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Varian 450-GC User Manual

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

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Summary of Contents for Varian 450-GC

  • Page 1 Varian BV Varian BV Herculesweg 8 Herculesweg 8 4330 EA Middelburg 4330 EA Middelburg The Netherlands The Netherlands 450-GC 450-GC User Manual User Manual North/South America North/South America Europe Europe  Australia/East Asia  Australia/East Asia 2700 Mitchell Drive 2700 Mitchell Drive P.O.
  • Page 2 450-GC shuts down the affected component and reports the 450-GC shuts down the affected component and reports the Error  Error on page 84 on page 84. .  After correcting the E  After correcting the Error, normal ope...

  • Page 3: Software Products

    Varian to perform as described in the accompanying Operator's 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 Manual and to be substantially free of those defects which cause failure to execute respective programming instructions; however, Varian does not does not warrant uninterrupted or error-free operation.

  • Page 4: Safety Information

    For Safety Information in German, French, Italian or Spanish please refer to the 430-GC, the 430-GC, 431-GC and 450-GC User Manual CD-rom (CP501414) which is included with the GC. 431-GC and 450-GC User Manual CD-rom (CP501414) which is included with the GC.
  • Page 5 Ionizing radiation source is present. Follow manual Ionizing radiation source is present. Follow manual instructions for safe instructions for safe operation. operation. Keep hands and fingers away. Keep hands and fingers away. Varian, Varian, Inc. Inc. User User Manual Manual 450-GC 450-GC Page: Page: V V...

  • Page 6: General Safety Precautions

    It is the responsibilit y of th It is the responsibilit y of th e C e Customer to inf ustomer to inf orm Varia orm Varian Customer n Customer Support Representa Support Repre sentatives if tives if the instrum...

  • Page 7: Electrical Hazards

    (Varian (Varian Part Nu Part Number mber 03-91832 03-918326-00) and has 6-00) and has a pressure rating a pressure rating significantly greater than the highest significantly greater than the highest outlet pressure from the regulator.

  • Page 8: Gc Safety Practices

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

  • Page 9: Service Availability

    AVAILABILITY SERVICE AVAILABILITY SERVICE AVAILABILITY It is the policy of Varian to provide operational spare parts for any instrument and It is the policy of Varian to provide operational spare parts for any instrument and Varian provides a variety of...

  • Page 10: Ce Declaration Of Conformity

    Safety Information Safety Information CE DECLARATION OF CONFORMITY CE DECLARATION OF CONFORMITY Page: Page: X X User User Manual Manual 450-GC 450-GC Varian, Varian, Inc. Inc.

  • Page 11: Table Of Contents

    Table of Contents TABLE OF CONTENTS VARIAN ANALYTICAL INSTRUMENT WARRANTY..............III ......................III  ARDWARE RODUCTS .......................III OFTWARE RODUCTS ..........................I II EMEDIES ......................III IMITATION OF  ARRANTY ..................III IMITATION OF EMEDIES AND IABILITY SAFETY INFORMATION......................I V ..........................I V NFORMATION ......................I V...

  • Page 12: Table Of Contents

    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...
  • Page 13 1061 Electronic Flow Control (EFC) ic Flow Control (EFC) ..................................222 1061 Injector Insert..1061 Injector Insert..........................................224 Column Column Installation Installation ............................................224 Column Installation..Column Installation..........................................224 Page: Page: XVI User User Manual Manual 450-GC 450-GC Varian, Varian, Inc. Inc.
  • Page 14 Baking Out the Injector......................................248 SAMPLE PRECONCENTRA SAMPLE PRECONCENTRATION TRAP (SPT) TION TRAP (SPT) ............................251 Description..Description................................................2 51 SPT temperature zone..SPT temperature zone........................................252 Varian, Varian, Inc. Inc. User User Manual Manual 450-GC 450-GC Page: Page: XVII XVII...
  • Page 15 Clean the Flame Tip and Internal Parts..............................292 Replace the Flame-Tip Ferrule..Replace the Flame-Tip Ferrule....................................293 FID Test Chromatogr FID Test Chromatogram am........................................293 Page: Page: XVIII XVIII User User Manual Manual 450-GC 450-GC Varian, Varian, Inc. Inc.
  • Page 16 Bead Condi Bead Conditioning tioning..........................................307 Optimization of the TSD Using the Varian Test Samp Optimization of the TSD Using the Varian Test Sample le ....................309 Determining Optimu Determining Optimum Hydrogen Flow m Hydrogen Flow ................
  • Page 17 Gas Flow Rates tes ....................................363 Split Valve..Split Valve................................................3 63 PFPD Gas Flow Diagram with EFC15..PFPD Gas Flow Diagram with EFC15................................364 Page: Page: XX User User Manual Manual 450-GC 450-GC Varian, Varian, Inc. Inc.
  • Page 18 Emission Timing ............................................404 Flame Composition..Flame Composition..........................................404 Filte Filters rs ....................................................4 05 Selenium Selective Detectio Selenium Selective Detection n ......................................405 Varian, Varian, Inc. Inc. User User Manual Manual 450-GC 450-GC Page: Page: XXI...
  • Page 19 SHIPPING, CLEANING AND DISPOSAL INSTRUCT SHIPPING, CLEANING AND DISPOSAL INSTRUCTIONS IONS......................439 ..........................................439 HIPPING HIPPING NSTRUCTIONS NSTRUCTIONS ..........................................439 LEANING LEANING NSTRUCTIONS NSTRUCTIONS Page: Page: XXII XXII User User Manual Manual 450-GC 450-GC Varian, Varian, Inc. Inc.
  • Page 20 ..............................................477 APPENDIX APPENDIX A: A: ERROR ERROR CODES CODES ......................................4 79 APPENDIX APPENDIX B: B: PUBLIC PUBLIC STATEMENT..STATEMENT..................................491 Varian, Varian, Inc. Inc. User User Manual Manual 450-GC 450-GC Page: Page: XXIII XXIII...

  • Page 21: Rear Panel

    Table of Contents Table of Contents Page: Page: XXIV XXIV User User Manual Manual 450-GC 450-GC Varian, Varian, Inc. Inc.

  • Page 22: Figures

    ......................41 IGURE IGURE ONNECTOR ONNECTOR 10: O O ............................................43 IGURE IGURE PTION PTION OARD OARD 11: 450-GC 450-GC B B ........................89 IGURE IGURE  ACK  ACK PANEL PANEL THERNET THERNET ONNECTION ONNECTION 12: P P ......

  • Page 23: Fuses Common

    HROMATOGRAM 61: TSD T ................421 IGURE HROMATOGRAM 62: TCD T ................422 IGURE HROMATOGRAM 63: ECD T ................423 IGURE HROMATOGRAM 64: PFPD P M ..............424 IGURE HROMATOGRAM 65: PFPD S M ..............425 IGURE HROMATOGRAM Page: XXVI User Manual 450-GC Varian, Inc.

  • Page 24: Tables

     ATES FOR 42: 1041 I ...........214  ABLE NJECTOR HROMATOGRAPHIC TESTING CONDITIONS 43: 1061 C 1/16" ..............221  ABLE OLUMN ERRULES  X  MM 44: C 1061 F ..........226  ABLE  ARRIER  AS  ATES FOR LASH NJECTOR Varian, Inc. User Manual 450-GC Page: XXVII...
  • Page 25 60: O PFPD..................400  ABLE PTIMUM LOW RATES 61: D ..................419  ABLE ETECTOR  AMPLES 62: M ..................427  ABLE  AINTENANCE REQUENCY 63: V ..................431  ABLE  ARIAN  AS LEAN ILTERS 64: I ..................433  ABLE NJECTOR  AKEOUT  ARTS Page: XXVIII User Manual 450-GC Varian, Inc.

  • Page 26: 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: alternating current...

  • Page 27: Installation

    (in (in case case of of EFC). EFC). Table 1: Hydrogen as Carrier Gas during Power off Table 1: Hydrogen as Carrier Gas during Power off Page: Page: 8 8 User User Manual Manual 450-GC 450-GC Varian, Varian, Inc. Inc.

  • Page 28: General Laboratory Precautions

    • • Turn Turn off the off the hydrogen hydrogen at its at its source source if a if a power power failure failure occurs. occurs. Varian, Varian, Inc. Inc. User User Manual Manual 450-GC 450-GC Page: Page: 9 9...

  • Page 29: Install Gas Regulators And Set Pressures

    ″ ″ back very slightly and tighten 3/4-turn past back very slightly and tighten 3/4-turn past finger-tight with a 7/16 finger-tight with a 7/16  wrench.  wrench. Page: Page: 10 User User Manual Manual 450-GC 450-GC Varian, Varian, Inc. Inc.

  • Page 30: Installing The Cp-8400/8410 Autosampler

    Installing the CP-8400/8410 AutoSampler Installing the CP-8400/8410 AutoSampler To install your CP-8400/8410 on a 450-GC, first unpack the AutoSampler and To install your CP-8400/8410 on a 450-GC, first unpack the AutoSampler and verify that all of verify that all of the parts required are present.

  • Page 31: Connect Gc To Power

    Plug the GC power-cord into an appropriate source of power. Plug the GC power-cord into an appropriate source of power. Varian supplies a numb rian supplies a numb er of power-cords qualifi er of power-cords qualifi ed to be used ed to be used with the power load of the GC.

  • Page 32: Column Installation And Conditioning

    Glass Injector Injector, , 4 4 mm mm ID, ID, unpacked, unpacked, single single gooseneck gooseneck 03-92611927 03-92611927 Table 3: Factory-Installed Injector Inserts Table 3: Factory-Installed Injector Inserts Varian, Varian, Inc. Inc. User User Manual Manual 450-GC 450-GC Page: Page: 13...

  • Page 33: Nuts And Ferrules For Capillary Columns

    CR211125 CR211125 0.53 0.53 mm mm ID CR214108 CR214108 CR212108 CR212108 CR213108 CR213108 CR211108 CR211108 SG073302 SG073302 Table 4: 1/16” Column Ferrules Table 4: 1/16” Column Ferrules Page: Page: 14 User User Manual Manual 450-GC 450-GC Varian, Varian, Inc. Inc.

  • Page 34: Connect Capillary Column To Injector

    Capillary column column ferrule ferrule Properly Properly cut cut column column end Improperly Improperly cut cut column column ends ends Figure 1: Column Ends Figure 1: Column Ends Varian, Varian, Inc. Inc. User User Manual Manual 450-GC 450-GC Page: Page: 15...
  • Page 35 12. Partially insert the column into the lower end of the Injector. Thread up the Partially insert the column into the lower end of the Injector. Thread up the capillary column nut and ferrule capillary column nut and ferrule finger-tight. finger-tight. Page: Page: 16 User User Manual Manual 450-GC 450-GC Varian, Varian, Inc. Inc.

  • Page 36: Tips For Tightening Column Ferrules

    Not recommended for 1041/1061/1093 Not recommended for 1041/1061/1093 Table 6: General Tightening and Re-tightening for Common Ferrules Table 6: General Tightening and Re-tightening for Common Ferrules Varian, Varian, Inc. Inc. User User Manual Manual 450-GC 450-GC Page: Page: 17...

  • Page 37: Nuts And Ferrules For Packed Columns

    • 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. Page: 18 User Manual 450-GC Varian, Inc.

  • Page 38: Varian Test Column

      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. For use with Column Descripti on...

  • Page 39: Split Vent Flow And Septum Purge Flow

    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.
  • Page 40 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. Varian, Inc. User Manual 450-GC Page: 21...

  • Page 41: Set Carrier Gas Flow Rate To Condition Column

    Temperature bakeout of Injectors on page 433. To prevent c ontamination and overheating of t he fused sili ca column, the colum n must NOT be connected to t he Injector dur ing the Injector bake-out procedure. Page: 22 User Manual 450-GC Varian, Inc.

  • Page 42: Column Conditioning

    Af ter the column f low is established, allow t he carrier gas to purge through t he column for 15 - 20 minutes before heating it. Varian, Inc. User Manual 450-GC Page: 23...

  • Page 43: Connect Capillary Column To Detector

    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.

  • Page 44: Connect Metal Packed Column To Detector

    Never use soaps, such as Snoop®. These may cont aminate 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...

  • Page 45: Basic Operation

     At points th roughout th is sec ti on, sp ecifi c v alues and conditi ons are given for analysis of t he Varian test samples on Varian test columns . Your analytical c olumn and application may require different values and conditi ons.
  • Page 46   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.

  • Page 47: 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.

  • Page 48: Method To Analyze A Varian Test Sample On A Varian Test Column

      Installation Method to Analyze a Varian Test Sample on a Varian Test Column Test Sample Part Number Concentrati ons of Test Compoun ds μ μ 82-005048-01 3.00 L of C  and C  in iso-octane. μ 82-005048-02 33.0 pg/ L of lindane and aldrin in iso-octane.

  • Page 49: Prepare The Test Sample

    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.

  • Page 50: Solvents For Gc

    Intermediate Ethyl Acetate 56.5 50% Phenyl, 50% Methyl Acetone Methyl iso-butyl ketone 127.0 81.6  Acetonitrile 64.7 Polar  Methanol Polyethyene Glycol Ethanol 78.5 2-Propanol 82.5 117.7 n-Butanol Table 15: Recommended Solvents for Gas Chromatography Varian, Inc. User Manual 450-GC Page: 31...

  • Page 51: Sample Volume And Injection Rate

    μ Use 1 L 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 52: Reference

    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.

  • Page 53: Peripheral Connectors

    Fuse F2, 6.3A, T see on page 44 J302 Temperature Probes Thermocouples for the Fuse F1, 6.3A, T see on page 44 Heaters See on page 37 Figure 3: Connectors for Peripheral Equipment Page: 34 User Manual 450-GC Varian, Inc.

  • Page 54: J504/J505 S.i.d. 1 And 2

    Peripheral Connectors 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...

  • Page 55: 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.

  • Page 56: J302 Temperature Probes

    Peripheral Connectors Top View J302 TEMPERATURE PROBES Temperature probe connectors for Heaters Figure 6: Connector J302 Varian, Inc. User Manual 450-GC Page: 37...

  • Page 57: J45/J46 Auxiliary 1 And 2

    Peripheral Connectors 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.

  • Page 58: J44 Cryo Valves (3)

    Peripheral Connectors J44 CRYO VALVES (3) 24 VDC Cryo valve connections Top View See Fuses on page 44 Figure 8: Connector J44 Varian, Inc. User Manual 450-GC Page: 39...

  • Page 59: J42/J43 External Events

    J42/J43 EXTERNAL EVENTS Timed 24 Volt (DC) contacts (7) connector, for more (optional) contacts see Option Board on page 43. See Fuses on page 44 See Fuses on page 44 Figure 9: Connector J42/J43 Page: 40 User Manual 450-GC Varian, Inc.

  • Page 60: J41 Heater Connections

    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...
  • Page 61 Use the correct (included) screws (metric) to mount t he 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...
  • Page 62  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.
  • Page 63 Injector(s) and reinstall the 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 Top- Cover.
  • Page 64 12. The base is secured to the Top-Cover via 2 (short) screws at the rear and 3 (long) screws underneath the AutoSampler/AutoInjector sample- carrousel/tray. 13. Plug the connector of the power/communication cable into the CP-8400/8410. Page: 108 User Manual 450-GC Varian, Inc.
  • Page 65 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, resulti ng in bent syrin ge needles. Varian, Inc. User Manual 450-GC Page: 109...
  • Page 66 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 commu nicati on betw een 450-GC and the Sampler. Do not turn off the Sampler power switch du ring normal operations.
  • Page 67 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...
  • Page 68 - Vial calibration, on page 113. - GC Injector calibration, on page 116. If during Calibration a question mark appears in a yellow triangle, this wil l indicate that the calibration is not corr ect! Page: 112 User Manual 450-GC Varian, Inc.
  • Page 69 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 i s s elected. Varian, Inc. User Manual 450-GC Page: 113...
  • Page 70 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.
  • Page 71 9. Press “Exit” button to exit the calibration screen, without saving the calibration data. If the used Vial is shorter/longer then the calibration t ool it ’s advisable to repeat only the Syringe calibration. Varian, Inc. User Manual 450-GC Page: 115...
  • Page 72 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.
  • Page 73 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...
  • Page 74 10. Press the “Exit” button if calibration is finished or leaving the calibration page without saving is needed. The “ Reset Calibration” button wi ll restore the factory settings to all calibration values. Page: 118 User Manual 450-GC Varian, Inc.
  • Page 75 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...
  • Page 76 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.
  • Page 77 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 78 The SPME Samplin g mo de can not be selected by the 450-GC display/keyboard. In order to configure th e system to use SPME you must set a switch on t he syringe sled to the correct posit ion and install the special SPME fiber hol der block.
  • Page 79   AutoSamplers SAMPLE DELIVERY PARAMETERS The 450-GC Sample Delivery page has parameters that represent the 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.
  • Page 80 - Plunger Speed Down (µL/s) 62.5 - Volume For Fill Strokes (µL) 0.75 3.75 37.5 187.5 - Number Of Clean Strokes - Viscosity Delay (s) Draw Sample - Plunger Speed During Fill (µL/s) - Viscosity Delay (s) Page: 124 User Manual 450-GC Varian, Inc.
  • Page 81 - Plunger Speed Up (µL/s) - Plunger Speed Down (µL/s) 62.5 If used: Any Pre-Injection Sample Clean Flushes (sample  waste) → - Volume (µL) 0.75 3.75 37.5 187.5 - Viscosity Delay (s) - Plunger Speed Up (µL/s) Varian, Inc. User Manual 450-GC Page: 125...
  • Page 82 The Neat sampling mode performs the following sequence of actions:  Al l Cl eanStr ok es- and Flush -Volumes are limi ted to 75% of t he syr inge capacity. Page: 126 User Manual 450-GC Varian, Inc.
  • Page 83 Observe the white switch, which wil l be just exposed once the sled has reached it s maximum downward travel. Set to SPME (UP-position) Push sledge down until switch appears Varian, Inc. User Manual 450-GC Page: 143...
  • Page 84 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.
  • Page 85 GC injector) and GC injector) Figure 17: SPME Syringe When performin g liq uid SPME, make sure that the fi ber sheath does NOT contact the liqui d. This may result in carry-over. Varian, Inc. User Manual 450-GC Page: 145...
  • Page 86 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.
  • Page 87 Penetration depth 60% SPME Adsorption Time The SPME adsorption time is the period between agitation strokes. If the  strokes is 0, the SPME adsorption time is equal to the number of agitation sampling time. Varian, Inc. User Manual 450-GC Page: 147...
  • Page 88 Sampling time = (5+0.01)*(10+1) is approx. 55 min Optimum analytical yield results are obtained wit h an adsorption ti me that is s et to 0. The sampling time is determined by th e number of agitation strokes only. Page: 148 User Manual 450-GC Varian, Inc.
  • Page 89 The switch on the sampler tower, mounted on the sled, must be set in the STD (Liquid Sampling) mode. Liquid Sampling “syringe” holder Syringe switch Figure 18: Liquid Sampling Syringe and Holder Figure 19: SPME/Standard Switch Varian, Inc. User Manual 450-GC Page: 149...
  • Page 90 Observe the white switch, which wil l be just exposed once the sled has reached it s maximum downward travel. Push sledge down Set to Liquid Sample until switch appears (DOWN-position) Page: 150 User Manual 450-GC Varian, Inc.
  • Page 91 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...
  • Page 92  AutoSamplers Page: 152 User Manual 450-GC Varian, Inc.
  • Page 93 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...
  • Page 94 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.
  • Page 95 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...
  • Page 96 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.
  • Page 97 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...
  • Page 98 Injectors – 1177 Split/Splitless Capillary Injector Figure 21: EFC21 and 1177 in Splitless mode Flow Diagram See Pencil Filters on page 437 Page: 158 User Manual 450-GC Varian, Inc.
  • Page 99 Injector. This allows the EFC25 to be used with Purge and Trap devices between EFC and Injector. Figure 22: EFC25 and 1177 Flow Diagram See Pencil Filters on page 437 Varian, Inc. User Manual 450-GC Page: 159...
  • Page 100 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 t he various modes of injection.
  • Page 101 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 key on the 450-GC keyboard. Varian, Inc. User Manual 450-GC Page: 161...
  • Page 102 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.
  • Page 103 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. Varian, Inc. User Manual 450-GC Page: 163...
  • Page 104 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.
  • Page 105 1177 Split/Splitless Capillary Injector - Injectors 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.
  • Page 106 (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.
  • Page 107 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 Concentrati ons of Test Compoun ds μ...
  • Page 108  I I n n  c c o o m m b b i i n n a a t t i i o o n n  w w i i t t h h  t t h h e e  P P F F P P D D  d d e e t t e e c c t t o o r  r    t t h h e e  S S i i l l t t e e k k  l l i i n n e e r  r    ( ( R R T T 2 2 1 1 0 0 4 4 6 6 2 2 1 1 4 4 5 5 ) )  m m u u s s t t  b b e e  u u s s e e d d . . Page: 170 User Manual 450-GC Varian, Inc.
  • Page 109 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...
  • Page 110 4. Condition the insert by setting the 1177 Injector to the split mode and ° purging with carrier gas for 30 min at 300 Page: 172 User Manual 450-GC Varian, Inc.
  • Page 111 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...
  • Page 112 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.
  • Page 113 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.
  • Page 114 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.
  • Page 115 CR213124 CR211124 0.25 mm ID and smaller SG073300 CR214105 CR212105 CR213105 CR211105 SG073301 0.32 mm ID CR212125 CR213125 CR211125 0.53 mm ID CR214108 CR212108 CR213108 CR211108 SG073302 Table 33: 1079 Column Ferrules 1/16" Varian, Inc. User Manual 450-GC Page: 177...
  • Page 116 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 µL of sample. Page: 178 User Manual 450-GC Varian, Inc.
  • Page 117 Injector is ramped to transfer the sample onto the column. The 1093 OC Injector  , on page 231 is optimized for On- Column applications. Especially for applications operating at an oven temperature range that require short wire-bore columns. Varian, Inc. User Manual 450-GC Page: 179...
  • Page 118 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.
  • Page 119 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...
  • Page 120 Injector. This allows the EFC25 to be used with Purge and Trap devices upstream from the Injector. Figure 26: EFC25 and 1079 Flow Diagram See Pencil Filters on page 437 Page: 182 User Manual 450-GC Varian, Inc.
  • Page 121 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 a 1079 PTV 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.
  • Page 122 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...
  • Page 123 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...
  • Page 124 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. Page: 186 User Manual 450-GC Varian, Inc.
  • Page 125 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...
  • Page 126 Injectors – 1079 PTV Injector Septum Purge Calibration The 450-GC is equipped with a septum purge for the Model 1079 PTV Injector and is controlled by a manual needle valve. This is located behind the front cover of the GC.
  • Page 127 1079 PTV Injector - Injectors Manual Pneumatics Tools and equipment needed • Bubble or electronic flowmeter, e.g., Varian Intelligent Digital Flowmeter, 01- 900115-00. 1. Turn the 1079 PTV Split Flow Controller (on the GC pneumatics panel) counterclockwise to open the split flow controller.
  • Page 128 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.
  • Page 129 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.
  • Page 130 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”...
  • Page 131 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).
  • Page 132 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 133 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.
  • Page 134 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.
  • Page 135 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.
  • Page 136 - 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.
  • Page 137  t t h h e e  f  f  a a u u l l t t  a a g g a a i i n n  i i n n  t t h h e e  n n e e x x t t  r  r  u u n n . .  I I t t  a a l l s s o o  p p r  r  e e v v e e n n t t s s  a a  w w o o r  r  k k s s t t a a t t i i o o n n  s s t t a a r  r  t t i i n n g g  a a  r  r  u u n n  w w h h i i l l e e  F F I I D D  i i g g n n i i t t i i o o n n  i i s s  s s t t i i l l l l g g o o i i n n g g  o o n n . . Varian, Inc. User Manual 450-GC Page: 287...
  • Page 138 Graphite/Vespel 40/60 max. 400°C (CR213200) Graphite (100%) max. 450°C (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.
  • Page 139  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...
  • Page 140 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.
  • Page 141 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...
  • Page 142 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.
  • Page 143 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.
  • Page 144 Detectors – Flame Ionization Detector (FID) Page: 294 User Manual 450-GC Varian, Inc.
  • Page 145 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.
  • Page 146 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 He continuum, neon exhibits a low ionization efficiency and low detector response. Page: 296 User Manual 450-GC Varian, Inc.
  • Page 147 Pulsed Discharge Helium Ionization Detector (PDHID) - Detectors 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...
  • Page 148 Exploded View Ground electrode (CP740764) Nut for ground electrode (CP914060) Spanner tool (CP740760) Detector cell (CP740765) High voltage cable (CP740763) Bias Cable assy (CP740761) Electrometer cable assy (CP740773) Figure 50: PDHID Exploded View Page: 298 User Manual 450-GC Varian, Inc.
  • Page 149 Pulsed Discharge Helium Ionization Detector (PDHID) - Detectors 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...
  • Page 150 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. Page: 300 User Manual 450-GC Varian, Inc.
  • Page 151 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. Varian, Inc. User Manual 450-GC Page: 301...
  • Page 152 • • Metal Metal forceps. forceps. • • Teflon Teflon combustor combustor extraction extraction device. device. • • Teflon Teflon tweezers. tweezers. • • Lab tissues. tissues. Varian, Varian, Inc. Inc. User User Manual Manual 450-GC 450-GC Page: Page: 357...
  • Page 153 (Item 13 er (Item 13) ) from the detector tower. Discard this from the detector tower. Discard this used crunch washer. used crunch washer. Page: Page: 358 User User Manual Manual 450-GC 450-GC Varian, Varian, Inc. Inc.
  • Page 154 360 insert the column on page 360, ignoring the instructions regarding use of ignoring the instructions regarding use of the Column Depth Gauge. the Column Depth Gauge. Varian, Varian, Inc. Inc. User User Manual Manual 450-GC 450-GC Page: Page: 359...
  • Page 155 Page: Page: 360 User User Manual Manual 450-GC 450-GC Varian, Varian, Inc. Inc.
  • Page 156 Phillips-head screwdriver. screwdriver. • • 9/64" 9/64" Allen Allen wrench. wrench. • • Teflon Teflon combustor combustor extraction extraction device. device. • • Metal Metal forceps. forceps. Varian, Varian, Inc. Inc. User User Manual Manual 450-GC 450-GC Page: Page: 361...
  • Page 157 PFPD with the quartz combustor just installed. combustor just installed. • • If If No No, the PFPD is ready for operation. , the PFPD is ready for operation. Page: Page: 362 User User Manual Manual 450-GC 450-GC Varian, Varian, Inc. Inc.
  • Page 158 If the PFPD If the PFPD Detector EFC option is installed on your 450-GC, detector gas Detector EFC option is installed on your 450-GC, detector gas flows are flows are set by...
  • Page 159 Split valve valve Wall Wall flow flow (H  + Air1 + Air2)  + Air1 + Air2) Center Center flow flow (H  + Air1)  + Air1) Igniter Igniter cap Page: Page: 364 User User Manual Manual 450-GC 450-GC Varian, Varian, Inc. Inc.
  • Page 160 Write down and save the dial setting for the setting for the Air1  Air1 mass flow  mass flow controller valve. controller valve. Turn the Air1 Turn the  Air1 flow controller Off.  flow controller Off. Varian, Varian, Inc. Inc. User User Manual Manual 450-GC 450-GC Page: Page: 365...
  • Page 161 " to 1/16" redu /16" reducing un cing union). Use ion). Use Teflon thread tape to make a gas-tight seal. Teflon thread tape to make a gas-tight seal. Page: Page: 366 User User Manual Manual 450-GC 450-GC Varian, Varian, Inc. Inc.
  • Page 162 Pulsed Flame Photometric Detector (PFPD) - Detectors  A Varian Int ellig ent Digit al Fl owmeter is hi ghly recommended fo r thi s 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.
  • Page 163 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.
  • Page 164 If you don’t 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...
  • Page 165 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 Gate Delay Gate Width...
  • Page 166 Setting the gate correctly prevents the h ydrocarbon and phosphorus responses from overlapping as the flame propagation slows in hydrocarbon-rich flames. Varian, Inc. User Manual 450-GC Page: 371...
  • Page 167 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. Varian, Inc. User Manual 450-GC Page: 407...
  • Page 168 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.
  • Page 169 Sulfur + Phosphorus mode: Use the optional WG-345 glass filter. Item 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...
  • Page 170 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.
  • Page 171 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...
  • Page 172 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.
  • Page 173 The split vent outlets are located on the left side panel of the 450-GC. Seal the septum purge by removing the outlet fitting fr om the septum purge valve and replacing it with a blank off plug (P/N SWB200P).
  • Page 174 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.
  • Page 175 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...
  • Page 176 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.
  • Page 177 Maintenance Page: 438 User Manual 450-GC Varian, Inc.
  • Page 178 SHIPPING, CLEANING AND DISPOSAL INSTRUCTIONS SHIPPING INSTRUCTIONS If you r 450-GC for any reason m ust s end back to the nearest Varian, Inc. subsidi ary or Varian, Inc. representative, it is v ery important to follow these additional preparation inst ructions : 1.
  • Page 179 Shipping, Cleaning and Disposal Instructions Page: 440 User Manual 450-GC Varian, Inc.
  • Page 180 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 Starter Kit 392611978 1 ea vials with 11 wide hole snap caps with Ultra septa) Varian, Inc. User Manual 450-GC Page: 441...
  • Page 181 392575001 1 ea SPME Parts 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 Page: 442 User Manual 450-GC Varian, Inc.
  • Page 182  P P l l e e a a s s e e  r  r  e e f  f  e e r  r    t t o o  L L i i n n e e r  r  / / I I n n s s e e r  r  t t  D D e e s s c c r  r  i i p p t t i i o o n n  o o n n  p p a a g g e e  4 4 4 4 5 5 Varian, Inc. User Manual 450-GC Page: 443...
  • Page 183 Liner for SPME Splitless insert SPI glass liner with packed glass wool Glass column guide for 3400, 3500, 3600 Glass column guide for 3700, 450-GC Split/Splitless liner with glass wool Split liner packed with 10% OV-101 on Chromosorb WHP 80/100...
  • Page 184  P P l l e e a a s s e e  r  r  e e f  f  e e r  r    t t o o  L L i i n n e e r  r  / / I I n n s s e e r  r  t t  D D e e s s c c r  r  i i p p t t i i o o n n  o o n n  p p a a g g e e  4 4 4 4 5 5 Varian, Inc. User Manual 450-GC Page: 445...
  • Page 185 Replacement Replacement Parts Parts 1177 Injector  1177 Injector  Deactivated Varian Injector Liners Deactivated Varian Injector Liners Goosene Gooseneck split/splitless Injector Liner, 2 MM ck split/splitless Injector Liner, 2 MM ID, 392611926 392611926 5/pk 5/pk modified 2 MM modified 2 MM...
  • Page 186 No Picture available No Picture available SGE splitless inlet liner, 2 SGE splitless inlet liner, 2 MM ID, Straight-through, MM ID, Straight-through, SG092004 SG092004 5/pk 5/pk Quartz Quartz Page: Page: 450 User User Manual Manual 450-GC 450-GC Varian, Varian, Inc. Inc.
  • Page 187 3.4 mm fritted Injector 3.4 mm fritted Injector insert for enhanced mixing for insert for enhanced mixing for 392611946 392611946 5/pk 5/pk linear split linear split performance performance Varian, Varian, Inc. Inc. User User Manual Manual 450-GC 450-GC Page: Page: 451...
  • Page 188 SG092038 SG092038 5/pk 5/pk SGE Splitless Splitless 2 2 mm mm ID ID inlet inlet liner, liner, single single taper taper SG09203 SG092039 9 5/pk 5/pk Page: Page: 452 User User Manual Manual 450-GC 450-GC Varian, Varian, Inc. Inc.
  • Page 189 1061, 1/4” 1/4” glass glass columns columns 03-925586-91 03-925586-91 Note that these kits contain Injector and detector adapters Note that these kits contain Injector and detector adapters Varian, Varian, Inc. Inc. User User Manual Manual 450-GC 450-GC Page: Page: 453...
  • Page 190 Liner No Picture Available No Picture Available 0.8mm ID, 0.5mm restriction SPI deactivated Injector 0.8mm ID, 0.5mm restriction SPI deactivated Injector SG092034 SG092034 5/pk 5/pk Liner Liner Page: Page: 454 User User Manual Manual 450-GC 450-GC Varian, Varian, Inc. Inc.
  • Page 191 03-925160-00 Combustor support, Combustor support, 2 2 mm 03-925178-00 03-925178-00 Combustor support, Combustor support, 3 3 mm 03-925179-01 03-925179-01 Combustor support Combustor support seal seal 03-925138-00 03-925138-00 Varian, Varian, Inc. Inc. User User Manual Manual 450-GC 450-GC Page: Page: 455...
  • Page 192 Replacement Parts Replacement Parts Page: Page: 456 User User Manual Manual 450-GC 450-GC Varian, Varian, Inc. Inc.
  • Page 193  S  S r   T  h  E r   M r   T  N r  Varian, Varian, Inc. Inc. User User Manual Manual 450-GC 450-GC Page: Page: 457...
  • Page 194 If a problem exists which cannot be If a problem exists which cannot be identified and/or corrected, call your identified and/or corrected, call your nearest Varian Service Center for nearest Varian Service Center for assistance. assistance. Sympto Sympto m m...
  • Page 195 μ  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-to- detector crossover connection (d)detector crossover-to- Varian, Inc. User Manual 450-GC Page: 459...
  • Page 196 High boiling compounds, C Wrong flame tip. Change to ceramic flame through C , not eluting tip, P/N 03-918351-00. Syringe hits insert Glass insert installed upside Reverse glass insert. down (wrong end facing up). Page: 460 User Manual 450-GC Varian, Inc.
  • Page 197 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.
  • Page 198 ) )  t t h h e e  E E r  r  r   r  o o r  r    l l e e v v e e l l  i i s s  E E r  r  r   r  o o r  r  , ,  i i n n  a a l l l l  o o t t h h e e r  r    c c a a s s e e s s  a a n n  A  Al l e e r  r  t t  i i s s  g g i i v v e e n n . . Page: 480 User Manual 450-GC Varian, Inc.
  • Page 199 Shorted sensor. Defect Sensor H2 flow set to 0.0 Check Column Oven zone mL/min Electronics off (all) Zone 1 Shorted Sensor Error Shorted sensor. Defect Sensor H2 flow set to 0.0 Check zone (1) mL/min Varian, Inc. User Manual 450-GC Page: 481...
  • Page 200 Zone 2 Max Temper Exceeded Error Defect Sensor H2 flow set to 0.0 Check zone (2) mL/min Electronics off (all) Zone 3 Max Temper Exceeded Error Defect Sensor H2 flow set to 0.0 Check zone (3) mL/min Page: 482 User Manual 450-GC Varian, Inc.
  • Page 202 Hazardous by default, basis of all AIN10V out of tolerance Error  measurement in system P5V ref out of tolerance Error  P2V5 ref out of tolerance Error  Page: 488 User Manual 450-GC Varian, Inc.
  • Page 203 CTS4 out of tolerance Error  Electronics off (all) H2 flow set to 0.0 mL/min CTS5 out of tolerance Error  CTS6 out of tolerance Error  Tref out of tolerance Error  Step motor moving Error  Option Board Errors Varian, Inc. User Manual 450-GC Page: 489...
  • Page 204  Appendix A: Error Codes Analogoutput buffer underrun Alert Buffer underrun Analogoutput buffer overflow Alert Buffer overrun Notification Message Analogoutput communication error Alert Notification Message Optionboard external events error Alert Notification Message Page: 490 User Manual 450-GC Varian, Inc.
  • Page 205 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”...

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