Chromatography-Gas - St. Louis Community College
Contents
1. You Need eann PANNE EE p oi un d amp CO DJ BS Chromatography Gas Varian installation Manual Table of Oplimum Capillary GC Carrier Flow Rate and Velocity Optimum Velocities and Flow Rates tor Capillary Columns ESPE EEE rer Co ntents Detector Carrier and Make up Gas Flow Rates and Gas Types P TEREE meS E EAE E E o RECOMMENDED PARTS amp 11 Gas Filters s A6 E Column and Injector Ferrules tor Capilary Columns O s a Calumn Forrulos tor Miere TCLD REED Glass Rum EN p Falun Quick Connect Kit IV METHOD DEVELOPMENT cernere rrr rrr nnne nni nin naa nura arra Recommended Solvents Tor Capillary Columns Recommended Injector and GC Parameters Column Installation Measurements for injectors amp Detectors Units of Measure Man RPetained lor Gc Detectors a i i2. mue Insert 1079 STLCC_CPLS Morrison 6 3 2013 Page 27 Chromatography Gas Varian Manual Pg 12 Micro TCD Ferrules rerrules tor Micro TCD Capillary column connection to the Micro TCD requires a special series of graphite Vespel ferrules see table below Column ID Ferrule Ferrule Part Number CP8SHis o 025mm CP470100 STLCC CPLS Morrison 6 3 2013 Page 28 Chromatography Gas Varian Manual Pg 12 Injector Inserts Capillary injector inserts have a direct effect on analysis results They are chosen depending on the injection mode split splitless on column flash vaporization and sample characteristics m The split and splitless inserts create homogenous mixture of sample and carrier gas transfer a Tepresentative sample into the column and minimizing molecular weight discrimination m The on column temperature programmable inserts for the 1079 provide quantitative sample transfer and retain the liquid sample during cold sample introduction m The flash vaporization insert 1061 provides an expansion volume for large samples and minimizes non volatile sample components from entering the column Insert variations for all injection modes are available for dirty sample matrices labile compounds and large volume injections Inserts should be replaced as soon as a loss in chromatographic is seen Note that all the 1079
3. Buck 310 Chromatography Gas Standard Operating Procedures Preliminary Detect Instrument Picture to Jump to that section of SOP Prepared by Bob Morrison STLCC CPLS Instrumentation Specialist and Mike Davies NIDUS Original Nov 10 Latest Revision Nov 11 add Varian manual Agilent Varian 3800 The GC is in the Bio processing Room along the front windows It is a Varian 3800CP pretty fancy when set up correctly with a flame ionization detector FID It has not been used at the college but it was removed from Covidien s St Louis plant in working condition The column will need to be replaced as well as all of the fittings The college does not have a software package such as Galaxie or TotalChrome at BRDG Park but the machine s on board screen allows the user to view results and adjust settings Hydrogen and or helium sources will be needed as well That s all that know about it but Denise Heinz may be able to help more either personally or through her company lan Rappold 5 2013 Pade 1 STLCC_CPLS Morrison 6 3 2013 9 Chromatography Gas Buck 310 eSmall size full peformance eDimensions 12 5 wide x 13 5 high x 14 5 deep eAmbient to 400 C programmable column oven eMounts up to four detectors Hot link to BUCK 310 Product Brochure pdf Hot link to Quick Start Guide SRI pdf Hot link to Gasless Education guide pdf Hotlink to Free Technical Support at SRI http www srigc com 20
4. I Page 14 Chromatography Gas Varian 3800 Keyboard Controls SINGLE METHOD SELECT yd METHOD SEQUENCE CJ PRIORITY SAMPLE INJECTOR COLUMN OVEN STLCC_CPLS Morrison 6 3 2013 FLOW f PRESSURE Page 15 4 Press SETUP 1 Press ENTER View Setup allows vou to check the current Instrument Configuration Choose Edit Setup if you want to change the Instrument Configuration SETUP MENU Tims and Date Heated Zones EFC oluan Parameters fiscellaneous tetup Parameters ea za Ries m 1 wr enn Cx Der ett eae MES it ue a ee Re Ind es bee Ree A h D e on o EEE ee RR Use CURSOR keys to highlight section TIME AND DATE HEATED ZONES COLUMN PARAMETERS VALVES MISCELLANEOUS Press ENTER to access section and modify Month day year Time hour min sec Device installed in each heated zone Temperature limit Coolant type Column oven zones 1 3 only Outlet pressure atm vacuum Display units psi kPa bar Minimum flow gas saver Make up gas type Length m ID Carrier gas type He H N Valve Numbers 1 7 Valve Type 22 choices m Ready in Contact State FID Flame out Enable m Micro TCD Filament Resistance Chromatagraphy Gas Varian 3800 Setup p
5. CE system The same hardware is supplied as standard equipment with every SRI 8610C 8610D 410 and 310 GC No hardware is installed in your computer so a notebook or netbook PC may be used instead of a full sized desktop PC PeakSimple chromatography acquisition and integration software for http www srigc com PeakSimple htm from SRI Instruments Make detectors PeakSimple Version 3 88 for Windows Vista downloaded and installed On Stratagene Laptop 11 12 10 by Bob Morrison Set Default COM 1 port ID to 1 under Edit Overall toolbar STLCC_CPLS Morrison 6 3 2013 Page 4 Chromatography Gas Buck310 Door must be closed before Oven with operate Open door to Set pots before run On Off main toggle Injection Port Screwdriver used to turn pot set screws for Temp other parameters See manual Toggle Switch Up position to set values Down position current readings displayed TEMP Column of buttons With toggle in up position buttons Temp Over will be used to adjust or calibrate Limit LED oven temp to ambient level STLCC_CPLS Morrison 6 3 2013 Page 5 Chromagraphy GAS Basic Start Guide Buck 310 HARDWARE 1 On the Front panel of the GC set the toggle switch to the UP position 2 Open the lid of the GC to expose the oven and pot set screw holes 3 Retrieve the screwdriver and insert in the hole or pot above the TEMP column While holding the top LOCAL row
6. Screen Initialization or Waking up Pop up EN Window will appear File Edit View Acquisition Help D Ed 5 2 3 4 5 6 131 828384 Waking up Pop up Window will check connectivity to the GC device validate COM port for RS232 connections and test basic parameters GC Edit Channels to Set Oven Temp and other Parameters ile Edit Channels 44 S B 81 82 33 54 Overall Colors Manual integration Valleys only Subtract Add channels Smoothing Re integrate Select EDIT then OVERALL to set or reset COM port ID Select EDIT then CHANNELS to set temperature and other parameters _GC Select Channels to Set Oven Temp other Parameters File Edit View Acquisition Help D dd amp BE tai 2 3 4 5 8 51 22 3 34 Channels Channel 1 CCOD CHANNEL 1 Channel 4 Channel 4 Active M Details Temperature Events Active D Details Temperature Events Display Display Integrate Integration Components Postrun m Integration Components Postrun Channel 2 Channe Channel 5 Channel 5 Active D Detal Temperature Events Active Details Temperature Events Display D Display D NM Integration CoMagnents Postrun NH Integratian Components Postrun Channel 3 Channel 3 Channel Channel 2 Active D Details Temperature Ew Active D Details Temperature Events Display
7. Timed programmed events for splitless injections manual 1079 only or switching valves For GCs with valves consult your custom plumbing diagram for programming Events for a typical split and splitless injection are as follows Time split Valve SPiN 0 00 min On Spl Mode 0 00 Off Splitis Made 1 00 min On Split m Selects Automation Mode m Method Automation Parameters Fronty Sample Activating the GC Method Press ACTIVATE from the Method section 2 Use the INCR or DECR keys to choose desired method Press the ACTIVATE NOW softkey S1NOTE If you edit the active method you must re activate it before running an analysis Chromatography Gas Manual pg 5 Activating Method Page 18 Chromatography Gas Varian Manual Pg 6 Single Injection Making a Single Injection Use the following procedure if performing a single injection If you are using the Star Chromatography Workstation refer to the instrument s Operator s Manual Confirm that the GC is in the Ready state The amber Ready light should be illuminated If you are making an injection with a 5vringe Inject the sample into the The GC method will pL asomatclly Gas or Liquid Sampling Valve using n air actuator STLCC_CPLS Morrison 6 3 2013 The gas or liquid sampling is in the fill position and the valve will rotate to the inject lop 15 loaded with sample positio
8. applications a Beige silicone r bber with 00 997623 0 face Standard Ia BMC 00 00 997628 03 m Standard septa for Varian GCs 00 997630 02 00 997630 03 size your septa here Q 10 mm 11 5 mm 1041 On column 1079 Injectos 1061 Flash Vaporization Page 32 Chromatography Gas Varian Manual Pg 15 Connect Kit This kit simplifies the installation of capillary columns into Varian injectors and detectors The kit contains split capillary column nuts reusable jacketed graphite ferrules for 250 320 550 ID columns and a column depth scale No felt tip pen typewriter correction fluid or tape is needed to mark column depth for any injector or detector The split nar design allows you to remove the nut trom the column when the columm is stored without having to remove the ferrule The split capillary column nuts are Knurled so that all tightening can be done by hand No tools are required Column Depth Scale YARAR x Included in This Kit P N 03 825751 90 Column Depth Scale Knurled Split Nui Graphite Jackered Peruule 2 each 0 4 ID Graphite Jacketed Ferale 0 5 mm ID Graphite Jacketed Ferrule 0 8 mm ID Part Number Graphite Jacketed Ferrule 10 each 13 975 484 04 0 2 mm ID Graphite Jacketed Ferrule 10 each 04 97 5484 05 1 0 5 mm 102 STLCC_CPLS Morrison 6 3 2013 Page 33 Chromatography Gas Va
9. button rotate the pot to the 0000 position This will indicate tha no increment is set above the current oven ambient room temperature 4 Close the GC lid Press the STATUS row TEMP button and observe that the oven is at ambient temperature The TOTAL row should show 0000 or close to it 5 Turn off the GC device and proceed to the SOFTWARE setup which will control the device parameters for run and analysis SOFTWARE 1 Download PeaksimpleSoftware to PC attach RS232 line from GC device to COM port 2 Turn GC toggle Initiate Peaksimple Software and monitor initialization and communication process between device and software If initialization fails Go to PeakSimple Edit option in top toolbar select Overall then enter COM port ID where the RS232 connect was made You may also need to change the type of connection USB or Serial on this same panel Repeat startup process 3 Select EDIT from the top toolbar then Channels Select the Active Display and Integrate options next to Channel 1 An X will show in the appropriate box 4 From the EDIT CHANNELS menu Select DETAILS then MAIN for channel 1 In the Control by section select Temperature 5 From the EDIT CHANNELS menu Select TEMPERATURE and enter the start delay and any ramp temperature conditions desired You may optionally LOAD a saved TEMPERATURE profile or SAVE new or modified TEMPERATURE profiles for this or STLCEUT EG MD S5 3 2012 Page 6 GC Startup
10. 05catalog cat109 htm The Buck 310 portable gas chromatograph is Multi detector system and can accommodate 2 4 detectors depending on your combination There are 9 specific detectors available for the Buck 310 GC Price is for base unit without detector s Designed to be durable and portable the compact 310 series is ideal for operation in the field and A S T M methods can be easily performed on site even in adverse field environments A GC with the versatility to meet your lab s specific needs The unique architecture of the Buck GC systems allow various detector and injector combinations so each GC can be configured to meet your specific lab requirements Automated Analyses let the GC do the work so you don t have to The Buck 310 offers total control of application parameters using PeakSimple software PeakSimple allows unlimited temperature programming electronic pressure control carrier gas pressure gas valve position gas solenoid actuation autosampler control and other options Just program your application parameters into the computer and let the 310 do the rest Over 12 different detector options to choose from for optimal measurement results STLCC CPLS Morrison 6 3 2013 Page 2 Chromatography Gas Buck310 CCD Catalytic Combustion Detector CCD Detector and protective is removed prior to installation The Catalytic Combustion Detectorresponds to all hydrocarbons with the selectivity ofan FI
11. D andthe sensitivity ofa TCD The entire detector s diameter is merely one centimeter Its sensor element consists ofa tiny coil ers 4 ofplatinum wire embedded ina catalytic ceramicbead Each CCD detector CCD on Column Oven agas of sensor elements The sensorsare housed in high grade flame proof nylon and protectively capped witha fine steel mesh In SRI GCs CCD detector is mounted on the wall of the Column Ovenina brass housing as showninthetop left picture Thearalytical column residing inthe Column Oven is connected to the detector through the oven wall the example shown at bottom left isan SRI Gas less E ducational GC featuringa CCD detedoranda 1m 3 Hayesep D packed column The Ei eee CCD detectoris especially suited for gas Lage m less operation because it can operate on RH ambient air requinng no high pressure cylinder gases suchashydrogen or helium Inthe GC system pictured at left a built in atr compressor supplies the carrier gas forthe CCD The CCD detector can also be used as a hydrocarbon monitorin non chromatographic appli cati ons where the CCD senses the total hydrocarbon content ofa flowing air stream orasa hydrogen hydrocarbon leak detector Chromatography Gas Buck310 PeakSimple Software PeakSimple chromatography data systems consist of hardware and software The hardware is available as a stand alone data system for connection to almost any model GC HPLC or
12. Display D Integrate Integratian Components Postrun E3591 Integratian Components Postrun J Select to Activate the ACTIVE DISPLAY and INTEGRATE options for Channel 1 and any others in use Admin ternet Links 2010 07 GC On Temp Window Load old profile or Enter new Data File Edit View Acquisition Help osha E 5 ta 1 2 3 4 5 6 81232 33 34 Channel 1 temperature control C peak388 32bit GP TEM Select EDIT then CHANNELS then NEMUS TEMPERATURE se LOAD retrieve TEMP profile buds CHANGE modify parameters SAVE store modified parameters for M MI a future run Display Integrate Active Events Display D Integrate Adn AT admin Internet Links 2010 07 GC Edit Channels to enter Description and Details File Edit View Acquisition Help gt 12346567 1222324 Select EDIT then CHANNELS then DETAILS To set temperature and other parameters Channel 1 details Description NN End time E 0 000 min Default display limits Remote start Control by Active W Timebase Events fe Wesks al 120 000 mv 71 Temperature C Postrun Integrate M L Min 32000 s 725915 3 Channel 2 Chann Ca Gradient Active D Everts A Datalogger made Display D Subtract baseline in channel f On Integrate Postrun Overlay data in c
13. ON SPME TEMP RAMP SPLITLESS 1079 SPLIT Chromatography Gas Varian Manual Pg 13 Insert Partnos Page 30 Chromatography Gas Varian Manual Pg 14 Septa septa allow the syringe needle to enter the GC injector yet maintain a leak free seal in the GC system hey are available in several different types of materials and sizes depending on injector mode and analysis needs The septum chosen for a GC analysis should exhibit low bleed resist leaks and be easy to pierce when performing injections septa should be changed every 50 to 100 injections or when you note a change in peak retention time or ghost peaks Tt 15 preferable to change septa routinely rather than after leaks develop thus minimizing instrument downtime and sample loss Change the septum at the end of the workday then keep the column oven temperature hot enough to prevent bleed from accumulating overnight Using needle guide a syringe free of burrs or an autosampler will prolong the septum life because single hole will be repeatedly pierced allowing easier re sealing Page 31 STLCC CPLS Morrison 6 3 2013 Varian Manual 14 Septa table STLCC_CPL a Red rubber IC Low bleed Long injection lite i 10 mm D 90688 0 10 mm LORD 1 998683 07 Easy sample injection 05 920357 0 03 970357 02 Green silicone rubber m Tani m Low bleed Recommended for all 1079 GC MS and ECD
14. P 3800 appears above the bold line on the display The information beneath the bold line is the method parameters of the EDIT METHOD Note that the EDIT METHOD and the ACTIVE METHOD may be different TONES esr WM vus UA ut RUN T due ved dore E UE NEN Mo TRE m _ OS e UMS ee un nekh d 1 1 0 00 e at set CFCS 50 50 Stabilization Time min 2 00 Column Oven off COLUMN Page 1 af 2 Page 21 STLCC CPLS Morrison 6 3 2013 Chromatagraphy Gas Varian Manual Pg 8 Hardware Column Column Installation Follow these steps to install the capillary column and set gas flow rates SILCC CPLS M y vo 4 V Cool all heated zones and replace depleted oxygen and moisture traps Replace critical injector inserts and septa Cut 2 cm from each column end Thread the nut and ferrule over the column oa both ends The ferrule should be installed with the taper end into the nut Cut 2 cm from each column end to remove ferrule fragments Mount the capillary column in the oven tlie column 7 3 cm the 1079 injector measured from the back of the nut The 1041 ard 1061 do noi require measuring They are installed all the way up into the injector 8 Set the approximate column head pressure Set the split ratio and septum purge flows 1079 only 10 11 12 Set injector and detector temperatures Do not e
15. ct the chromatography system from potential contamination The following filters are recommended for systems Filter m Descriplon 0 mm mm Part Number Moisture Gas Filter Installed between pas tank and GC inlet 17971 Molecular speve Removes water vapor Filter should be changed when indicator shows filter is spent Installed between gas tank and GC inlet CP17972 Activated charcoal Removes organic contaminants Filter should be changed when indicator shows filter is Installed between carrier gas filter and GC inlet CP17970 Removes oxygen and water vapor Charcoal Gas Filter Oxygen Gas Filter Recommemtied with capillary columns Required for ECD Filter should be changed when indicator shows Hilter 15 Spent STLCC CPLS Morrison 6 3 2013 Page 26 Chromatography Gas Varian Manual Pg 11 Ferrules Column and Injector Ferrules for Capillary Columns A Ferrule n Graphite Polyimide Graphite Ferrule Size microns 10 10 pk 10 pk ms No hole 28 694503 0 28 604590 0 1 16 fitting 0 4 mm ID 80 2 540 25 hU045865 0 2 504581 01 24 694 520 0 1 16 Fitting 0 5 mm ITF 320 OS 908 561 01 28 694561 01 28 659458 1 01 1 16 fitting 0 5 mm ID 530 28 894852 01 28 694042 01 28 594582 01 1716 fitting 15 mmm ferrule for 03 9245342
16. dence Time Imm EN Hot Needle 0 Time in Isothermal Temp Temp program or temp program Initial temp progr m Initial 20 C from the solvent boiling NC from point With the solvent larger sample hailing volumes solute point focusing 16 possible with initial 10 20 above solvent boiling pont Chromatography Gas Varian Manual Pg 17 Recommended Injector and CG Parameters Page 35 Cn 8 i E E 3 e e zo T5cm TO 3 9 1177 el 2 7 r 21 2 Units of Measure Parts per I ousand Paris per piion per Non Retained Compounds for GC Detectors etector Compounds D Methane propane butane z slzlelalaly Air methane butane Methylene chloride headspace vapors Acetonitrile headspace vapors butane Sulfur hexafluoride methane propane butane Carbon dioxide Air methane butane Micro TCD 4 AK VA a gt 2 Chromatography Gas Varian Manual Pg 17 Measurements Page 36 Chromatography Gas FID Defined FID stands for Flame lonization Detector What that means is that as the effluent carrier gas and any organic compounds comes out of the column they are ignited in a flame made of hydrogen and air The compounds produce ions as they burn These ions conduct electricity Changes in current within the flame are measured a
17. g 3 Page 16 Press ENTER Typical parameters for a GC method m Column Injector and Detector temperatures m Flow or Pressure program if EFC is installed Detector range and autozero Valve program if performing a manual pneumatics splitless injection or rotating a sampling or switching valve m 3200 utoSampler Follow the method sections below to build your GC method You can advance to any section by pressing the appropriate section key The Following Method Section COLUMN OVEN INJECTOR Column temperature isothermal or programmable Stabilization time Coolant on off Enable coolant on off temperature Coolant timeout Injector temperature isothermal and programmable Coolant onoff Enable coolant temperature Coolant timeout Split state EFC only split ratio EFC only m Plow Pressure 1079 Valving Chromatography Gas Varian Manual pg 4 Building a Method Page 17 The Following Method Section DETECTOR SAMPLE DELIVERY VALVE TABLE Automation Will allow you to modify these method parameters Detector temperature Range and autozero time programmable Detector time constant PCD temperature and polarity time programmable PFPD PMT voltage gate width delay trigger level TSD bead current and power time programmable ECD contact potential and cell current Detector flow EFC only S5200 Sampling Parameters
18. hannel 7000 Relative retention shifts based at 0 000 min Gain f 000 Display D Unretained solute time O 000 mir DE Integrate ecimal places Channel 3 Chann Active Events Pastrun Reverse polarity Absorbance mode 1 for autoranging Multiply norm area results by f Admin Internet Links 2010 07 GC Set Channels then Components E File Edit View Acquisition Help S E a 2 345 E 8152 23 24 ZA Select EDIT then CHANNELS then COMPONENTS to define Peaks Channel 1 components ES blz CFT Channels Peak Start Calibration SOLVENT 0 350 Channel 1 COD C Benzene 1 480 BENZENE CAL Toluene 2500 TOLUENE CAL DE 8 Ehlarbergere 3 430 CHLOROE CAL Display Ethwlbenzene 3 680 ETHYLE CAL Integrate m p Dichlorabe 5 M PDICHL CAL a Dichlorabenz 6 070 O0 DICHL CAL Events Active 0 Events Display D NE Il Postrur Active Do Events Display D Integrate T Pastrun Add Change Remove Calibrate Load Save Clear Print UFER BNC connector for 10 Chromatography Gas Varian 3800 base 2 Ethernet cable The Varian 3800 GC is Varian s top of line Gas Chromatograph with a flexible platform for single dual or three channel configuration for maximum productivity Large LCD screen and straig
19. htforward user interface for easy viewing and editing of GC parameters Spacious column oven accommodates three or more columns Fast heat up 100 C min and rapid cool down column oven 400 C to 50 C in 4 5 min allow for faster cycle times and increased productivity Concurrent installation and operation of up to three injectors and three detectors permanently on the GC Wide range of injectors and detectors to choose from for the most complicated application Choose from manual pneumatic control or electronic flow control for all injectors and detectors Wide range of autosamplers to choose from for complete sample introduction and preparation automation It is fully functional as a standalone GC or controlled through the Varian Star Workstation or the Humidity 5 to 95 relative Galaxie Chromatography Data System GC System Type Modular Depth 56 cm Height 53 cm Width 66 cm Power Requirements 101V 120V 230V Hot Link to Varian Brochure 18 pgs pdf Weight 43 kg Hot Link to Varian Basic Instructions pdf Hot Link to Varian Laurier Sci User Manual STLCC CPLS Morrison 6 3 2013 Hot Link to Varian Maintenance Parts Brochure pdfe 13 Hot Link to Varian 3800 User Manual format pages included in this document COV hs MANNI E EE LL ELE LLL LLL instrument Building Methad Automation Activating the ac Method Making a Single Injection
20. inserts are deactivated Lu ud Description Part Number High Performance Insert 1 900 109 06 13010 320 ID columns Quantitative liquid sample transfer E Used for cold on column injections m 530 um ID Columns Quantitative liquid sample transfer m Used for cold on column injections bs aco o 29 STE LE VQIVIMZIELTIL INZNZL T MJ JI aW IJ Description Fria Insert Linear split adequate sample mixing 03 918464 01 03 9 8464 00 03 918956 00 03 91 8466 00 instantaneous sample vaporization 3 4 mm ID Unpacked Insert Can packed with quartz wool glass beads etc 3 4 mm ID Packed Insert 3 4 mm ID Open Insert u The narrow bore minimizes dead volume ensuring efficient transfer of sample to the column 1079 is shipped with this insert installed 2mm ID Unpacked Insert 03 918464 00 3 4 mm ID lg ee Open Insert 03 925331 00 e Trace analysis The low surface arca makes it ideal for thermolabile and 4 polar components 1 5 mm IN Packed Insert 03 925350 00 e Deactivated glass wool packing Can bc used in all three modes For non polar compounds above 1 ng level 2 mm ID SPME Insert For SPME injections s 15 mm ID 03 925330 00 03 918339 00 MEME e 530 um columns only Packed column insert 37 000813 00 LASH 1079 VAPORIZATI
21. n and the GC method Press START will start Page 19 SILCC Chromatography Gas Varian Manual Pg 7 Status The Instrument STATUS key allows the user to view the current status of the various components of the CP 3800 instrument Note that the current status of individual components can also be viewed by pressing the relevant key in the GC CONTROL keyboard section The primary status information provided using the STATUS key is the actual component vemperature carrier gas flow and pressure f EPC is installed and detector analog output signal The following is an example of a status screen for a CP 3800 equipped with 1079 injector and PIL Note that the status screen reflects the current state of the If the instrument is running method the status fields will update as the values change during the ron at a rate of once per second fa component 15 not ready or faulted this will be indicated on the STATUS screen Note that the status screens are in location ie Front Middle and 1 Rear lethed 3 gathed 1 INSTRUMENT STATUS FRONT 1 3 Component Actual 4079 ven pag Column Flow ml min Colunn Pressure ipsi Column oven Temp 9C FID ven FID utput tav Chromatography Gas Varian Manual Pg 7 Control When one of the six GC Control keys is pressed the user is presented with a split display The status information reflecting the current status of the C
22. nd sent to the computer to be seen as peaks on the chromatogram FID is a good general detector for organic compounds and is able to detect at the nanogram level Flame lonizaton Detector Collector electrode Flame ignition coll 300 Polarizing voltage Hydrogen Column STLCC_CPLS Morrison 6 3 2013 Page 37
23. rian Manual Pg 16 Solvents The choice of solvents for a chromatographic analysis depends on the component solubility detector and the polarity of the analytical column Solvents should ideally match the polarity of the column especially when injecting large volumes and performing on column or splitless injections Non par columns perform best with non polar solvents Polar columns perform best with pelar solvents however they also perform well with non polar solvents Below are recommended solvents for non polar intermediate and polar phase columns Nan Palar m 100 Methyl m Phenyl 9555 Methyl Iniermediate m DB Pheuyl 0 Polar m Polyethylene Glycol STLCC_CPLS Morrison 6 3 2013 n Hexane Cyclohexane vooctane Benzene Toluene Ethyl Ether Methyl tert butyl ether Methylene Chloride Carbon Tetrachloride Carbon Disulfide Ethyl Acetate Accione Methyl iso hbutyl ketone Acetonitribe Methanol Exhanal n Propanol n Burannol Page 34 On Calumm 1041 1079 109 1079 1079 Flash Vaporizing 1061 Using Using Split Insert Splitless On Column High Insert Insert Performance _ _ Insert For For For Far Large Bore Capillary All Large Bore All Capillary Columns 530 jm Capillary Capillary Columns 180 Packed Columns Columns Columns 320 pum 10 530 um ID 1 Injection 0 Ji Needle Resi
24. us substance compatible with the detector Page 18 Calculate the column velocity then flow rate and split ratio if applicable usme the equations below Cole Velocitv cap iec Column lengh erm Unretained peak time 3ec HETF Column Flow Rate folio 1 BOX Katie Split veni flow mL min Coburn flowrate mL Average Linear Velocity emisar Chromatagraphy Gas Varian 3800 Manual Pg 9 Optimum Flow Rates umn ID microns STLCC_CPLS Morrison 6 3 2013 Page 24 Chromatography Gas Varian Manual Pg 10 Optimum Flow Rates Use the following guide for determining the appropriate gases for your GC system and setting am and make up flow rates Air 1 1 Same gas FID 20 A lume tip ECD IT Ns Ar CH No ArCH He Hayt PFPD Element specific fetes i PFFD Operator s Manual ee Inlet Cylinder 80 psi AD qii 60 psi 60 psi Pressure 00 EPu 18 kPa 420 kPa 420 kPa Purity 5r 99 999 99 999 Zero Zeno Lk Grade rade Total Hof flow any used For carrier or makeup eas sticc may be used only when capillary column flow rates are 10 mL min Page 25 Chromatography Gas Varian Manual Pg 11 Filters Carrier and detector filters should always be installed to further clean high purity gases reduce detector noise and prote
25. xceed the column s Tmar 14 15 Connect the column to the detector at the appropriate distance see Page 18 Check for leaks using a leak detector Do not use soaps or liquid based leak detectors Set make up and detector gas flow rates see Page 10 Condition the column at its recommended conditioning temperature for two hours Run test mixtures to confirm proper installation and column performance 16 Calibrate instrument and inject samples Page 22 Chromatography Gas Varian Manual 9 Flow Rate After conditioning your column the carrier gas flow rate should be set for optimum separation of sample components Since the flow rate is dependent on column temperature pressure regulated system it ts important to set the carrier gas at the same columm temperature for given analysis For convenience the carrier gas is often set at the initial temperature of the analysis For a slightly faster analysis and improved separation set the optimum flow rate at the maximum temperature of the analysis For critical or hard to separate peak pairs in the chromatogram set the optimum linear velocity at the oven temperature where they elute If you have Electronic Flow Control installed in your GC setting the column flows is as simple as entering the column dimensions and carrier gas type in SETUP and building the appropriate flow or pressure program in the Method If you don t have EFC installed inject 5 pL of a non retained gaseo
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