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03-914647-00:4

Recommended Solvents for Gas Chromatography

Column Phase

Recommended Solvent

Boiling Point

(

°

C)

Non-Polar

•

Pentane

36.1

•

100%

Methyl

•

n-Hexane

69.0

•

5% Phenyl, 95% Methyl

•

Cyclohexane

80.7

•

Iso-octane

99.3

•

Benzene

80.1

•

Toluene

110.6

•

Ethyl

Ether

34.6

•

Methyl tert-butyl ether

55.2

•

Methylene

Chloride

39.8

•

Chloroform

61.2

•

Carbon

Disulfide

46.5

Intermediate

•

Ethyl

Acetate

77.0

•

50% Phenyl, 50% Methyl

•

Acetone

56.5

•

Methyl iso-butyl ketone

127.0

•

Acetonitrile

81.6

Polar

•

Methanol

64.7

•

Polyethyene

Glycol

•

Ethanol

78.5

•

2-Propanol

82.5

•

n-Butanol

117.7

Sample Volume and Injection Rate

The quality of your chromatogram can be greatly affected by the sample
volume and injection rate. These vary according to the type of injector and
column you are using. Shown below are some recommended sample
volumes and injection rates. Draw the appropriate volume of sample into
your syringe and inject at specified rate.

Injector

On-Column, Flash Vaporizing
(1041/1061)

Split
(1079)

Splitless
(1079)

Column

For

•

Large-bore Capillary Columns

(0.53 mm ID)

•

Packed Columns

For
All
Capillary
Columns

For
All
Capillary
Columns

Sample
Volume in

µ

L

•

0.1-1

•

1

-

5

0.2-1

1-5

Injection Rate,
in

µ

L/sec

•

0.5-5

•

1

-

10

5

1

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Содержание CP-3800 GC

Страница 1: ...ed in U S A 03 914647 00 Rev 41 CP 3800 GC Getting Started Manual Getting Started Installation Basic Operation Maintenance Parts and Supplies Varian Analytical Instruments 2700 Mitchell Drive Walnut C...

Страница 2: ...tector Heating an ECD to elevated temperatures without carrier or make up gas flowing through it can damage the ECD cell This can happen inadvertently especially when the ECD is not in use For this re...

Страница 3: ...ect GC to Power 14 Turn Power On 14 Factory Default States and Settings 14 Quick Guide to the 3800 Keyboard and Display 15 Getting Around the Keyboard 15 Column Installation and Conditioning 29 Connec...

Страница 4: ...s Insert 56 Clean the Glass Insert 57 Deactivate the Glass Insert 58 1041 Injector 60 Hardware Replacement and Cleaning Procedures 60 Septum Replacement 60 Needle Syringe Cleaning 61 Leak Checking 62...

Страница 5: ...Flame Photometric Detector 77 Micro TCD 77 Figure 1 Connectors for Peripheral Equipment 11 Figure 2 3800 GC Keyboard 15 Figure 3 1079 Injector Cross Sectional View 54 Figure 4 1041 Injector Assembly...

Страница 6: ...on intended to familiarize the new user with the 3800 The Operator s Manual contains more detailed information including information on the specific installed options on the 3800 Abbreviations The fol...

Страница 7: ...n Trap MS Large swing out pneumatics for easy access Seven heated zones and seven external events for maximum flexibility and custom configurations Up to eight separately programmed and stored analyti...

Страница 8: ...If a valve oven is installed it normally replaces two injector positions Any combination of three detectors can be installed with the following exceptions Only two TCD or PFPD detectors can be instal...

Страница 9: ...ied with an IEC 320 style socket The power cord assembly can be changed to suit your local power and socket requirements In the United States and Japan the instrument is equipped with a fixed power co...

Страница 10: ...ns of the 3800 GC System Components Height Width Depth Weight Instrument in cm in cm in cm lb kg 3800 GC 20 51 26 66 22 56 95 43 8200 AutoSampler 20 51 6 16 16 41 24 11 Tekmar 3000 Purge and Trap 19 4...

Страница 11: ...ear Panel Ethernet Connector BNC connector for 10 base 2 cable Printer Connector 25 pin D connector intended for future use AC Power Input 230V units only Top of Instrument under detector cover J4 Sam...

Страница 12: ...caps plugs and restraints Prior to operating remove Shipping dowel for oven fan motor from hole in GC rear panel Detector tower plugs under detector cover Gas bulkhead fitting plugs on rear panel Any...

Страница 13: ...to 100 psi low pressure stage Set cylinder regulator pressure to match the GC gas inlet pressures listed below Gas Inlet Pressure Carrier gas 80 psi Make up 80 psi Air 60 psi H2 40 psi Connect Gases...

Страница 14: ...fer to page 9 Turn Power On Turn on the GC power switch located at the top left of the GC The GC display should illuminate after a few moments and go through an initialization sequence The 3800 automa...

Страница 15: ...OVEN DETECTOR OUTPUT METHOD SEQUENCE SELECT EDIT PRIORITY SAMPLE METHOD AUTOMATION ACTIVATE SINGLE METHOD EDIT MENU NOT READY READY RUN START STOP STATUS SETUP MENU 7 8 9 4 5 6 1 2 3 0 SUSPEND RESUME...

Страница 16: ...value is entered In the latter case the ENTER key must be pressed again to advance to the next parameter A more convenient way to enter parameters is to use the cursor keys to move from one field to...

Страница 17: ...d column parameters or verify the instrument configuration If the instrument configuration is changed such as when adding a field upgrade kit the instrument SETUP screens must be updated The same scre...

Страница 18: ...detectors the location also refers to the relative positions of the detector electrometers installed on the main electronics board By default zones 1 2 and 3 are identified as front middle and rear a...

Страница 19: ...e Autocalibrate softkey This procedure should be carried out every six months or when a new EFC module is installed Failure to AutoCalibrate may cause a mis match between set and actual flowrates resu...

Страница 20: ...page allows changing the polarity of the Ready In sync signal Also if an FID electrometer is installed it allows enabling disabling of the flameout diagnostics STATUS The Instrument STATUS key allows...

Страница 21: ...the above status information specific status information on individual components can be accessed by pressing the relevant key on the 3800 keyboard For example to view the current status of the column...

Страница 22: ...tive method and the method being edited are identified on the top line of the 3800 display A method is edited by entering method parameters into the various components of the GC CONTROL keyboard secti...

Страница 23: ...TIME 01 2 01 2 01 2 01 2 34 5 6 34 5 6 The above screen represents the temperature settings for the 1079 injector operated in typical isothermal mode If the injector were temperature programmed a new...

Страница 24: ...io is reduced to 5 1 after 1 5 minutes The 1079 SPLIT STATE screen is accessed by pressing the PAGE DOWN key on the 3800 keyboard until page 3 of 3 is presented ACTIVE METHOD EDIT METHOD CTRL RUN TIME...

Страница 25: ...njector if installed Enable coolant refers to the temperature at which the coolant is turned on when the injector is set to a specific temperature For example if the injector is cooling from 300 C to...

Страница 26: ...the Sample Introduction section of the 3800 Operator s Manual ACTIVE METHOD EDIT METHOD CTRL RUN TIME END TIME 0 2 7 0 8 2 0 2 7 0 8 2 0 8 2 7 0 8 2 0 8 2 7 0 8 2 66 66 5 6 5 6 0 2 0 2 0 8 2 0 8 2 0...

Страница 27: ...0 2 0 2 3 3 66 66 Page 2 of the Column Oven parameters consists of fixed parameters which are rarely changed These consist of coolant on off coolant activation temperature coolant time out and stabili...

Страница 28: ...The following is an example of an FID method For the FID the only adjustments item is the detector time constant Fast or Slow ACTIVE METHOD EDIT METHOD CTRL RUN TIME END TIME 01 2 01 2 5 0 2 01 2 01 2...

Страница 29: ...of applications If your application calls for a different insert replace the factory installed insert prior to installing your column Refer to the Injector section of the Operator s Manual for instruc...

Страница 30: ...10 pk Polyimide Graphite 10 pk No hole 1 16 fitting 28 694503 01 28 694590 01 0 4 mm 1 16 fitting 50 250 28 694586 01 28 694583 01 28 694580 01 0 5 mm 1 16 fitting 320 03 908361 01 28 694561 01 28 69...

Страница 31: ...ool 1 2 2 4 cm from end of the column Inspect the cut to verify it is square and smooth 5 Move nut and ferrule to within 5 cm of column end For 1079 injector except on column modes Measure and mark co...

Страница 32: ...n use by installing the appropriate adapters 1 Place nuts and ferrules on both ends of column as shown in the previous diagram 2 If your column is metal insert it into the injector fitting and gently...

Страница 33: ...factory through the rear bulkhead fittings into the inlet manifold then to the pneumatic controls in the pneumatics compartment The pneumatic controls can be either electronically controlled EFC or m...

Страница 34: ...key to access the SPLIT STATE screen page 3 of 3 When Electronic Flow Control is installed in addition to programming the split state the split ratio can also be programmed 4 Set the initial split sta...

Страница 35: ...for Capillary Column Users Verify gas is flowing through the column by dipping the detector end of column into a beaker containing a solvent such as isopropanol Positive carrier gas flow should be in...

Страница 36: ...ate table should only consist of the initial line Verify that the split ratio is set to 100 To condition the column press the COLUMN key in the GC CONTROL section of the 3800 keyboard and build the fo...

Страница 37: ...k this distance Refer to diagram below for correct distances DO NOT let the column nut and ferrule fall past this mark The marking medium can contaminate the ferrule Column Insertion Depths for Varian...

Страница 38: ...ocate the packed column detector adapter in the Packed Column Kit and install on the inlet to the detector The TCD inlet is designed for packed column installation 2 Insert the open end of the packed...

Страница 39: ...ned flow is typically 30 mL min Table 2 Flow Rates for Carrier and Detector Gases for the 3800 Gas Chromatograph Detector Carrier Gas Carrier Gas Flow Rate mL min Packed Capillary Make Up Gas Make Up...

Страница 40: ...ing the flow controller knob fully counter clockwise or until the turns counting dial reads zero 3 Observe reading on flowmeter Ensure it is within the range described in the table for carrier gas flo...

Страница 41: ...nd that there is no split time program Set the split ratio to 100 2 Press the COLUMN key and set the initial column oven temperature to 250 C 3 Press the DETECTOR key and set the detector oven tempera...

Страница 42: ...column s Tmax 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 Colu...

Страница 43: ...less Split Initial split state OFF On Step 1 time min 0 75 Step 1 split state ON Step 1 split ratio 100 25 1 TCD Filament temp 270 20 C filament current 200 10 mA polarity positive Prepare the Test Sa...

Страница 44: ...yethyene Glycol Ethanol 78 5 2 Propanol 82 5 n Butanol 117 7 Sample Volume and Injection Rate The quality of your chromatogram can be greatly affected by the sample volume and injection rate These var...

Страница 45: ...injector switch and depress it completely simultaneously pressing down the syringe plunger Remove the syringe from the injector immediately The RUN light comes on and stays on until the analysis ends...

Страница 46: ...ems 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 b...

Страница 47: ...arrier gas before connecting to the GC This will avoid introducing a large amount of air into the GC Detector fuel gases The typical detector fuel gases are hydrogen and air These should be changed wh...

Страница 48: ...m purge and split vent outlets If more than one injector is present then the outlets of all the injectors must be sealed The following procedure refers to one injector but should be duplicated for eve...

Страница 49: ...m leak detector is available from Varian P N 01 900153 01 This device can detect helium concentration in the air as low as 2 ppm and is very effective at identifying the precise location of a helium l...

Страница 50: ...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 addi...

Страница 51: ...are very common As septum replacement is common to all liquid injectors on the 3800 this procedure is presented first followed by specific maintenance procedures for the individual injectors Septum R...

Страница 52: ...tighten an extra 1 4 turn Turn on the carrier gas supply On occasion to save time you may want to change a septum while the injector is hot Use an injector wrench P N 03 908423 00 to remove and reinst...

Страница 53: ...lit Vent 8 Glass Insert 9 Fused Silica Column 10 Capillary Column Nut 11 Vespel Ferrule 12 Point of Injection Tools Required Tweezers or septum pick P N 72 000084 00 Injector nut wrench P N 03 908423...

Страница 54: ...blade screwdriver to unscrew the septum support nut Item 4 until it is loose 4 Remove the septum support with the tweezers or septum pick Note Typically when the septum support is removed the insert...

Страница 55: ...e and insert seated in it If there is any graphite extruded past bottom of the septum support cut it off with a blade or sharp knife Carefully wipe off any graphite flakes which may adhere to the inse...

Страница 56: ...s with solvent or soak the inserts in hot acid Heat them in a glass annealing oven to 500 C or pass the inserts through the flame of a Bunsen burner Wash in a 1 1 1 mixture of methanol methylene chlor...

Страница 57: ...erts 3 times with 10 mL isooctane hexane or toluene Each rinse should include 2 3 min of sonication 5 Add 10 mL of methanol and sonicate for 2 3 min Decant the methanol and repeat the methanol rinse s...

Страница 58: ...that it has not been damaged Slide the end of the fused silica column into the opening of the injector 8 Gently twist the column nut in the opposite direction used to tighten the nut Place the column...

Страница 59: ...matic start switch assembly may be very hot during instrument operation and should not be touched with unprotected hands Allow sufficient time for the injector nut and surrounding assemblies to cool b...

Страница 60: ...the needle syringe by slowly drawing up and quickly expelling solvent or the next sample to be used Repeat the process several times Note When rinsing with the next sample DO NOT expel sample back in...

Страница 61: ...pply 3 A pressure drop less than or equal to 1 2 psig in 15 minutes is acceptable Locate leaks with an appropriate leak detector Note Any changes in temperature while performing this test may result i...

Страница 62: ...de Natural Gas containing methanethiol 2 x 10 10 50 TSD Dichloromethane 2 x 10 12 2 Visual Leak Checking The least preferred method of leak checking is to place a drop of pure solvent isopropyl alcoho...

Страница 63: ...a new insert Note that there are two different glass inserts one for use with large bore 0 53 mm ID capillary columns and one for use with packed columns These inserts are not interchangeable Large bo...

Страница 64: ...o grasp the glass insert and remove it from the injector Note The glass inserts can be cleaned and reused Replace the Glass Insert Follow these steps to replace the glass insert in the 1061 Injector 1...

Страница 65: ...rom the injector Inserts can be at high temperatures and are likely hot Place hot inserts on a clean glass or metal surface only 2 To clean glass inserts use one of the following procedures the choice...

Страница 66: ...ts to the solution Note Deactivate glass inserts only after they have been thoroughly cleaned using the above procedure 4 Sonicate the inserts in the cylinder for 10 min Rinse the inserts 3 times with...

Страница 67: ...oxic and flammable chemicals Exercise appropriate care when you use and dispose of these substances 1 Remove the detector and internal parts 2 Scrape the deposits from the bore of the collector tube t...

Страница 68: ...unstable baseline noise and reduced sensitivity In this situation or when the detector is to be operated at temperatures above 350 C you must replace the ferrule Be sure to select the proper ferrule...

Страница 69: ...NING EYE HAZARD WARNING FIRE HAZARD Use proper eye and skin protection Methanol and acetone are toxic and flammable chemicals Exercise appropriate precautions when these chemicals are used 1 Remove th...

Страница 70: ...ure 7 Thermionic Specific Detector Assembly 1 Signal Cable 2 Signal Probe 3 Bead Supply Cable 4 Bead Probe 5 Ceramic Bead 6 Collector 7 Ceramic Insulators 8 TSD Tower 9 Flame Tip 10 Aluminum Crunch Wa...

Страница 71: ...g With Carrier Gas Use N2 or Ar CH4 as the carrier gas to thermally clean the ECD Refer to Table 2 on page 39 for flow rates 1 With carrier gas and makeup gas flowing through the ECD cell increase the...

Страница 72: ...rnight Check and readjust the Contact Potential setting if necessary 5 If the performance of the detector is not restored by these cleaning methods refer to the Radiation Safety Manual P N 03 913999 0...

Страница 73: ...01 Septum pick 72 000084 00 Graphite ferrule for insert 5 mm package of 2 03 925342 02 Open 0 5 mm ID insert 03 925331 00 SPME open insert 0 8 mm ID 03 925330 00 Splitless insert 2 mm ID 03 918466 00...

Страница 74: ...39 00 1061 Glass insert for Packed Columns 37 000813 00 Septa package of 25 10 mm 00 997628 02 Detectors Flame Ionization Detector Flame Tip Assembly 0 02 ID 02 001938 00 Flame Tip Assembly 0 01 ID 02...

Страница 75: ...mbustor Quartz 2mm ID 03 925176 00 Combustor Quartz 3 mm ID 03 925177 00 Filter Assembly Sulfur 03 925151 01 Filter Assembly Phosphorus 03 925151 02 Ignitor Assembly 03 925160 00 Combustor support 2 m...

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