9. Typical Chromatograph of SOP Sample of 10 ppm Methyl
Parathion in Hexane FPD-S mode ( with Sulphur filter 393 nm )

Operating Procedure
Fig. 10.1
Passing Crieteria : Area of 10 ppm Methyl Parathion Peak should be

greater than 20,00,000 counts (uV) on Chrom-card data acquisition system
@ 10 Hz
While on Iris-32 Area of Methyl Parathion Peak should be greater than 200
counts (mV).
@ with Sample Qty of Injection 1.0 microlitre cold needle split less
injection .

Checkout Using FPD with S/SL Injector (Phosphorus mode)
Checkout Using
Shut off the FPD flame gases ,Cool down the FPD detector Replace
FPD with S/SL the Sulphur interference filter (P/N-525249984 ) by Phosphorous
Injector filter (P/N-525249985 ) and perform the FPD Phosphorus mode
(Phosphorus checkout for details please refer to service manual for detail
mode) procedure for changing filters in FPD detector
All other procedure, operating sequence are same as performed in S-

mode.
Table 10.2 : FPD-S/SL Analytical Conditions (P-mode)
Parameters Setting
Injected 1 µl + needle of Test Mixture
Volume
Air-1 = 60 ml/min
Air-2 =160 ml/min
FPD Supply PMT Voltage = 500-600 volt
FPD PMT voltage = 5.50 (dial set approx,550 V)
Frequency
Typical Chromatograph of SOP Sample of 10 ppm Methyl Parathion
in Hexane FPD-P mode ( with Phosphorous filter 526 nm )

Checkout Using FPD with S/SL Injector (Phosphorus mode)
Fig 10.2
Passing Crieteria : Area of 10 ppm Methyl Parathion Peak should

be greater than 1,00,00,000 counts (uV) on Chrom-card data
acquisition system @ 10 Hz
While on Iris-32 Area of Methyl Parathion Peak should be greater

than 1000 counts (mV).
@ with Sample Qty of Injection 1.0 microlitre cold needle split less

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Thermo Fisher Scientific

Published by Thermo Fisher Scientific India Pvt. Ltd.

Printing History: First Edition, released July 2013.

This publication is not part of the Agreement of Sale between

Reference to System Configurations and Specifications supersede all

Chapter 1 About This Manual ........................................................................... 1

Chapter 2 General Overview ............................................................................ 1

Chapter 3 Checkout Using FID with PKD Injector......................................... 1

Chapter 4 Checkout Using FID with S/SL Injector ......................................... 1

Chapter 5 Checkout Using FID with PTV Injector ......................................... 1

Thermo Fisher Scientific Trace 1110 SOP Guide i

Checkout Using TCD with PKD Injector ....................................... 1

Chapter 7 Checkout Using TCD with S/SL Injector ....................................... 1

Chapter 8 Checkout Using ECD with S/SL Injector ....................................... 1

Chapter 9 Checkout Using NPD with S/SL Injector........................................ 1

ii Trace 1110 User Guide Thermo Fisher Scientific

Conventions The following symbols and typographical conventions are used

Thermo Fisher Scientific Trace 1110 SOP Guide 1

Informational Informational symbols used in this manual and their meaning:

Some important information is given, which can be noted down

Warning pertaining to a possible explosion hazard.

Abbreviations for Table 1.1

2 Trace 1110 SOP Guide Thermo Fisher Scientific

WARNING! : Hydrogen is a harmful gas that mixed with air may

Precaution for the Electron Capture Detector

WARNING! : The Electron Capture Detector (ECD) contains a 63Ni

Preinstallation Manual : (PN 827S07132) this manual and diskette

Operating Manual : (PN 827S07130) this manual provides

Service Manual : (PN 827S07133) this manual contains instructions

Thermo Fisher Scientific Trace 1110 SOP Guide 3

Standard Operating Procedures : (PN 827S07134) this manual

Spare Parts Catalog : (PN 827S07133) this catalog contains a list of

The SOPs Overview section contains a general description of the

Chapter 2 General Overview contains a guideline to apply correctly

4 Trace 1110 SOP Guide Thermo Fisher Scientific

For specific operating or maintenance questions, please refer to

Thermo Fisher Scientific Trace 1110 SOP Guide 1

Part Description Part

Note : under un avoidable circumstances Nitrogen can be used as a

Getting Started Before starting checkout, perform the following preliminary

1. Gas Supply Connections : Connect the gas supplies following

2. Data Handling Connections : Connect your data handling

2 Trace 1110 SOP Guide Thermo Fisher Scientific

3. Column Installation : Install the test column according to the

• Preparing a Capillary Column

4. Glass Liner and Septum Installation : Install the glass liner

• Chapter 6: Split/Splitless Injector

Column conditioning consists of passing a flow of carrier gas through

Detector Connections This operation should be carried out at the end

Thermo Fisher Scientific Trace 1110 SOP Guide 3

• Connecting a Capillary Column to an FID, FPD or NPD

Before beginning, press CONFIG to verify the GC configuration:

4 Trace 1110 SOP Guide Thermo Fisher Scientific

Parts Referenced Table 3.1 : FID-Packed Injector Parts Referenced

Part Description Part number

Thermo Fisher Scientific Trace 1110 SOP Guide 1

Recommended Before starting the checkout, the following operations should be

Before beginning, press CONFIG to verify the GC configuration:

2 Trace 1110 SOP Guide Thermo Fisher Scientific