Gas Chromatograph
Gas Chromatograph
Gas Chromatograph
GAS CHROMATOGRAPH
P/N 03-914689-00
Rev 4
TABLE OF CONTENTS
I. GC OPERATION ...................................................................................................................................... 2
Overview ............................................................................................................................................................... 2
Instrument Setup................................................................................................................................................... 3
Building a Method ................................................................................................................................................. 4
Automation ............................................................................................................................................................ 5
Activating the GC Method ..................................................................................................................................... 5
Making a Single Injection ...................................................................................................................................... 6
Do You Need HELP? ........................................................................................................................................... 6
GC Status.............................................................................................................................................................. 7
GC Control ............................................................................................................................................................ 7
This guide is intended for the novice and experienced user. You will find this to be an invaluable reference for
setting up your GC, programming the system, and finding the most frequently needed part numbers.
Keep this guide near your GC for convenient reference.
1
I. GC OPERATION
Overview
The CP-3800 user interface is designed for maximum ease of use. The keyboard is laid out in functional sections
allowing quick access to the necessary information. There are 8 available methods, one of which must be active at
any given time. For more detailed information see the Operator’s Manual, CP-3800 Keyboard and Display.
CP-3800 Keyboard
2
Instrument Setup
Action
1. Press SETUP.
2. Choose View Setup/Edit Setup using cursor keys.
3. Press ENTER.
“View Setup” allows you to check the current Instrument Configuration. Choose “Edit Setup”
if you want to change the Instrument Configuration.
ACTIVE EDIT RUN END
METHOD METHOD CTRL TIME TIME
3
Building a Method
Follow these steps to build or edit a GC Method.
Action
1. Press EDIT from the Method section of the keypad.
2. Use the INCR or DECR keys to choose desired method.
3. Press ENTER.
Follow the method sections below to build your GC method. You can advance to any section by pressing the
appropriate section key.
4
The Following
Method Section ... Will allow you to modify these method parameters ...
DETECTOR Detector temperature
Range, and autozero (time programmable)
Detector time constant
TCD filament temperature and polarity (time programmable)
PFPD → PMT voltage, gate width + delay, trigger level
TSD bead current and power (time programmable)
ECD contact potential and cell current
Detector flow (EFC only)
SAMPLE DELIVERY/ 8400/8410 or 8200 Sampling Parameters
VALVE TABLE Timed programmed events for splitless injections
(manual 1177/1079 only), or switching valves
For GCs with valves, consult your custom plumbing diagram
for programming
Events for a typical split and splitless injection are as follows:
Automation
Selects Automation Mode
Method Automation Parameters
Priority Sample
NOTE: If you edit the active method, you must re-activate it before running an analysis.
5
Making a Single Injection
Use the following procedure if performing a single injection. If you are using the Star Chromatography
Workstation, refer to the instrument’s Operator’s Manual.
Confirm that the GC is in the Ready state. The amber “Ready” light should be illuminated.
Gas or Liquid Sampling Confirm the sampling valve is The gas or liquid sampling
Valve using an air in the fill position and the valve will rotate to the inject
actuator loop is loaded with sample. position and the GC method
Press START will start.
Pressing HELP gives the user an explanation for the specific parameter.
6
GC Status
The Instrument STATUS key allows the user to view the current status of the various components of the CP-3800
instrument. Note that the current status of individual components can also be viewed by pressing the relevant key in
the GC CONTROL keyboard section.
The primary status information provided using the STATUS key is the actual component temperature, carrier gas
flow and pressure (if EFC is installed), and detector analog output signal. The following is an example of a status
screen for a CP-3800 equipped with a 1079 injector and FID. Note that the status screen reflects the current state of
the instrument. If the instrument is running a method, the status fields will update as the values change during the
run at a rate of once per second. If a component is not ready or faulted, this will be indicated on the STATUS
screen. Note that the status screens are presented in location order, i.e., Front, Middle and Rear.
ACTIVE EDIT RUN END
METHOD METHOD CTRL TIME TIME
GC Control
When one of the six GC Control keys is pressed, the user is presented with a split display. The status information
reflecting the current status of the CP-3800 appears above the bold line on the display. The information beneath the
bold line is the method parameters of the EDIT METHOD. Note that the EDIT METHOD and the ACTIVE
METHOD may be different.
ACTIVE EDIT RUN END
METHOD METHOD CTRL TIME TIME
7
II. HARDWARE INSTALLATION & SETUP
Column Installation
Follow these steps to install the capillary column and set gas flow rates:
1. Cool all heated zones and replace depleted oxygen and moisture traps.
2. Replace critical injector inserts and septa.
3. Cut 2 cm from each column end.
4. Thread the nut and ferrule over the column on both ends. The ferrule should be installed
with the taper end into the nut.
5. Cut 2 cm from each column end to remove ferrule fragments.
6. Mount the capillary column in the oven.
7. Install the column 3.7 cm into the 1177 Injector or 7.5 cm into the 1079 Injector, measured from the back of the
nut. The 1041 and 1061 do not require measuring. They are installed all the way up into the injector.
8. Set the approximate column head pressure.
9. Set the split ratio and septum purge flows, 1177 and 1079 Injectors.
10. Connect the column to the detector at the appropriate distance (see Page 18).
11. Check for leaks using a leak detector. Do not use soaps or liquid-based leak detectors.
12. Set make-up and detector gas flow rates (see Page 10).
13. Set injector and detector temperatures. Do not exceed the column’s Tmax.
14. Condition the column at its recommended conditioning temperature for two hours.
15. Run test mixtures to confirm proper installation and column performance.
16. Calibrate instrument and inject samples.
03-926119-43
530 μm columns only
03-926119-44
Packed column insert
8
Optimum Capillary GC Carrier Flow Rate and Velocity
After conditioning your column, the carrier gas flow rate should be set for optimum separation of sample
components. Since the flow rate is dependent on column temperature in a pressure regulated system, it is important
to set the carrier gas at the same column temperature for a given analysis. For convenience, the carrier gas is often
set at the initial temperature of the analysis. For a slightly faster analysis and improved separation, set the optimum
flow rate at the maximum temperature of the analysis. For critical or hard to separate peak pairs in the
chromatogram, set the optimum linear velocity at the oven temperature where they elute.
If you have Electronic Flow Control installed in your GC, setting the column flows is as simple as entering the
column dimensions and carrier gas type in SETUP and building the appropriate flow or pressure program in the
Method.
If you don’t have EFC installed, inject 5 μL of a non-retained gaseous substance compatible with the detector
(Page 18). Calculate the column velocity, then flow rate and split ratio, if applicable, using the equations below.
Split Ratio =
Split vent flow (mL min )
Column flowrate (mL min )
Average Linear Velocity (μ, cm/sec)
9
Detector, Carrier, and Make-up Gas Flow Rates
and Gas Types
Use the following guide for determining the appropriate gases for your GC system and setting detector, carrier gas,
and make-up flow rates.
10
III. RECOMMENDED PARTS & SUPPLIES
Gas Filters
Carrier and detector filters should always be installed to further clean high purity gases, reduce detector noise, and
protect the chromatography system from potential contamination. The following filters are recommended for GC
systems:
Filter Description Part
Number
Moisture Gas Filter Installed between gas tank and GC inlet CP17971
Molecular sieve
Removes water vapor
Change filter when indicator shows filter is spent
Charcoal Gas Filter Installed between gas tank and GC inlet CP17972
Activated charcoal
Removes organic contaminants
Change filter when indicator shows filter is spent
Oxygen Gas Filter Installed between carrier gas filter and GC inlet CP17970
Removes oxygen and water vapor
Recommended with capillary columns
Required for ECD
Change filter when indicator shows filter is spent
11
Glass Injector Inserts
Capillary injector inserts have a direct effect on analysis results. They are chosen depending on the injection mode
(split, splitless, on-column, flash vaporization) and sample characteristics.
The split and splitless inserts create a homogenous mixture of sample and carrier gas, transfer a representative
sample into the column and minimizing molecular weight discrimination.
The on-column temperature programmable inserts for the 1079 provide quantitative sample transfer and retain
the liquid sample during cold sample introduction.
The flash vaporization insert (1061) provides an expansion volume for large samples and minimizes non-
volatile sample components from entering the column.
Insert variations for all injection modes are available for dirty sample matrices, labile compounds, and large volume
injections. Inserts should be replaced as soon as a loss in chromatographic performance is seen. Note that all the
1079 inserts are deactivated.
12
Mode Insert 1079 Description Part Number
Fritted Enhances sample mixing to ensure linear split,
3.4 mm ID instantaneous sample vaporization.
Split Mode 03-926119-46
Splitless Open Can be packed with quartz wool, glass beads, etc.
3.4 mm ID Can be used with the full range of capillary columns. 03-926119-45
Mode
(isothermal)
Splitless Open Trace analysis. The low surface area makes it ideal for
(Temperature 0.5 mm ID thermolabile and polar compounds. Used with narrow to
Ramp Mode) wide bore columns (50 - 320 µm). 03-926119-49
Split/Splitless Packed Deactivated glass wool packing. Can be used for split,
(Temperature 2 mm ID splitless and temperature ramp modes.
Ramp Mode) 03-926119-53
SPME Mode Open Mainly used with SPME, this insert is designed for
0.8 mm ID maximum analyte transfer from the SPME fiber. 03-926119-48
High Tapered The tapered internal design allows sealing 0.18 - 0.32 mm
Performance insert for ID capillary columns inside the insert. The low surface
Mode column area makes it ideal for thermolabile and polar compounds. 01-900109-06
sealing
On-Column Tapered On-column insert for large bore (0.53 mm) capillary
Mode insert for columns. Like the high performance insert the column is
column sealed within the insert. 01-900109-07
sealing
13
Septa
Septa allow the syringe needle to enter the GC injector, yet maintain a leak-free seal in the GC system. They are
available in several different types of materials and sizes depending on injector model and analysis needs. The
septum chosen for a GC analysis should exhibit low bleed, resist leaks, and be easy to pierce when performing
injections.
Septa should be changed every 50 to 100 injections or when you note a change in peak retention time or ghost
peaks. It is preferable to change septa routinely, rather than after leaks develop, thus minimizing instrument
downtime and sample loss. Change the septum at the end of the workday, then keep the column oven temperature
hot enough to prevent bleed from accumulating overnight. Using a needle guide, a syringe free of burrs, or an
autosampler will prolong the septum life because a single hole will be repeatedly pierced allowing easier re-sealing.
9.5 mm 11.5 mm
1041 On-column 1079 Injector
1061 Flash Vaporization
14
Column Quick Connect Kit
This kit simplifies the installation of capillary columns into Varian injectors and detectors. The kit contains split
capillary column nuts, reusable jacketed graphite ferrules (for 250μ, 320μ, 530μ ID columns) and a column depth
scale. No felt tip pen, typewriter correction fluid or tape is needed to mark column depth for any injector or
detector. The split nut design allows you to remove the nut from the column when the column is stored without
having to remove the ferrule. The split capillary column nuts are knurled so that all tightening can be done by hand.
No tools are required.
Description Quantity
Column Depth Scale 1 each
Knurled Split Nut 2 each
Graphite Jacketed Ferrule 2 each
(0.4 mm ID)
Graphite Jacketed Ferrule 2 each
(0.5 mm ID)
Graphite Jacketed Ferrule 2 each
(0.8 mm ID)
Spare Parts
15
IV. METHOD DEVELOPMENT
Recommended Solvents for Capillary Columns
The choice of solvents for a chromatographic analysis depends on the component solubility, detector, and the
polarity of the analytical column. Solvents should ideally match the polarity of the column, especially when
injecting large volumes and performing on-column or splitless injections. Non-polar columns perform best with
non-polar solvents. Polar columns perform best with polar solvents, however, they also perform well with non-
polar solvents.
Below are recommended solvents for non-polar, intermediate, and polar phase columns.
16
Recommended Injector and GC Parameters
Injector On-Column, Flash Vaporizing Split Splitless
(1041/1061) (1079/1177) (1079/1177)
Column For For For
Large Bore Capillary Columns All All
(530 μm ID) Capillary Capillary
Packed Columns
Columns Columns
17
Column Installation Measurements for Injectors & Detectors
Units of Measure
Weight/ Weight/ Volume/
Name Abbreviation weight volume volume
Parts per ‰ mg/g μg/μL mL/L
Thousand mg/mL
g/L
Parts per ppm μg/g ng/μL nL/mL
Million mg/kg μg/mL μL/L
mg/L
Parts per ppb ng/g pg/μL nL/L
Billion μg/kg ng/mL
μg/L
Parts per ppt pg/g fg/μL pL/L
Trillion ng/kg pg/mL
ng/L
Not to Scale
Varian, Inc.
2700 Mitchell Drive
Walnut Creek, CA 94598/usa
18
Other Quick Reference Items for your GC
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
_____________________________________________________________________________________
19