Varian CP-3800 GC Getting Started Manual
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Varian CP-3800 GC Getting Started Manual

Gas chromatography
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CP-3800 GC
Getting Started Manual


Getting Started
Installation
Basic Operation

Maintenance
Parts and Supplies
Varian Analytical Instruments
2700 Mitchell Drive
Walnut Creek, CA 94598-1675/usa
©Varian, Inc. 1999
Printed in U.S.A.
03-914647-00:Rev. 4
1

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  • Page 1 CP-3800 GC Getting Started Manual Getting Started Installation Basic Operation Maintenance Parts and Supplies Varian Analytical Instruments 2700 Mitchell Drive Walnut Creek, CA 94598-1675/usa ©Varian, Inc. 1999 Printed in U.S.A. 03-914647-00:Rev. 4...
  • Page 2 Read Before Operating Important Safeguards C A U T IO N 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. •...

  • Page 3: Table Of Contents

    Note for Capillary Column Users ..................35 Conditioning the Injector and Column ................35 Connect Capillary Column to Detector ................36 Column Insertion Depths for Varian Detectors..............37 Connect Metal Packed Column to Detector ..............38 Check for Leaks .......................38 CP-3800 GC Getting Started Manual...
  • Page 4 Setting Carrier and Detector Gas Flow Rates ..............39 Condition the GC System ....................41 Build a Method to Analyze a Test Sample ................41 Method to Analyze a Varian Test Sample on a Varian Test Column........42 Prepare the Test Sample..................... 43 Solvents for GC ........................43 Sample Volume and Injection Rate ..................
  • Page 5 Figure 6 Flame Ionization Detector Assembly .................69 Figure 7 Thermionic Specific Detector Assembly ..............71 Table 1 Physical Dimensions of the 3800 GC System Components ........10 Table 2 Flow Rates for Carrier and Detector Gases for the 3800 Gas Chromatograph..39 CP-3800 GC Getting Started Manual...

  • Page 6: Introduction

    Guide to the 3800 User Manuals The purpose of these User Manuals is to provide instructions for the safe installation and operation of the Varian 3800 Gas Chromatograph. The 3800 is supplied with two user manuals: a Getting Started Manual Finding and an Operator’s Manual.

  • Page 7: Brief Description Of The 3800 Gas Chromatograph

    Brief Description of the 3800 Gas Chromatograph The following are some of the key features of the 3800: • Three injectors, columns and detectors can be installed and operated simultaneously. • The 1079 Universal Capillary Injector provides five modes of injection - isothermal split and splitless, temperature ramped splitless, on-column and large volume.

  • Page 8: Configuration And Options

    Installed options on the 3800 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. CP-3800 GC Getting Started Manual...

  • Page 9: Installation

    Fuses There are four fuses accessible on the top of the 3800: F1: 6.3A T, F2: 6.3A T, F3: 10.0A F, F4: 6.3A T CP-3800 GC Getting Started Manual...

  • Page 10: Space Requirements

    2000m, however, the 3800 is designed for use at higher altitudes. Varian GCs should be protected from corrosive chemicals or gases, dust/ particulate accumulation, and direct venting of air conditioners, heaters, furnaces or fans.

  • Page 11: Peripheral Connectors

    2, 25 pin “D” connector, typically used for autosampler control. Analog Out, for connection to data handling devices that handle analog signals such as integrators, 15 pin “D” connector. Figure 1 Connectors for Peripheral Equipment CP-3800 GC Getting Started Manual...

  • Page 12: Gc Installation

    Handling Peripherals • If the Varian Star Chromatography Workstation with 3800 control is being installed follow the installation instructions in the communications section of the 3800 Operator’s manual. This installation simply involves making a connection to the Ethernet®...

  • Page 13: Select Gases

    3/4-turn past finger-tight with a 7/16″ wrench. 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. CP-3800 GC Getting Started Manual...

  • Page 14: Connect Gc To Power

    Front Ferrule Swagelok® Nut Cylinder Regulator Back Ferrule 1/8" Copper Tubing 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. Make sure the gas supply control valve, which controls gas pressure to the GC, is completely closed.

  • Page 15: Quick Guide To The 3800 Keyboard And Display

    Because the pertinent information cannot always fit on one screen, multiple pages are sometimes used. Where multiple pages are used this is always indicated on the title line of the display, e.g., Column Oven, Page 1 of 2. CP-3800 GC Getting Started Manual...
  • Page 16 TABLE E DIT If you are modifying a table such as a temperature ramp table or N EW D ELE T E C LEA R timed events table, the TABLE EDIT keys can be used to add new LIN E LIN E TA BLE lines to the table, delete the highlighted line from the table, or clear...
  • Page 17 (  )""# #* $$ '  + '  + Time and Date is used to update to the current local time and date. Selection of the desire date format and language for display is also performed here. CP-3800 GC Getting Started Manual...
  • Page 18 Heated Zones identify the type of device installed in each of the heated zones of the 3800, the upper temperature limit of these devices, their location and what type of coolant, if any, the device uses. Column oven always occupies one heated zone. The other available heated zones are numbered 1 through 6 and can be occupied by one of the following devices: 1079 injector, 1041 injector, 1061 injector, SPT, FID, TCD, ECD, TSD, PFPD, Micro-TCD, large valve oven, small valve oven, or methanizer.
  • Page 19 Note that the valves are normally identified on the 3800 display by their abbreviation, but when the display cursor is placed on a specific valve its full name is given on the prompt line of the display. CP-3800 GC Getting Started Manual...
  • Page 20 Valve Type Abbr. Default State (-) Activated State (+) Front Split Valve ON (split) OFF (splitless) Middle Split Valve ON (split) OFF (splitless) Rear Split Valve ON (split) OFF (splitless) Gas Sampling Valve Fill Inject Liquid Sampling Valve Fill Inject Sample Internal Standard Surrogate Standard...
  • Page 21 The column oven status field is shown at the top of the screen. Note that the stabilization time is also shown. This represents the period of time for which the instrument will stabilize after reaching its set temperatures and before going to the ready state. CP-3800 GC Getting Started Manual...
  • Page 22 ACTIVE EDIT CTRL METHOD METHOD TIME TIME          01 2: %  01 2: % ,)#" 01 2: % ,)#" 01 2: % ;"<  02: ;"<  02: "# -': - "# -': - -/ -& = 5  6...
  • Page 23 When the split state is ON, the sample is split in the injector with typically the smaller fraction entering the column and the larger fraction being vented. CP-3800 GC Getting Started Manual...
  • Page 24 The example shown below is a splitless injection with EFC pneumatics. In this case the injector is held in the split OFF state for a period of time at the beginning of the run (the sampling time). The injector is then switched to the split ON state, typically after 0.5 - 1.5 minutes, to vent the injector of any residual solvent.
  • Page 25 250°C. 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. CP-3800 GC Getting Started Manual...
  • Page 26 FLO W / If the 3800 is equipped with Electronic Flow Control, then pressing the P R E S S U R E FLOW/PRESSURE key will bring up the screens associated with programming EFC. EFC modules are identified by type and location to coincide with the sample delivery or injection device with which they are associated.
  • Page 27 The first three operate the same as described above for the 1079. Stabilization time is the time taken for the column oven to stabilize at its set temperature before allowing the GC to go to the ready state. CP-3800 GC Getting Started Manual...
  • Page 28 D E TE C TO R The 3800 detector methods generally have two method parameter pages and an additional adjustments page. The adjustments page is generally used for advanced features of the specific detectors and also for setting detector gas flows, if EFC is installed.

  • Page 29: Column Installation And Conditioning

    (2), and graphite jacketed ferrules (2 each of 0.4, 0.5 and 0.8 mm ID, for 250 µm, 320 µm, and 530 µm columns respectively). CP-3800 GC Getting Started Manual...
  • Page 30 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 the following table. Part Number Ferrule ID Fitting Size Column ID...

  • Page 31: Connect Capillary Column To Injector

    Finger-tighten the column nut while holding the column in place, then tighten a further 1/4 to 1/2-turn with a 5/16″ wrench. CP-3800 GC Getting Started Manual...

  • Page 32: Nuts And Ferrules For Packed Columns

    • Metal packed columns are usually installed with a metal 2-piece ferrule. Nuts and Ferrules for (A commonly used metal packed column is 1/8″ OD stainless steel. It Packed uses a 1/8″ ID stainless steel ferrule.) Columns • Glass packed columns are 1/4″ OD and are installed with a graphite front ferrule and a metal back ferrule installed backwards.

  • Page 33: Varian Test Column

    Column Installation and Conditioning At points throughout this manual, specific values and conditions are given Varian Test for the analysis of Varian Test Samples on Varian Test Columns. The Column following table provides information on Varian Test Columns. Varian Test Columns...

  • Page 34: 1079 Split Vent Flow And Septum Purge Flow

    Whether you are making an injection in the split or splitless mode, a split 1079 Split Vent vent flow rate needs to be set. In this example, the split vent flow is set to Flow and 100 mL/min. The split state is set in the Injector section of the 3800 Septum Purge method if EFC is installed and in the VALVE TABLE section of SAMPLE Flow...

  • Page 35: Note For Capillary Column Users

    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. CP-3800 GC Getting Started Manual...

  • Page 36: Connect Capillary Column To Detector

    In this example the injector and column are conditioned at 250°C for two hours. The column is programmed to 250°C at 5°C/min as a gentle temperature program is generally recommended for column conditioning. After this conditioning is complete, allow the column oven to cool and re- tighten the column nut attaching the column to the injector.

  • Page 37: Column Insertion Depths For Varian Detectors

    F used S ilica C olum n 3.9 cm 9 .5 cm 9.7 cm 10.5 cm For the Micro-TCD, the end of the column should be flush with the end of the ferrule when installed on the detector fitting. CP-3800 GC Getting Started Manual...

  • Page 38: Connect Metal Packed Column To Detector

    Place the column into the base of the detector. Thread 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.

  • Page 39: Basic Operation

    IMPORTANT Note: 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.
  • Page 40 The following instructions are for instruments configured with manual pneumatics. Gas flows for detectors with EFC are set in the Adjustments Section of the detector method. Follow the steps below to set all gas flow rates on the 3800 Gas Chromatograph.

  • Page 41: Condition The Gc System

    • 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. CP-3800 GC Getting Started Manual...

  • Page 42: Method To Analyze A Varian Test Sample On A Varian Test Column

    T . See Column Manufacturer’s specifications for your column. For Systems with 1041/1061 Injectors: Method Settings to Analyze Varian Test Samples on Varian GCs Installed with Varian Test Columns Note: Capillary columns use a temperature program while packed columns use isothermal conditions.

  • Page 43: Prepare The Test Sample

    8200/SPME AutoSampler Operator’s Manual, P/N 03-914692-00. You may inject your sample neat or diluted in a solvent. The Varian PFPD test sample should be diluted 1:20 in iso-octane if you intend to use it for a splitless injection.

  • Page 44: Sample Volume And Injection Rate

    Recommended Solvents for Gas Chromatography Column Phase Recommended Solvent Boiling Point (° C) • Non-Polar 36.1 Pentane • • 69.0 100% Methyl n-Hexane • • 80.7 5% Phenyl, 95% Methyl Cyclohexane • 99.3 Iso-octane • 80.1 Benzene • 110.6 Toluene •...

  • Page 45: Inject The Test Sample

    Inject the Test Sample Inject the Test Sample Use 1µL 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.

  • Page 46: Maintenance

    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 carried out on a routine basis.

  • Page 47: General Gc 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.
  • Page 48 (P/N 16-000154-00). Seal the split vent outlet by installing a Swagelok union on the outlet tube and sealing it with a blank off plug. CP-3800 GC Getting Started Manual...
  • Page 49 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 rear panel of the 3800. Varian supplies several types of carrier gas purifiers. These include a combined moisture / hydrocarbon trap, indicating moisture trap, and indicating or non- indicating oxygen traps.
  • Page 50 Use the following procedure to install or replace a carrier gas purifier on the 3800. Gas purifiers supplied by Varian and most other chromatography suppliers are equipped with 1/8″ Swagelok fittings. This facilitates easy removal and replacement of purifiers. In addition gas purifiers are sealed at both ends for protection.

  • Page 51: Injector Maintenance

    The following are the gas purifiers available from Varian. Purifier Part Number High capacity oxygen trap 03-949770-02 Indicating oxygen trap 88-501019-00 Combined hydrocarbon and moisture trap 03-949862-00 Indicating moisture trap 01-900007-00 The injector is the component of the Gas Chromatograph that requires the Injector most frequent maintenance.

  • Page 52: 1079 Injector

    AINTENANCE 1079 Injector Use the following procedure to change a septum on any Varian injector: Cool the column oven and injector oven to 50°C. This ensures safe handling of injector parts and protects the column from elevated temperatures while it is exposed to air.
  • Page 53 Refer to the figure below when removing and/or replacing the glass insert. Injector Nut Septum Septum Purge Septum Support Graphite Ferrule Carrier Gas Inlet Split Vent Glass Insert Fused Silica Column Capillary Column Nut Vespel® Ferrule Point of Injection Tools Required •...

  • Page 54: Remove The Glass Insert

    Note: The glass inserts can be cleaned and reused. Unless the graphite ferrule is obviously damaged, it can be reused as well. However, replace the 5 mm graphite ferrule after the glass insert has been changed three or four times. CP-3800 GC Getting Started Manual...

  • Page 55: Replace The Glass Insert

    Septum Support Insert Ferrule Glass Insert Insert/ferrule Insert/ferrule positioning tool positioning tool Follow these steps to replace the glass insert in the 1079 Injector. Replace the Glass Insert Use the insert/ferrule positioning tool supplied in the 1079 accessory kit to set the 5 mm graphite ferrule on the insert and in the septum support.

  • Page 56: Clean The Glass Insert

    Note: Rinsing the glass inserts with strong acids or bases or heating to a high temperature will remove the deactivation coating on the glass inserts. Rinsing the glass inserts with solvents or mixed solvents will not remove the deactivation coating. CP-3800 GC Getting Started Manual...

  • Page 57: Deactivate The Glass Insert

    Follow these steps to deactivate the glass insert in the 1079 Injector. Deactivate the Glass Note: This procedure can be used on all glass inserts except inserts packed Insert with 10% OV-101 on Chromosorb W-HP (P/N 03-918956-00). Up to three inserts can be deactivated at a time using this procedure.

  • Page 58: Injector

    Set the Relay to the split mode. If the flow meter indicates a flow less than previously measured, the injector has a leak. 12. Turn the column oven back on by pressing the “TURN OVEN ON” softkey in the column oven section of the method. CP-3800 GC Getting Started Manual...

  • Page 59: 1041 Injector

    1041 Injector Hardware Routine cleaning and maintenance of the 1041 Universal Injector system includes septum replacement and column conditioning. Pressure testing Replacement and leak checking procedures are included to assure proper functioning of and Cleaning the system. Procedures Septum replacement represents the major part of routine chromatographic Septum maintenance.
  • Page 60 For normal use, rinse the needle/syringe by slowly drawing up and quickly Needle/ expelling solvent or the next sample to be used. Repeat the process several Syringe times. Cleaning Note: When rinsing with the next sample, DO NOT expel sample back into the sample container. CP-3800 GC Getting Started Manual...

  • Page 61: Leak Checking

    Leak checking methods used with the 1041 Universal Injector are presented Leak in order of overall sensitivity and performance. When leak checking the Checking injector only, be sure to use the appropriate procedure. Remove the test column and plug the injector outlet with a 1/16″ no- hole ferrule (P/N 28-694503-00).

  • Page 62: Injector

    The syringe must be leak tight. To check the syringe, insert the needle in an injector operating at 20 to 30 psig with a no-hole ferrule. Place a drop of solvent at suspect leak locations and look for bubbles. CP-3800 GC Getting Started Manual...

  • Page 63: 1061 Injector

    1061 Injector 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.

  • Page 64: Remove The Glass Insert

    If this does not happen there is an indication of a leak. Condition the insert by setting the 1061 Injector temperature to 300°C and allowing the system condition for 30 minutes. CP-3800 GC Getting Started Manual...

  • Page 65: Clean The Glass Insert

    Glass inserts must be clean and free from sample residue and particulate Clean the matter (such as bits of septum rubber or graphite). Follow these steps to Glass Insert clean the glass insert of the 1061 Injector. Remove the glass insert. It is safest to cool the injector to 50°C before removing the insert.
  • Page 66 Cover the beaker with aluminum foil and bake at 200°C for 1 hour. After the inserts cool to room temperature, store them in a clean screw cap glass vial or the original packaging. CP-3800 GC Getting Started Manual...

  • Page 67: Flame Ionization Detector

    Flame Ionization Detector 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. If the FID noise increases with frequent spikes, the internal parts may be Clean the fouled and need to be cleaned.
  • Page 68 350°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 350°C. CP-3800 GC Getting Started Manual...

  • Page 69: Clean The Flame Tip And Internal Parts

    Thermionic Specific Detector When the TSD exhibits low sensitivity or high background noise, Cleaning/ cleaning is indicated. Visual inspection may also indicate a need for Maintenance 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.

  • Page 70: Thermionic Specific Detector

    Thermionic Specific Detector Signal Cable Signal Probe Bead Supply Cable Bead Probe Ceramic Bead Collector Ceramic Insulators TSD Tower Flame Tip Aluminum Crunch Washer Detector Base Column Ferrule Column Nut Figure 7 Thermionic Specific Detector Assembly CP-3800 GC Getting Started Manual...

  • Page 71: Electron Capture Detector

    Note: Although all heated zones on the 3800 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.)

  • Page 72: Thermal Conductivity Detector

    Pulsed Flame Photometric Detector For PFPD maintenance procedures see the PFPD Operator’s Manual, P/N 03-914649-00. Micro Thermal Conductivity Detector The Micro-TCD is not user serviceable and has no replacement parts. CP-3800 GC Getting Started Manual...

  • Page 73: Parts And Supplies

    In the USA and Canada, call 1-800-926-3000. Parts and • Supplies … In Europe, call your local Country office. • In the rest of the world, call your local Varian representative • Or, contact Varian on the Internet at http://www.varian.com Injectors 1079 Injector Description...

  • Page 74: Injector

    1041/1061 Injector 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 Note that these kits contain injector and detector adapters Packed Column Adapter Kit for 1/4” glass columns 03-925586-91 Packed Column Adapter Kit for 1/4”...

  • Page 75: Thermal Conductivity Detector

    Combustor support, 2 mm 03-925178-00 Combustor support, 3 mm 03-925179-00 Combustor support seal 03-925138-00 Micro-TCD Ferrule, 0.25 mm ID CP85888 Ferrule, 0.4 mm ID CP85889 Ferrule, 0.5 mm ID CP470100 Ferrule, 0.8 mm ID CP470101 CP-3800 GC Getting Started Manual...

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