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430-GC User Manual

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1. Slide a 1 8 Swagelok nut back ferrule and front ferrule over one end of the copper tubing and attach to the outlet fitting on the cylinder regulator Push the copper tubing into the outlet fitting as far as it will go then pull back very slightly and tighten 3 4 turn past finger tight with a 7 16 wrench Front Ferrule Swagelok Nut Xs Back Ferrule Figure 8 Proper Ferrule Orientation Push the other end of the copper tubing into the filter base inlet fitting as far as it will go then pull back very slightly and tighten 3 4 turn past finger tight with a 7 16 wrench Connect another length of copper tubing to the outlet of the filter base using a 1 8 Swagelok nut and back and front ferrules as above Push the copper tubing into the bulkhead fitting on the back of the 430 GC as far as it will go then pull back very slightly and tighten 3 4 turn past finger tight with a 7 16 wrench Make sure the gas supply control valve which controls gas pressure to the GC is completely closed Open this valve slowly and monitor the pressure gauges on the dual stage regulator The first pressure gauge should now read the pressure of the cylinder User Manual 430 GC and 431 GC Page 19 Installation 8 Cautiously turn the regulator valve to supply gas to the GC Watch the pressure gauge closely and adjust the pressure to 80 psi 9 Install the carrier gas filter cartridge into the filter base following inst
2. Store cylinders in a well ventilated area away from heat direct sunshine freezing temperatures and ignition sources Mark cylinders clearly so there is no doubt as to their contents Use only approved regulators and connections Use only connector tubing that is chromatographically clean Varian Part Number 03 918326 00 and has a pressure rating significantly greater than the highest outlet pressure from the regulator User Manual 430 GC and 431 GC Page VII Safety Information GC SAFETY PRACTICES Exhaust System No special exhaust ducting is necessary for GC detectors installed in a well ventilated room except when the detectors are used to test hazardous chemicals If you do install ducting a Use only fireproof ducting a Install a blower at the duct outlet Secure air duct intakes such that their vibration or air movement does not effect detector operation Check periodically for proper operation of the duct Ensure proper ventilation in lab area Radioactive Source Detectors Read carefully and comply with all NOTES CAUTIONS and WARNINGS in the Ni ECD manual Perform the tests for removable radioactive contamination described in the Ni ECD manual Comply with leak test schedules and procedures Burn Hazard Heated or cryogenically cooled zones of the GC can remain hot or cold for a considerable time after instrument power is turned off To prevent painful burns ensure that all heated or coo
3. Company Network 2 Ethernet ler switch Uplink connection to Company Network Ethernet Patch Cables p n 03 926129 01 or 02 Figure 11 Company Network Page 22 User Manual 430 GC and 431 GC Varian Inc Installation Network Terminology If you are unfamiliar with network terminology the following brief glossary of terms may be useful BNC Connector This is a bayonet style connector used for a two conductor style hardware connection BNC connectors are used with the CP 3800 GC If you will be mixing 430 GCs and CP 3800 GCs within your lab you will want to make certain that you have hubs that support the 10Base2 BNC style connectors BOOTP Server This is software that allows you to assign IP Addresses and designate host names to Ethernet devices such as the 430 GC 450 GC CP 3800 GC 3900 GC and Star 800 box that require static IP Address assignments The Star Workstation has a BOOTP server built into it that may be accessed by clicking on Instrument menu and selecting Setup Ethernet Communications Crossover Cable A cable that is only used to connect two Ethernet devices together Domain This is one of several settings that reside within the TCP IP configuration that identifies paths that are used to establish connections with Ethernet devices The Domain is an IP Address Ethernet Address This is a unique identifier that every Ethernet communication device has assigned to it Typically the Ethern
4. KEY The Automation Schedule is not a method section This section is only available if a CP 8400 or CP 8410 is connected to the 430 GC The parameters under this icon modify the behavior of the key and it is for this reason it is grouped O00 The 000 key is where you schedule what vials your CP 8400 or CP 8410 will inject and with which method This is different from the Automation Method Section where the actual AutoSampler parameters are entered This icon is grouped with the 000 STOP and START keys since once the schedule of samples is entered Q cause the Automation to begin and O stop automation You will know when the Automation Schedule is set to Single Method and is thus active by the LED located immediately above the Automation Schedule icon If that LED is illuminated then pressing Q begin Automation If the LED is not illuminated then the 430 GC is in manual mode Automation Outline Automation Mode Manual Single Method Automation Method Automation Starting Vial Automation End Vial Number of Injections Vial Page 42 User Manual 430 GC and 431 GC Varian Inc Maintenance Parts and Supplies MAINTENANCE PARTS AND SUPPLIES It is important for the GC user to learn general maintenance techniques and perform them on a regular basis Some common GC maintenance procedures are changing septa and injector inserts checking for leaks conditioning columns and changing filters Note that a qualifie
5. and hold it just above the FID tower being careful not to get too close to the hot surfaces If you observe condensation then the flame is still lit you may wish to change your fuel gas mixture or some other operating characteristic that would allow a slightly higher background signal Once a flame out is detected the system will attempt to ignite the flame 3 times before reporting the flame out condition The Error is cleared by either igniting the flame using the Ignite FID Flame Command or by turning the Detector electronics off FLOW gt MAX DEFC FLOW Fatal Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative GAS SAVER TIMEOUT Soft The GC has been idle for a period of time equal to or greater than the set Gas Saver timeout period Activate a method to clear the Error INJ RESPNSE TOO FAST Fatal Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative INJ RESPNSE TOO SLOW Fatal Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative INJ TEMP PROBE OPEN Fatal Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative INJ TEMP PROBE SHORT Fatal Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative INJ TEMP TOO LOW Fatal Turn off instrument and turn it back on If the Error recurs call your Varian
6. e When installed components that use a heated zone are turned on in the active method and default to a set temperature of 140 C for the injector and 200 C for the detector CALIBRATING THE CP 8400 8410 AUTOSAMPLER Before working with the AutoSampler it is mandatory that the calibration procedure must be performed written in the CP 8400 8410 Operator s Manual 03 914852 00 CAUTION The goal of the calibration procedure is to align the AutoSampler needle with the first vial and with the injector Page 26 User Manual 430 GC and 431 GC Varian Inc Installation INSTALLATION CONCLUSION The rest of this manual provides more detailed descriptions of how to set and use the various aspects of your GC Please refer to the manual if some aspect of the instrument is not immediately clear or if you would like to understand more how this GC operates Varian Inc User Manual 430 GC and 431 GC Page 27 Use Er to scroll up through the various display pages and to cancel an edit before pressing DN gt will start automation if present start a run if automation is NOT present or allow to Autolnject a sample mO key ends a run in progress Use the 00 automation Pressing view the actual conditions of the GC Press oC to change instrument basic configurations settings to program local Led s show the GC run state AWN Ready Run Stabilize Not Ready Error Use to perform actions
7. max 350 C CR212200 Graphite Vespel 40 60 max 400 C CR213200 Graphite 100 max 450 C CR211200 Aluminum Seal Washer 1500334701 a 16 Detector Base 392547501 7 para eel Figure 20 FID Exploded View Column Nut 394955100 Flow Tube 200187600 Large Stopper 394958600 Replacement parts on page 101 or click here Page 80 User Manual 430 GC and 431 GC Varian Inc Detectors Disassemble the FID 1 Setthe FID to 50 C and wait for it to cool before disassembly Turn the detector electronics and detector oven OFF in the active method Remove the GC top covers on page 46 2 Turn off the main GC gas supplies to the detector at the pneumatics panel These are the make up hydrogen and air supplies 3 Disconnect the signal and ignitor cables from their probes on the detector tower 4 Remove the signal and ignitor probes from the detector tower DO NOT rotate the probes as you disconnect them from the electrical contacts in the tower Place the probes on a clean surface such as a lint free laboratory tissue 5 Remove the two 8 32 x 2 3 4 inch tower mounting screws from the top of detector tower The screws should be tightened to no more than 20 inch pounds of torque 6 Remove the tower assembly from the detector oven lifting straight up until clear of the flame tip Remove the collector tube and insulator from the detector tower Avoid contamination of the ceramic insulator and probes If the detector is not
8. observe this problem call your Varian Service Representative A S TOWER ERROR Fatal The A S tower has one or more internal Errors and has failed to properly come up Turn off the power and then turn it back on If the problem recurs call your Varian Service Representative A S TRAY MISSING Soft The CP 8410 sample tray has been removed from the base Replace the tray the CP 8410 should automatically sense that the tray has been replaced If the message persists call your Varian Service Representative A S TWR SENSOR ERROR Fatal The tower sensor does not conform to its expected operation Turn the GC off and then on again If the problem persists call your Varian Service Representative A S VIAL MISSING Soft The AutoSampler has failed to detect a vial within an expected range of vials This message is an advisory message If you have a vial in the position and it has been missed check that a septum is installed Lack of a septum and dark colors may cause the tower sensor to fail to identify the vial A S VIAL SENSOR ERR Fatal The AutoSampler vial sensor has failed to conform to its expected operation Turn off the GC and then on again If the problem persists call your Varian Service Representative A S VIAL UNREACHABLE Soft This message informs you that the CP 8410 tray is oriented such that the requested sample vial does not fall under the arc of the tower Re orient the tray or change the requested vial from which you intend to
9. snap cap and Ultra GC MS septa 392612007 100 pk 10 mL 22 mm x 45 mm sample vials for CP 8410 w 392611973 50 pk snap cap and septa 392611972 100 pk Ultra GC MS Starter Kit 10 ea 2 mL vials with caps Starter Kit and Ultra septa 6 ea 5 mL vials and 5 ea 10 mL 392611978 1 ea vials with 11 wide hole snap caps with Ultra septa Varian Inc User Manual 430 GC and 431 GC Page 101 Replacement Parts CP 8400 8410 Syringes 1 Hamilton 5 uL 701 syringe 26 gauge HM87900 1ea SU Hamilton 10 uL 701N syringe 26 gauge eae Hin SGE 10 uL syringe conical tip needle 26 gauge SG002980 1ea 100 uL CP 8400 8410 Replacement Trays CP 8400 AutoSampler 100 vial Sample Tray CP738642 1ea Quick Connect Ferrules and Column Scales Graphite Quick Connect ferrules w brass jackets not for use connecting to MS detector 0 4 mm for 0 25 mm ID columns 392538401 2 pk 0 5 mm for 0 32 mm ID columns 392538402 2 pk 0 8 mm for 0 53 mm ID columns 392538403 2 pk 1041 Injector Insert for 0 53 mm ID columns 392543101 1 ea 9 5 mm Advanced Green 3 Centerguide septa CR246124 50 pk Page 102 User Manual 430 GC and 431 GC Varian Inc Replacement Parts 1177 Injector Inserts Siltek 4 mm ID fritted injector insert for split and ne RT210462145 5 pk splitless injections Siltek 4 mm ID unpacked single gooseneck glass ae RT207992145 5 pk injector inserts Siltek 4 mm ID unpacked ope
10. 20 00 Default 20 Hold Time 0 00 to 999 99 Hold Time 0 00 to 999 99 Hold Time 0 00 to 999 99 Hold Time 0 00 to 999 99 Hold Time 0 00 to 999 99 You may add lines to the Pressure and Total Flow program by pressing the F key You may delete a line by scrolling so that the desired line is displayed and then pressing the key Page 38 User Manual 430 GC and 431 GC Varian Inc THE m OVEN KEY This key will give access to the Oven settings Oven Outline Stabilize Time Initial Temp Ramp End Temp Ramp End Temp Ramp End Temp Ramp End Temp Ramp End Temp Ramp End Temp Ramp End Temp Column Coolant Enable Disable Coolant Threshold Temperature 0 0 to 10 0 minutes 30 to 450 C 30 to 450 C 30 to 450 C 30 to 450 C 30 to 450 C 30 to 450 C 30 to 450 C 30 to 450 C Enabled or Disabled 50 to 250 C Display and Keyboard 0 to 999 99 min 0 to 999 99 min 0 to 999 99 min 0 to 999 99 min 0 to 999 99 min 0 to 999 99 min 0 to 999 99 min 0 to 999 99 min OO M O O 4 _ A _4 _4a L A You may add lines to the Column Oven program by pressing the key You may delete a line by scrolling so that the desired line is displayed and then pressing the E key Varian Inc User Manual 430 GC and 431 GC Page 39 Keyboard and Display THE Li DETECTOR KEY This key will give access to the Detector Flow settings FID Detector Oven On Off Temperature 50 to 45
11. Gea seas as ate eta 64 TAT 7 Injector Assembly ariris iine nE AEAEE es EEE NEEE EE iA 65 M CE E EE E EE 66 TORR UIC aera E E E E E EAS 66 Remove Ie COSS TST e raa E E E TE ATA 66 TOC IS TSC a A EN O E IA I IE T E OOE E EA E E EEN 67 TCC OV OG CC IO AE A ENEON IONE S ENO EO E A IE I E E E E E E E 68 THE 1041 ON COLUMN INJECTOR sssssssessseeeeeessesssssssssssrerreeeresrssssssseteterereesessssssssssetetetereeeessssssssssestrttets 71 ALODE SOT W O eE T E E E E EE T EREA AIEE N 72 Meor ASS nY ONA SOTT rE E E EE T OE A EE 73 CDT SIO Ossie caida mcs ernie EAE ENE E RI OE TR EOE ee ed ee ee 74 Column CORT CRON RS COE co cistsasaanascecenice ssecusesasentiiacedcatea E S 74 1041 Electronic Flow Control cccccccccccccccccssneeseseeeceeee ee eeeeeeeeee ena eeeeeeeeeeeeaaeeeeeeeeeeeaaaasseseeeeeeaaaaeseeseeeeaas 75 seline the Carrier Gas FIOW serscacsnssaccocnesacessusiudenseadsdanentvnsleraadneiedeawes didaaawsdeavasandininanigeteded dua E ERSE AEREE 76 Flow Rates Tor Operaio kesesini Eara aaea arti 77 OS MA INU ase a cece pasanat ana ns aessencnne E A I7 Varian Inc User Manual 430 GC and 431 GC Page 3 Table of Contents TES CIE NOFA IN COOP Cir E tiie atzieeiapsdedabadenbea attendee EOE T II DETECTOR CONNECTIONS AND HARDWARE diocra eina a A A aa 78 THE FRID DETECTOR ukuna a a a E 79 Tasta at onI ASS OLY orius E EE A A A E E SO Exploded Vie W esneda sue dobarenscacncun soa E eden Pa steed E aga TSLCRD Giana hdmi ETE 80 Disassemble TS TLD se acai
12. Method tables If you wish to add a program line step to the External Events relay program Injector Split Ratio table Column Oven program or the Detector Range Attenuation time program you press i If you have currently displayed the last line of a table on the display noted by the expression 3 3 in the example below then pressing Er will append a line to the end of the table INJ 3 3 A TIME OF EVENT 9919 99 In the middle of a table pressing F will insert a line into the table immediately after the step currently shown on the display Note that there are either two three or four display pages for each line Each page shows a part of the table line being operated on The figure below demonstrates how the table lines are displayed Time of Event 1 00 Split State On Split Ratio 100 Step 2 Time of Event 25 00 Split State On Split Ratio 10 Step 3 Time of Event 30 00 Split State Off Split Ratio INJ 37 6 STEP 1 TIME OF EVENT 1 00 INJ 3 6 STEP 1 SPETTESIATET ON INJ 3 6 STEP l SPLIT RATIO 100 Figure 12 Table Operations with Local User Interface Each table line is represented by multiple display pages in this case three display pages The key will remove the currently displayed step from the table Please note that it does not matter which of the fields for a given step are displayed in the table All table entries belonging to Step 1 for instance are part of the same table e
13. Service Representative INJ THERMAL RUNAWAY Fatal Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative INTERNAL TEMP EXCDED Fatal Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative IOP COMM FAILURE Fatal Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative MAIN BOARD FAILURE Fatal Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative RUN ENDED BEFORE INJ The AutoSampler failed to complete the injection sequence Restart Automation to clear the Error If the problem recurs call your Varian Service Representative START AFTER INJ FAIL Soft Restart Automation to clear this Error If it recurs check that the inject switch installed on the injector nut is functioning properly Call your Varian Service Representative if the problem persists Page 96 User Manual 430 GC and 431 GC Varian Inc Errors STEP MOTOR ERROR The column oven vent stepper motor has failed to reach its internally set position within the step tolerance Turn the power off and then on again If the problem persists call your Varian Service Representative TEMP gt MAX COL SETUP Soft Change either temperature limit or the programmed temperature and re activate the method TEMP gt MAX COL TEMP Fatal Turn off instrument and turn it back on If the Error recurs call
14. at the flow rate listed below Adjustments to the carrier gas flow rate are made using the Injector icon for column flow and Detector icon for makeup and or reference flow Carrier Gas Helium Inlet Pressure 80 psig Purity 99 999 Column Flow Rate 30 mL min Reference Column Flow Rate 30 mL min Note Tightly cap gas filters when not used Prolonged exposure of the contents of the filter to room air degrades the performance of the filters User Manual 430 GC and 431 GC Varian Inc Errors ERRORS The 430 GC has an Error LED on the right bottom panel next to the Run LED and on the upper right area of the keypad The Error LED on the lower panel will illuminate when there is an Error that is considered fatal a hard Error A fatal Error can not be cleared by any user action other than turning off the GC and then turning it back on The Error LED on the keypad illuminates for any type Error If the Error LED on the keypad is illuminated and the one on the lower panel is not this is a soft Error you can clear the Error by removing its cause and activating a method or beginning Automation in most cases Error k 5V OUT OF RANGE Fatal Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative 5V OUT OF RANGE Fatal The 5V power line is outside of its allowed tolerance for correct GC operation Turn the power off and then on again If the problem persists call your Varian Service Represent
15. desired column flow rate Table 3 Split Injection Typical Conditions Varian Inc User Manual 430 GC and 431 GC Page 63 Injectors 1177 Split Splitless Capillary Injector Splitless Injection The classical splitless injection technique involves vaporizing the sample in a hot injector and slow transfer to the column The split state is OFF during the sampling period therefore all of the injected sample should enter the column The initial column temperature is maintained for at least the sampling time to trap all sample components at the head of the column At the end of the sampling period typically 0 5 to 1 5 minutes the split state is turned ON to vent any residual sample or solvent from the injector The following table describes typical method parameters for an isothermal splitless injection 50 C initial for 1 min ramp to 250 C at 20 C min hold 5 minutes Set the initial split mode to OFF and time program it to ON after 0 75 minutes In this case the splitless sampling time is 0 75 minutes The split ratio during the split ON period should be set to 50 Set the appropriate pressure or pressure ramp to achieve the desired column flow rate Table 4 Splitless Injection Method Parameters Carrier gas control Note that in all the above cases the parameters given are generic and need optimization including column position for specific applications Particular care should be taken with the large volume mode of
16. eet cit a ease see Sess ta saad cua W an aces see T AA ACE 6l Reassen ole TC VDDD orina r a e T E E 52 THERMAL CONDUCTIVITY DETECTOR TCD Jonis irii r aranne A A ANN 85 PUOL SCE U DRE E E EEE NOEN ENEN a Lan E NEE NOE O AONE 86 TEOD AdLUSINEN I S EANN NEET O E T N TO N E NNO EA NO 87 Setane the Filament Temperature Tani jssecs cacnees caseSecseacsaubacactdueubscaceovossecuwtcddactuosn EI 87 ODT OVO seca iahcond ce E E A ees wicuaibed ental uke EE EE OA 5S Bee Operas the TE D sacra teste ade E acct date Cuactesaasatdaveluicucudestt laa A 88 Ranse EMO ren E sua enes Haseae diauenay setanthe T 89 Lowe ERO TES O02 SO TAA Sia ie caters a aE n bu a siren UO dale cate sn Uda au bv deen NO dae weed ae ca Nba tdees we A 90 Esa aie Ga Xe ay Scie OOI a a UO TE RES Teme Tmt ON TNE eRe ORE RNa Tomer ee 91 Calculate Detector Sensitivity arresi EE E EEE E S Setwsainlonses 91 Calculate Detector Detectiy Myersa dave ER a A a n a 92 REVE POAN e E A A E TAR dca 92 Adjust 1 CD Carrier GOS T low Rale cscs eisai BEE CEEE ects Sars RETRE RE EENET EA 92 ERROR S N N 93 SHIPPING CLEANING AND DISPOSAL INSTRUCT IOONG sssscscccccccssssscsccccccccessscsoees 99 SAIPPINGIN STRUC HON inccasiatssssermsccaccnhenson mada E TETE 99 C LEANING INSTRUCTION S irrena E TEE E ETR 99 DISPOSAIINSTRUC TION Sasainn E e neces stdaccocmeceestatesaetine aes 2 99 O IIIIIIETT crcccssssssccccssssccccccsencceccssssssecesssssscccessesenscsssssseeeesssesssssooooossse
17. injection where the initial injector temperature and timing of the split states have to be carefully selected Page 64 User Manual 430 GC and 431 GC Varian Inc 1177 Split Splitless Capillary Injector Injectors 1177 Injector Assembly 1 Injector Nut 892597501 Injector Nut Wrench 390842300 Knob 392597101 Inject Switch Assembly 390820601 Septum 9 mm BTO lowest bleed CR298713 Marathon Autosampler CR239778 Advanced Green 3 general purpose CR246713 Septum pick 7200008400 5 Septum Purge Head Pneumatic Type Stainless Steel UltiMetal EFC21 392597301 392597303 Pneumatics 6 Purge head screw 2x 391866308 7 O ring Liner Graphite 6 5mm for Splitless 392611930 Viton 6 3mm 8850103100 8 Spacer 39258101 9 Glass Insert default 392611927 More liners 10 Injector Body Stainless Steel 392599401 UltiMetal 392599411 Manual 392599501 11 Column Ferrule see table below 12 Capillary Column Nut 394955100 13 Insulation 14 Cover ra le Figure 16 1177 Injector Assembly Teflon Vespel 40 Graphite Graphite SilTite Column ID Holes 60 Vespel Max 250 C Max 350 C Max 400 C Max 450 C Metal GC MS 018mm ID and smaller 1 CR214103 CR212103 R213103 a f cRam04 cR212104 CR213104 cR 0 25 mm ID Ca oret2t24 crasa crana o25smmiDandsmaer 1 o O O T o EE C2 eraa cras crama Table 5 1177 Column Ferrules 1 16 Varian I
18. injector sealing all exits from the injector and pressurizing the system Page 44 User Manual 430 GC and 431 GC Varian Inc Maintenance Parts and Supplies Use the following procedure to leak check the 430 GC Required Materials DUDU DDO A WARNING 1 No hole ferrule Unused septum Column fitting Crescent wrench Supply valve Leak detector When conducting leak check procedures it is important to completely seal all carrier gas exits including septum purge and split vent outlets The injector nut may be hot Lower the injector temperature to 50 C and permit the injector nut to cool before proceeding Remove injector septum nut and install a new septum An older septum can often be the source of a substantial leak Remove the column from the injector Use the appropriate nut and ferrule to seal the base of the injector For capillary systems use a capillary nut 03 949551 00 with a no hole ferrule 28 694590 01 The septum purge and split vent outlets must be sealed The septum purge outlet is located on the top frame surrounding the column oven behind the cap above the column oven door The split vent outlet is located on the left side panel of the 430 GC Seal the septum purge by removing the fitting from the septum purge valve and replacing it with a blank off plug 28 247071 01 You may set the Splitless Vent Flow in the 430 GC configuration to a flow of 0 and set the split ratio to off With all outlet
19. on the number of injections and whether the injections are by hand or with an autosampler In general the septum should be replaced every 50 100 injections or when symptoms of a septum leak are seen septum peaks in chromatogram These symptoms include changing retention times reduced detector response or a drop in column head pressure A The injector nut may be hot Lower the injector temperature to 50 C and permit the injector nut to cool before proceeding WARNING 1 Turn off the carrier gas supply to the injector 2 Remove the injector nut by turning it counterclockwise 3 Remove the old septum using metal tweezers or a septum pick 72 000084 00 Do not handle any internal parts of the injector with hands or gloves Lint free 4 Install the new septum again using tweezers to avoid contaminating the injector 5 Replace the injector nut and tighten it finger tight until you feel resistance from the septum then tighten an extra 1 4 turn Turn on the carrier gas supply monitor carrier pressure when power up On occasion to save time you may want to change a septum while the injector is hot Use an injector wrench 03 908423 00 to remove and reinstall the injector nut In all instances the column oven should be cool before removing the injector nut to minimize damage to the column caused by air entering the injector when the septum is removed Page 48 User Manual 430 GC and 431 GC Varian Inc Maintenance Parts an
20. tasucacaneshedecsnnasec cask adecame i aaanens ba dacune ieee tase ne estos ancanstheheusnae eee ceesbaaesane 39 THE PIE TE CLO WB aaa E AEE 40 THE DETECTOR KEY vrevsccececovacecavovenswcaduacexesdtacuvedduacuuctetestivaedudsueaessecasteduecanetetaeveaadvaseueesacds 41 Page 2 User Manual 430 GC and 431 GC Varian Inc Table of Contents THE 000 ACTO E aia siecpastosa seu negate de agaaiioanegus te necatanes A E E i 42 a en Oe NO IEOMUEMIIITTN ssssscccssssscccccccencccccssssscscessssssccccsccossssessscsssssccccssssssoooones 43 OE TINS cauranios oynador n Ra TE TE denated omnis nies heiten TEN EES 44 Checking and Renewing Gas SUPP WOS siscccscssssausnnstsassmacndadiresiescsdensnsehsasieseradnaatensceseseiansesuticstsseendtcs 44 EAEE EOE EA N EA E E E TEATE N E E T A 44 Gas Filter Cartridge Replacement nneenennnnnnnnnnnnnssneennnnesssssseerenssssseeresssssssrreossssssereeesssseeerressssses 46 INJECTOR MAINTENANCE c2c scsesecsscsnsacesaseneangaansequsbasaantonintacasnuanaanasansasunaawanentataseeannaasanbanianacteotemnenceianaenens 46 Septum Replacement scassaanchaasseisaraasaatacninaciesiseansvanascesnsauscaaiaassaussAaasaetsnansauaaeaieaadnabacsoaias onl vatnassauseateas 48 insert Replacement sisccsesassanisssesrsansdedidotecweasaad a ihn asad oa ALOR EAA 49 Removing the Glass MSC coscossccsnascadeaseneadeionncadaaraxideoieansdeeseasadagutanateamiatnensaaeaeoesdaacntseecaataeizeatanrodenaeenndaaanenes 49 Merine me as TE e S 5
21. that are NOT part of the method time program NOTE Press Q multiple times to jump between sections Use the or Er to step through the various entries one at a time Use T or to change values in editable fields Use to scroll down display pages and to accept changes made to editable fields denoted by flashing right cursor Pressing 000 displays the AutoSampler and External Events methods for editing Pressing Li allows turning the Injector heater ON or OFF and displays the injector data EF ona E Use and to add and delete program lines to Method time program tables Pressing fu allows editing and build column oven temperature programs Pressing FE allows turning the Detector heater and electronics ON or OFF and displays the detector data Page 28 User Manual 430 GC Keyboard and Display Varian Inc Display and Keyboard KEYPAD KEYS AND DISPLAY The described software version in this section has revision 6 93 THE STATUS KEY The Q key allows you to observe various instrument setpoints and actual conditions for thermal and gas control settings Once you are in the Status display mode you may use either to scroll down through the I t Status pages or 5 to scroll up through the Status pages Note that Status wraps around if you were to press until you observe the last line of Status and then press again you would observe the first Status page displayed again Simil
22. the Autolnjection selection you will be prompted for the sample vial the sample volume and the number of replicate injections you wish to perform You may cancel an Autolnjection by pressing the Er or Q keys Once a run is started you may either allow the run to complete or press the O to terminate it Page 30 User Manual 430 GC and 431 GC Varian Inc Display and Keyboard THE O STOP KEY The O is to terminate an executing method and cycle back to initial conditions The O key is also used to interrupt Local Automation THE ENTER KEY The amp key performs two functions 1 Ifan editable field has been changed the key will accept and execute that change 2 If no changes have been made then the e key will advance to the next line on the display If you edit a field you will press to accept the edited value and advance to the next line of the display Note that once you change the entry for a field a flashing underscore cursor will be displayed showing that the field is being edited If the underscore cursor is flashing and you do not want to accept the changed field you may press the er key located at the left side of the display to discard any edits that may have been made to that field If you press the edits will be accepted Varian Inc User Manual 430 GC and 431 GC Page 31 Keyboard and Display THE i NEW LINE AND S DELETE LINE KEY The Ey and keys operate on
23. used only to connect Ethernet devices to hubs or your company network RJ45 Connector This is a telephone jack style connector used for a several conductor style hardware connection 10BaseT RJ45 style connectors is used by the 430 GC TCP IP This particular Ethernet protocol supports the 430 GC 3900 GC CP 3800 GC and the Star 800 box You may find several network protocols supported by your PC Overview The following steps are required to establish Ethernet communication with the 430 GC and are described in the following sections Load the appropriate software onto your Workstation PC Set the network properties of your Workstation PC Connect cables Set up the BOOTP server to assign an IP Address to your 430 GC Configure your 430 GC into a Galaxie Workstation instrument Cee 2 ye Loading the Appropriate Software onto your Workstation PC Make sure that you have the necessary software installed on your Workstation PC Follow the instructions that come with your upgrade installation media to add 430 GC control to your Workstation Setting the Network Properties of your Workstation PC If you will be connecting your Workstation PC to your company network contact your Network Administrator to set your PC s network properties in the TCP IP section If you will be connecting your Workstation PC directly to one or more GCs with no connection to the company network then set the following network properties on your PC Ga
24. 0 C Electronics On Off Range 9 10 11 12 AutoZero Yes No Time Constant Slow Fast Slow Attenuation 1 to 1024 Initial Range Attenuation A Z Time Range Attenuation A Z Time Range Attenuation A Z Time Range Attenuation A Z Time Range Attenuation A Z H2 Flow 0 00 to 50 00 Air Flow 0 00 to 500 0 Makeup Flow 0 00 to 50 00 You may add lines to the Detector Attenuation program by pressing the Er key You may delete a line by scrolling so that the desired line is displayed and then pressing the E gt key Page 40 User Manual 430 GC and 431 GC Varian Inc Display and Keyboard THE Li DETECTOR KEY This key will give access to the Detector Flow settings TCD Detector Oven On Off Temperature 50 to 450 C Electronics On Off Detector Filament Temp 0 to 390 or O to 490 C Range 5 0 5 0 05 AutoZero Yes No Time Constant Slow Fast Slow Initial Polarity Positive Negative Filament Temperature Limit 390 or 490 C Attenuation 1 to 1024 Initial Range Attenuation A Z Time Range Attenuation A Z Time Range Attenuation A Z Time Range Attenuation A Z Time Range Attenuation A Z Detector Carrier Gas He H gt or N Ar Reference Flow Makeup Flow You may add lines to the Detector Attenuation program by pressing the F key You may delete a line by scrolling so that the desired line is displayed and then pressing the Es key Varian Inc User Manual 430 GC and 431 GC Page 41 Keyboard and Display THE 000 AUTO
25. 0 a E a A EEI AAEE I A EE E E ET EET AAT TE TT AT al THE 1177 SPLE SPLIILESS CAPILLARY INIBCUOR wetsicwssntesuesbetsscnscccneuienesoecintoseeebetoecw stings OA 53 TOOTS o e L177 CCU ara an E TA E Oa 54 AMONG SAG O E iraa AAA E EAE 54 EEEE T E E a EE EE E N EAO E ATE EE A E A ET AA ES 54 EPEE e GS Of E EAE E AO A GS 55 aM e e A i E EE E eased ce cand oanioecoestook 55 SPE es a E E E EAE OEE E NEE EEE TEE 53 1177 Electronic Flow Control EFC cccccccccccsscccccsecscccsesccccsesccccuesccecsececcuessscucueseseuuscescuesesecuessseunses 56 TIT 7 Manual PRCUINGICS oscccczvscssasasdecoragiecescs inais naaa i aS nA a aaeain iienaa E Wiis 59 Operation of the 1177 ANF CCL iecssccscccssassascancasssausasanaaeacosiasisaaaes deana sad aandoutonesdactotna dansai ee 59 Column Ties Pal AIO seieren re E con arose soutonsasesce ataeiacboaseatunds 59 Condihon the Conies ises eE E Ees ETE Sr e 59 Columa Tistall anim tt DEtECIOL ici sntrceriveccaetvendunvabienvieusscndoeneired ueedawubseduelyshicetoandhTesislslustedaavobsiedutsnlbendennbiedcclust 59 SRE LIT GOST TOWT AOE rE E RE ETE OET EO 60 PTC FNCU IAC rE AE E AER E E EAEE E E E EE ER 60 SEPUR TUTOE COUTO OR irinin OR CE E REEE E EE EEEO 61 Mo UCU IIT T EEE ENE EE R EEEE say saicete E N 62 Tools and eguipmient needed sarsies e e E EE 62 LL 7 Modes of OPerd ON sisisi nice aa Eea raea AOE 63 gt Le Ui eO r Ter ery neon erent nr TTT er or er rete 63 IE OS COLO iets tetas ews onde os oso es tao hase achalasia case ile
26. 00 AutoSamplers if the sample injection time the time between the insertion and removal of the syringe needle from the injector exceeds the peak width peaks can broaden tail or chromatographic performance will be degraded With broader later eluting peaks it is less important that you inject the sample quickly The split ratio fraction of sample that enters the column is the ratio of the flow of carrier gas out the split vent to the flow through the column Splitless Mode Varian Inc The 4 mm insert packed with glass wool is typically used for isothermal splitless injection The small capillary section of the glass insert fits around the syringe needle and restricts backflash of the sample vapor during injection In the splitless injection mode the sample enters the column during a variable sampling time at the beginning of the analysis This period is typically 30 90 seconds during which there is no flow from the injector to the split vent After the sampling time the injector is vented to remove any residual solvent and sample out of the injector User Manual 430 GC and 431 GC Page 55 Injectors 1177 Split Splitless Capillary Injector 1177 Electronic Flow Control EFC The EFC module used on an 1177 injector is the EFC21 or EFC25 The EFC21 or EFC25 type is designed specifically for the 1177 and 1079 PTV injectors to support their various modes of operation It duplicates the behavior of the Split Splitless manual pneuma
27. CTOR CONNECTIONS AND HARDWARE Page 78 The 430 GC uses either a Flame lonization Detector FID or a Thermal Conductivity Detector TCD to detect compounds in the effluent of the column Both are installed at the factory to begin using your 430 GC you simply need to connect the following gas supplies see FID section or TCD section as it relates to your GC Make up typically the same gas as the carrier gas set to at least 80 psi and no more than 100 psi Hydrogen set to 40 psi and Air set to 60 psi The default settings in the 430 GC for the make up 25 mL min hydrogen 30 mL min and air 300 mL min are the recommended settings for those gases If you do need to ot Be the gas flow rate you desire to change is displayed User Manual 430 GC and 431 GC Varian Inc Detectors THE FID DETECTOR Varian Inc The flame ionization detector FID is the most sensitive gas chromatographic detector for hydrocarbons such as butane or hexane With a linear range for 6 or 7 orders of magnitude 10 to 10 and limits of detection in the low picogram or femtogram range the FID is the gas chromatographic detector for volatile hydrocarbons and many carbon containing compounds The FID detector employs hydrogen as the combustion gas which is mixed with the column eluent helium nitrogen or other appropriate gas and burnt at a small jet situated inside a cylindrical electrode A potential of a few hundred volts is applied be
28. Column Ferrule Selection Table FerruleID_ Column ID Figure 7 Column Ends Varian Inc User Manual 430 GC and 431 GC Page 17 Installation New graphite ferrule 1 4 turn past finger tight 1 4 to 1 2 turn past finger tight may be required to achieve a seal Used graphite ferrule 1 4 turn past finger tight If a different size of column is used more tightening may be required New polyimide graphite 1 4 to 1 2 turn past finger May require retightening after ferrule tight first or second programmed run Over tightening will destroy ferrule and seal Used polyimide graphite 1 4 turn past finger tight Re use only on same size ferrule column New 100 polyimide Not recommended with 1041 ferrule Injector Used 100 polyimide Not recommended with 1041 ferrule Injector Table 1 General Tightening and Retightening for Common Ferrules Page 18 User Manual 430 GC and 431 GC Varian Inc Installation CONNECTING GASES Connecting Gases The only carrier gas allowed for the 430 GC is 99 999 pure helium or better Carrier gas supplied from cylinders or manifolds should have a two stage regulator with O to 100 psi low pressure stage Set cylinder regulator pressure to 80 psi Follow the steps below to connect gas supplies to your 430 GC 1 1 8 Copper Tubing Varian Inc Cut required lengths of heat cleaned 1 8 copper tubing for the carrier gas plumbing Clean the ends of the tubing with a metal file
29. DRAFT ay xs VARIAN Varian BV Herculesweg 8 4330 EA Middelburg The Netherlands ay me VARIAN 430 GC and 431 GC User Manual North South America 2700 Mitchell Drive Walnut Creek 94598 California USA Tel 1 9259392400 Fax 1 9259452360 or 1 9259452344 2008 Varian Inc All Rights Reserved Europe P O Box 8033 4330 EA Middelburg The Netherlands Tel 31 118671000 Fax 31 118623193 Printed in the Netherlands Australia East Asia 679 Springvale Road Mulgrave Victoria 3171 Australia Tel 61 395607133 Fax 61 395607950 CP501406 Rev February 7 2008 Warranty Read Before Operating Important Safeguards The following items are frequently not recognized or are overlooked by new users while learning to operate a GC or a GC MS They are brought to your attention to safeguard against damage to your equipment Carrier gas must be flowing through the column before heating the column oven Carefully evaluate columns that have been heated with no carrier gas flowing through and discard if damaged Ensure the injector contains a septum and there is a positive flow of carrier gas before heating the column The column outlet in a GC MS system is at a vacuum Do not use columns which are wide bore and short in length with constant flow at low flow rates since the inlet pressure may be less than the ambient 1 atmosphere An inlet pressure less than ambient will be indicated a
30. EEEE A A A E E EAE A E EA 25 CONNECTING POWER dscissicaitadaaySensiasvaeioadivauciiaiabedocareauseisinsedeavadutesssadeleduataundssavweseudcauhossaubteetuntdusisnaubioes 26 FACTORY DEFAULT STATES AND SETTINGS cccccceccsscccscccscccsccessccesccesscecceesseesccescseesscesssessseusceeceeass 26 CALIBRATING THE CP 8400 8410 AUTOSAMPLER c ccccccsscccscccusccesccesccesccuscecssceucseesceesesesseusceuceeacs 26 INSTALLATION CONC Oscars were sicccienssarsb E acts nares rE a T 27 L ME ccccccccccccccccccccccccccccccvccccccccccccccevccceccccccccecsccccecccceccceccccececcccescceccocs 29 SATU EE irene rer rr re eer rrr ner rn rr eer re nr er ree 29 i y wd a 0 cal 1 Sel Se eT PN eee RECT Pe CER CTeT TRE ERE CTT TNT ENE Cer ERT CT aRe TTT Crane eer eee 30 SLART EEY eraino rii EA EE dyantenativaaheceacideracitsanesacteaataestoantequnededemetaatiees 30 THE i ss BO celal Gi ois E A AA AAA N AAA AAE Oe AA EIA 31 THE ANIER WEN cc anci danced cdeacace a cdeacacaedeie ade viuedscicaincede taicacsedainateeieeiscieeseceeeete 31 e THE NEWLINE AND DELETE LINE KEY cicccccccccscccsccccccccccccccccscececsesstssssssccccceceees 32 THE SETO FEY ooann EEEN AEE EA E EEOAE AEEA AE E NAERAN 33 THE O COMMAND EEY narerriicerrr ri OAERTN AEEA ATENEA 35 ae E pie OD o gt ke ooops THE Li INIECIOR REX perrito i EEEE EEE EER 37 THE Li INIECTOR KEY orrea E TAER EEEN 38 THE CJ AEN NY ac htace nec
31. Filter I I I I I I I j I i hots leven Charcoal GP742210 sibver color I I I I I I l I l I Pressure Sensing Figure 18 EFC23 Flow Diagram e See Pencil Filters on page 51 Varian Inc User Manual 430 GC and 431 GC Page 75 Injectors 1041 On Column Injector The type EFC24 flow diagram shown below is an indication of the control mechanism of this type of EFC module GC Control l l l l l I l BDA taye Digital Flow Control Molsieve Charconl CPP42210 siver color Carrier Gas inlet Headspace gt Flow sensor a E Sampler or other devices rt I Digital Pressure Control o a vent uk Figure 19 EFC24 Flow Diagram See Pencil Filters on page 51 Setting the Carrier Gas Flow With type EFC24 equipped injectors a flow range of 0 100 mL min may be set from the 430 GC keyboard Press the I key and select the desired pressure and total flow rate Both the pressure and total flow are programmable use the insert line and delete line to build the tables as desired and then edit the entries as needed Page 76 User Manual 430 GC and 431 GC Varian Inc 1041 On Column Injector Injectors Flow Rates for Operation Recommended flow rates differ depending on the column Capillary Mode When operating the injector
32. GC The 430 GC is designed to be a single channel to use and easy to maintain Gas Chromatograph The Injector and Detector of the 430 GC are all electronic controlled It may be equipped with either an 1177 split splitless or a 1041 On Column injector and either an FID or a TCD detector Optionally it may have liquid CO column oven cryogenics additional gas sampling valves and an Ethernet communications option Typically the only operator interactions with the GC are to turn on the GC put vials into the AutoSampler carrousel change the AutoSampler syringe when required change the column when needed and change the injector septum when needed Column dimensions temperature limits A S position calibration and other configuration functions are entered through the 430 GC keypad methods can be built from the Workstation and downloaded either manually or as part of an automated SampleList or Sequence or they can be built from the keypad All electrical connections and carrier gas supply connections are made at the back of the 430 GC on page 13 Page 6 User Manual 430 GC and 431 GC Varian Inc Introduction KEYPAD The Varian 430 GC is an all electronic single channel gas chromatograph The keypad relies on icons to identify the actions of the keys on the keypad on page 29 The keys 000 AUTO SETUP COMMAND vif INJECTOR OVER wa DETECTOR with a LED indicate that entries underneath are prese
33. GC firmware that an external device has been connected The 430 GC is then waiting for Ready In pin 1 to get start permission Page 14 User Manual 430 GC and 431 GC Varian Inc Connector J22 External Events Installation In the software of the 430 GC under key 000 AUTO on page 36 you will find the External Events 1 and 2 In combination with the Connector J22 it is possible to switch a relay or other devices J12 SERVICE NOA J22 EXTERNAL EVENTS Varian Inc User Manual 430 GC and 431 GC Connector J22 430 GC External Events 4 24 Volt DC 53 2 Out 2 maximum 700 mA 24 Volt DC ot gt Out 1 maximum 700 mA Figure 5 Connector J22 External Events Page 15 Installation Column Installation FID NOT TO SCALE a Q S TCD V 1177 Capillary Column Nut S P N 03 949551 00 3 S r A 4 He Ferrule 3 7 cm 3 9 cm 9 5 cm Fused Silica Column 1041 Injector insert column until seated Figure 6 Column Insertion Depths Column Length and Dimension Procedure 1 Install the capillary column to the correct distances as outlined in the above Figure 2 Press and press aa until the COLUMN SETUP ENTER LENGTH is displayed and enter column length using the T or 4 key and press 3 COLUMN SETUP ENTER I D is then displayed and enter the column internal diameter using T or 4 key
34. Your AutoSampler Autolnjector manual will describe each of these parameters in detail Autosampler Page 36 AutoSampler Mode Sample Penetration Depth Solvent Penetration Depth of Pre Injection Solvent Clean Flushes of Post Injection Solvent Clean Flushes of Pre Injection Sample Clean Flushes Clean Solvent Source Vial Default Clean Vial Default Clean Volume uL Default Clean Drawup Speed Number of Default Clean Strokes Air Plug After Sample uL Sample Air Gap Number of Fill Strokes Fill volume for Fill Strokes uL Viscosity Delay sec Plunger Speed during Fill uL sec Plunger Speed during Injection uL sec Pre Injection Delay sec Post Injection Delay sec Use Internal Standard Internal Standard Vial Internal Standard Size uL Internal Standard Drawup Speed uL sec Internal Standard Pause Time sec Internal Standard Air Gap Vial for Solvent Plug Solvent Plug Size uL Solvent Drawup Speed uL sec Solvent Pause Time sec Solvent Air Gap User Manual 430 GC and 431 GC Standard Split Splitless Volatile Viscous Neat Standard OC User Default 90 0 to 100 Default 90 0 to 100 Default 3 0 to 99 Default 1 0 to 99 Default 0 0 to 99 Default 1 1 2 3 1 amp 2 1 amp 3 2 amp 3 1 amp 28 amp 3 Default 1 1 2 3 Default 5 0 to 5 or 10 or 100 Default 5 0 to 25 or 50 Default 1 1 to 10 Default 1 0 to 5 or 10 Default No Yes or No Defaul
35. and press aa 4 Column length and dimension procedure is complete If the 430 GC is equipped with a septum purge for the 1177 split splitless injector follow the Septum Purge Calibration procedure on page 61 Page 16 User Manual 430 GC and 431 GC Varian Inc Installation Before installing your column make certain that the ends of the column are in good shape and the column ends are cut perpendicularly Preparing Column Ends To ensure a leak free connection of capillary columns the ends of the column must be cut squarely and as smoothly as possible To achieve this a proper scoring tool is required A ceramic scoring wafer P N 01 900158 00 is recommended Before cutting the sealed ends of the column slide the capillary column nut over the column end Install the appropriate Vespel graphite Vespel or graphite ferrule onto the column with the tapered end toward the capillary column nut This procedure prevents contaminating the column with ferrule material 1 Grasp the column securely between the thumb and forefinger of one hand Score the column once lightly with the cutting tool N See figure next page bend column slightly to break it at the score mark A magnifying lens recommended 20X magnifier P N 00 997369 00 is necessary to determine the quality of the cut If small splinters of silica or some of the outer coating remains on the column end it is advisable to make a fresh cut vA x 6 lt 90
36. ardware to facilitate use of the injector with 1 8 metal packed columns In addition adapter kits are available for 1 4 columns Full instructions on converting the 1041 to packed column use are included with the packed column kit Available in manual pneumatics and electronic flow control EFC for different laboratory requirement Choose from EFC23 constant flow control and EFC24 constant pressure control and constant total flow control for different application requirement Varian Inc User Manual 430 GC and 431 GC Page 71 Injectors 1041 On Column Injector Automatic Start Switch The automatic start switch is a spring loaded actuator that fits over and is aligned with the injection port of the 1041 universal injector nut The GC run is started when the actuator is depressed by the syringe barrel or manually pressed at the moment of sample injection The GC run can also be manually started by pressing on the keyboard The injector nut and automatic start switch assembly may be very hot during instrument operation and should not be touched with unprotected hands WARNING Page 72 User Manual 430 GC and 431 GC Varian Inc 1041 On Column Injector Injectors Injector Assembly and Insert A cross sectional view of the 1041 Universal Injector with insert and 530u ID fused silica capillary column is shown below yee oN Septum 9 5 mm 4 Injector Body on SON Figure 17 1041 Universa
37. arly if you were to press t Er immediately after entering Status you would observe the last page of the Status display mode Status pages are summarized below e General Status Instrument State vial if A S present run time and column oven temperature Thermal zones actual temperatures Active method Injector EFC Pressure Status Injector EFC Flow Status Detector EFC Flow and Signal status Software version Error Log GC MAC and IP address Q Performs no operations on the GC except to change the display Thus you may cancel any change to an editable field by pressing Q instead of Varian Inc User Manual 430 GC and 431 GC Page 29 Keyboard and Display THE UP LINE KEY g simply moves the display to the immediate preceding page for viewing It does not operate on any function of the GC other than the currently displayed page If the display is already at the top of a section then pressing Er will take you to the last line of the section THE START KEY The key operates on your 430 GC in one of two ways lf NO CP 8400 or a CP 8410 is present pressing Ovi cause the 430 GC to execute the currently active method The run time will begin incrementing and any time programs will be executed If a CP 8400 or a CP 8410 is present pressing Q allow you to either perform an Autolnjection or start the currently active method The default action is to perform an Autolnjection Upon accepting
38. ative A S STROKES gt LIMIT Soft This is an advisory message that the plunger stroke count has exceeded the limit that was set for it You should change the syringe and zero the plunger stroke counter soon after you observe this message A S CAR SENSOR ERROR Fatal The AutoSampler carrousel sensor has failed to conform to its expected operation Turn off the GC and then on again If the problem persists call your Varian Service Representative A S CARROUSEL ERROR Fatal The A S carrousel base has encountered one or more internal Errors and has failed to properly come up Turn off the power and then turn it back on If the problem recurs call your Varian Service Representative A S COMM ERROR Fatal The AutoSampler Autolnjector has experienced an error during communications that was unrecoverable Turn GC power Off and On If the problem persists call your Varian Service Representative A S FAILURE Fatal The A S has failed to properly come up Turn off the power and then turn it back on If the problem recurs call your Varian Service Representative A S OVER MAX PLNG SP Soft This message is displayed if you have built a method with one syringe that supports a fast injection speed and have subsequently changed and configured a different syringe Correct the syringe speed in your method for the new syringe A S PLUNGER ERROR Soft The syringe plunger has either jammed or become inoperable Check that the syringe is properly mounted and
39. atograms illustrate the high sensitivity and detectivity 18 ppm of Neon in air that is possible with the TC Detector Also a comparison of chromatogram A with chromatogram B shows that with the use of the bridge output signal amplifier you can obtain the same analytical results at half the filament current thereby extending the lifetime of the TCD filament The Neon peak in chromatogram C illustrates how you can use a high filament current 300 mA with a high amplification setting to increase the effective sensitivity of the TCD 3 3 A Filament current 290 mA 1 Ne 3 Filament temperature 300 C 2 O2 2 At 1 5 minutes range and attenuation changes from 2 x 0 5 mV to 128 x 5 0 mV B Filament current 151 mA Filament temperature 160 C At 1 5 minutes range and attenuation changes B c from 2 x 0 05 mV to 128 x 0 5 mV C Filament current 299 mA Filament temperature 300 C At 1 5 minutes range and attenuation changes g from 4 x 0 05 mV to 128 x 5 0 mV w w Conditions Carrier gas He 2 S Sample Air 2 mL o v r Column 10 ft molecular sieve 5A z 30 60 mesh at 50 C lt 113 z Injection Gas sample valve n g TCD oven temperature 120 C lt lt rr rs mana rr rs a rr rs a 0 3 6 9 0 3 6 9 0 3 6 9 MINUTES Figure 22 TCD Sensitivity and Amplification Page 90 User Manual 430 GC and 431 GC Varian Inc Thermal Conductivity Detector TCD Detectors High Currents 300 mA To obtain the
40. bed below next page It is important that you operate your equipment in accordance with this instruction manual and any additional information which may be provided by Varian Address any questions regarding the safe and proper use of your equipment to your local Varian office Page IV User Manual 430 GC and 431 GC Varian Inc Safety Information A A CAUTION WARNING Information to aid you in Alerts you to situations Alerts you to potentially obtaining optimal that may cause hazardous situations that performance from your moderate injury and or could result in serious instrument equipment damage and injury and how to avoid how to avoid these these situations situations Warning Symbol WARNING SHOCK HAZARD WARNING CHEMICAL HAZARD WARNING BURN HAZARD WARNING EYE HAZARD WARNING FIRE HAZARD WARNING EXPLOSION HAZARD WARNING RADIATION SOURCE WARNING MOVING PARTS Warning Description Hazardous voltages are present inside instrument Disconnect from main power before removing screw attached panels Hazardous chemicals may be present Avoid contact especially when replenishing reservoirs Use proper eye and skin protection Very hot or cryogenically cold surfaces may be exposed Use proper skin protection Eye damage could occur either from flying particles chemicals or UV radiation Use proper eye and face protection The potential for fi
41. ce see Figure 21 below Secure the signal probe by tightening the knurled nut Make sure the notch in the detector tower arm does not cut the O ring seal 10 Connect the ignitor cable to the ignitor probe and the signal cable to the signal probe TOP VIEW Detector Tower Ignitor Coil Spring Clip Flame Tip Figure 21 FID Top View Varian Inc User Manual 430 GC and 431 GC Page 83 Detectors Flame lonization Detector FID Page 84 User Manual 430 GC and 431 GC Varian Inc Thermal Conductivity Detector TCD Detectors THERMAL CONDUCTIVITY DETECTOR TCD Varian Inc A TCD detector consists of an electrically heated wire or thermistor The temperature of the sensing element depends on the thermal conductivity of the gas flowing around it Changes in thermal conductivity such as when organic molecules displace some of the carrier gas cause a temperature rise in the element which is sensed as a change in resistance The TCD is not as sensitive as other detectors but it is non specific and non destructive The Thermal Conductivity Detector TCD is mounted directly above the column oven on the 430 GC The TCD electronic Board is installed in the electronics cabinet on the back right side of the instrument TCD operating parameters are set at the 430 GC Display Keyboard These include carrier gas type detector temperature range temperature limit and filament temperature The gas flows are set and controlle
42. cking and Renewing Gas Supplies The pressure of the various GC gas supplies should be checked on a weekly basis and the following guidelines used for frequency of renewing supplies The carrier gas supply cylinder should be changed when its pressure drops below 200 psi This ensures that high purity carrier gas is always supplied to the instrument With typical usage on one gas chromatograph a cylinder of carrier gas should last for three to six months When a new cylinder is installed the regulator and tubing should be purged with carrier gas before connecting to the GC This will avoid introducing a large amount of air into the GC Leak Checking Leak checking is one of the most important maintenance tasks performed on a GC Leaks in the GC system may lead to poor chromatographic performance or may damage components such as the analytical column The presence of oxygen in the GC carrier gas at elevated temperatures can lead to permanent column phase degradation While the use of an oxygen filter on the carrier supply to the instrument can help leaks downstream of the filter are generally more likely to be the problem The use of soap based leak detection fluids is not recommended for a high A performance capillary Gas Chromatograph due to the danger of introducing contaminants into the system CAUTION The most important step in leak checking is to verify that the GC system can hold pressure This is done by removing the column from the
43. column stand then prepare column end and complete column connections to both the injector and detector fittings click here for more details on page 17 Column connection to Injector A CAUTION Page 74 IMPORTANT ALIGNMENT OF THE CAPILLARY COLUMN When a 0 53 mm ID capillary column is used in combination with the Varian 1041 injector alignment of the column is critical Use the following steps to precisely align the capillary column Unless this procedure is followed the injection syringe may damage the top of the column or peak tailing may result Install the capillary injector insert nut and the reversed ferrule on the column Uncoil about 20 cm of the injector end of the column Gently push the column fully up into the injector approximately 9 cm until the column comes to a firm stop This correctly positions the column against the upper end of the injector insert The column must go in the full distance If it does not the injector will not function properly Tighten the column nut just enough to prevent column movement Manually insert the syringe that will be used with the column into the 1041 injector checking that the syringe goes into the injector completely with no binding or interference If interference occurs repeat the above column insertion procedure until the syringe moves smoothly into the injector Continue to hold the column firmly in place as you tighten the column nut carefully and only enough to hold t
44. completely cool use a metal tool Such as tweezers or a hooked wire to remove parts from the tower assembly Place parts on a clean Kimwipe Never place them on a counter or painted surface 7 Remove the flame tip assembly from the detector base Take care not to break the ceramic flame tip tube or the Vespel graphite or graphite ferrule 8 Remove and discard the aluminum seal washer from the detector base 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 430 GC and 431 GC Page 81 Detectors Flame lonization Detector FID A CAUTION 6 Page 82 Reassemble the FID To reassemble the FID proceed as follows 1 If you removed the detector base from the plenum restore the base to its former position and reinstall the four screws holding the oven to the plenum Install the flame tip in the detector base e f you are installing the flame tip with a new Vespel graphite ferrule tighten the assembly finger tight plus an extra 1 6 turn e If you are installing the flame tip assembly with a used graphite ferrule tighten about 1 3 turn past finger tight The Vespel graphite ferrule supplied with the GC has a maximum temperature limit of 350 C If it is necessary to operate the detector above 350 C you may need to replace the Vespel graphite ferrule
45. contractual or as needed basis upplies contact your local Varian office Argentina Buenos Aires Tel 54 11 4 783 5306 Australia Mulgrave Victoria Tel 61 3 9560 7133 Austria Poettelsdorf Tel 43 2626 20090 Benelux Middelburg Tel 31 118 671500 Brazil and Latin America S Sao Paulo Tel 55 11 3845 0444 Canada Mississauga Ontario Tel 800 387 2216 China Beijing Tel 86 106310 8550 Europe Middelburg The Netherlands Tel 31 118 671 000 Varian Inc France Les Ulis C dex Tel 33 1 6986 3838 Germany Darmstadt Tel 49 6151 7030 India Mumbai Tel 91 22 2570 8595 97 Italy Torino Tel 39 011 997 9111 Japan Tokyo Tel 81 3 5232 1239 Korea Seoul Tel 82 333 665 5171 Mexico and Latin America N Mexico City Tel 52 5 55 5239465 026 Russian Federation Moscow Tel 7 095 937 4280 Spain Madrid Tel 34 91 472 7612 Sweden Solna Tel 46 8 445 1620 Switzerland Steinhausen Tel 41 848 803 800 Taiwan Shih Chi Tel 886 22 698 9555 United Kingdom and Ireland Oxford Tel 44 1865 291500 Venezuela Caracas Tel 58 212 285 0320 2494 User Manual 430 GC and 431 GC United States Walnut Creek California USA Tel 1 800 926 3000 GC and GC MS Tel 1 800 367 4752 LC ap mS VARIAN http www varianinc com Page IX Safety Information Page X User Manual 430 GC and 431 GC Varian Inc Table of Contents Table
46. d CP736530 filter kits replacement filters can be ordered from Varian Replacement parts on page 101 or click here INJECTOR MAINTENANCE The injector is the component of the gas chromatograph that requires the most frequent maintenance The sample is deposited in the injector leading to potential contamination and build up of non volatile deposits The most frequent injector maintenance is septum replacement Insert replacement and injector cleaning are also very common To access the injector and the top of the GC undo the captured thumb screws on either side of the detector cover and tilt it back Page 46 User Manual 430 GC and 431 GC Varian Inc Maintenance Parts and Supplies Unscrew the 4 retaining screws holdng the top cover to the GC Lift Top cover slightly and gently slide it towards the rear of the GC The top cover is equipped with rollers Note that you do not need to remove the CP 8400 8410 AutoSampler to access the injector To replace the cover slide it forward until it drops into place Note that the position of the CP 8400 8410 AutoSampler is fixed relative to its mounting hole You do not need recalibrate your AutoSampler unless you unscrew and remove it from the top cover Varian Inc User Manual 430 GC and 431 GC Page 47 Maintenance Parts and Supplies Septum Replacement The injector septum is an expendable part and must be replaced on a routine basis The frequency of replacement depends
47. d Supplies Insert Replacement The 1177 is a Split Splitless capillary injector Typically to change from Split operation to Splitless may involve changing the injector insert The insert should also be cleaned or replaced on a routine basis This is especially important when dirty samples are being analyzed Removing the Glass Insert Follow these steps to remove the glass insert from the 1177 Injector A The injector nut may be hot Lower the injector temperature to 50 C and permit the injector nut to cool before proceeding WARNING 1 Use the injector nut wrench to remove the injector nut Place the nut on a clean surface e g Clean tissue 2 With tweezers or septum pick lift the edge of the septum Remove the septum Note Replace the injector septum each time the glass insert is replaced 3 Remove the start switch by unscrewing the retaining nut 4 Unscrew the two captive screws holding the septum purge head to the base Carefully move this assembly straight up until it clears the top of the insert 5 Use a laboratory tissue or clean tweezers to grasp the glass insert and remove it from the injector body Use care when removing inserts from the injector Inserts can be at high temperatures and are likely hot Place hot inserts on a clean glass or metal WARNING surface only 6 To remove the O ring from the glass insert use clean lab tissues to hold the O ring and the glass insert Gently turn the glass insert
48. d Varian service representative should perform service procedures such as repair or replacement of electronic components For maintenance problems where mechanical or electrical assemblies need to be repaired or replaced please call your local Varian service center Certain maintenance tasks should be performed on a routine basis to ensure that the 430 GC will continue to operate at optimum performance Following is a brief summary of some common maintenance tasks and their typical frequency Replacement parts on page 101 or click here Maintenance Task Check column nuts are tight Condition column Replace injector inserts Check gas supplies Leak check Monthly Change gas cylinders When pressure drops below 200 psi Condition system Semi annually Replace aas filter cartridaes Semi annually or when indicator i J shows filter is saturated Replace Column Periodically or when required Table 2 Maintenance Schedule Varian Inc User Manual 430 GC and 431 GC Page 43 Maintenance Parts and Supplies GENERAL GC MAINTENANCE The most common GC maintenance tasks are checking and changing gas supply cylinders leak checking and changing gas filter cartridges These tasks should be performed at the frequency suggested in the above table The following procedures are critical to the successful long term operation of a 430 GC It is very important to leak check the system on a routine basis and to ensure the quality of gas supplies Che
49. d either from the 430 GC Display Keyboard if detector EFC is installed or at the pneumatics panel User Manual 430 GC and 431 GC Page 85 Detectors Thermal Conductivity Detector TCD Page 86 Initial Set Up To set up the TCD proceed as follows Note that the TCD is a two channel detector and requires both a sample flow of carrier gas and a reference flow of the same gas Either channel can be used as the sample stream but there must always be a reference stream 1 Connect the gas lines to the appropriate bulkhead fittings on the GC 2 Check the gas supply pressures Set at 80 psig 3 Establish carrier gas flow through the Sample right side of the TCD and an equal Reference gas flow through the Reference left side of the detector If you are using a capillary column the total of column flow and makeup flow should equal the Reference gas flow 4 Perform a Leak Check on both the Sample and Reference pneumatics before proceeding to apply power to the TCD filaments Even a small leak can supply enough oxygen to cause filament oxidation and consequent baseline drift 5 Select 3 ner EFC and set the gas type to He H2 or N2 based on the selected gas type The TCD is equipped with Detector EFC The carrier gas and detector EFC gas selections must be the same type Oid EF Hydrogen For all other carrier gases select the N2 Ar setting User Manual 430 GC and 431 GC Varian Inc Thermal Conductivity Detector TCD De
50. e Representative DET RESPNSE TOO SLOW Fatal Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative DET TEMP PROBE OPEN Fatal Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative DET TEMP PROBE SHORT Fatal Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative DET TEMP TOO LOW Fatal The detector oven temperature is below the allowed temperature Turn the GC off and then on again If the problem persists call your Varian Service Representative DIAG TEMP ERROR Fatal The actual temperature of a temperature controlled resistor block used for automatic instrument calibration has exceeded its allowed temperature set point Turn the power to the GC off and then on again If the problem persists call your Varian Service Representative FAN UNPLUGGED IN RUN Fatal Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative Varian Inc User Manual 430 GC and 431 GC Page 95 Errors FID FLAME OUT Soft The FID flame has been quenched The flame detection is based on a background signal intensity of approximately 330 microvolts It is possible for very clean GC systems to have baselines less than 330 microvolts causing spurious flameout messages If you suspect that the flameout message is spurious use a shiny cool metal object Such as a box end wrench
51. e ede ei Ae eeieie adicee 10 INSTALLING THE CP 8400 8410 AUTOSAMPLER cccccsssccccssecccessecccaeccecueeceeaeeecesseeceeseecesaeeeeesaeeees 11 Mounting the CP S400 8410 onto the 430 GC cccccccccccccsnsssseeesesseeeceeeeeeeeeeeaaaaeeeneseeeeeeeeeeeeeeaaaaaaaaeaes Il Connecting AutoSampler Power and COMMUNICATION CADLES ccccccccccsseesescceeeeenseesseceseeeaaaaeseseess 12 430 GC REAR PANEL CONNECTORS ssisiactasstteseeaitade hain ade ele Be ee 13 Connector IZS VNC ANGO SOUL wires Ai iA GS A A ARE RE 14 CONECO S22 TRXICING L VENIS cahaorsecucccvnsiehies dead sacautel teiectsvucsnites doacimsdund asides E tctavadacbaseees detec 15 CONES TANG OW EREE RE E a N tuk a ducuptaui aa a a aa 16 Column Length and Dimension PVOCCAUTC vis secs divsasiuiceldecamisvasaclesssamedenstuledelsleceuesdanastiaiduaaseeidetetseceweenss 16 Peepar no COMMITS esan a tbundat Set deus A A taconite sae A RET 17 CON NEG TING GASES onara e E a 19 COE I GASES oaa E E E A O E A E A AE AR R 19 SE UP INEOR MATION orian A T A 20 FEIHERNET COMMUNICATIONS ccccctessxensatwsre ar N 20 NECIWOIR TD CIININOLO ON urii E E E E E E ade Cartunnionte 23 Loading the Appropriate Software onto your Workstation PC ccccccccccssseeescccceceeneeeseeecceesesaaaaeeees 24 Varian Inc User Manual 430 GC and 431 GC Page 1 Table of Contents Setting the Network Properties Of your Workstation PC ccccccccccccssssseescccccccenaeeeseeceeeeeaaaseseeceeeeeeeaaaes 24 CONC CIOS EE setae sata
52. e is dirty never clean the inside clean it with a soft clean cloth dampened with mild detergent e Never use alcohol or thinners to clean the 430 GC these chemicals can damage the case e Be careful not to get water on the electronic components e Do not use compressed air to clean DISPOSAL INSTRUCTIONS When the lifetime of the 430 GC or parts of it has reached the end of its useful life disposal must be carried out in accordance with all environment regulations applicable in your country Varian Inc User Manual 430 GC and 431 GC Page 99 Shipping Cleaning and Disposal Instructions Page 100 User Manual 430 GC Varian Inc Replacement Parts REPLACEMENT PARTS Replacement Parts for the CP 8400 AutoSampler CP 8410 Autolnjector 1177 Injector 1041 Injector 1061 Injector and 1079 Injector CP 8400 8410 Vials 2 mL Ultra GC MS vials screw top wide opening clear glass 9 mm caps w Ultra GC MS septa 392611979 100 pk 2 mL Ultra GC MS vials screw top wide opening amber glass 9 mm caps w Ultra GC MS septa 392612016 100 pk 2 mL Vials Crimping tool 11 mm 100 pk 5 mL Ultra GC MS vials 20 mm x 38 mm solvent vials 39261 1980 and CP 8410 sample vials w snap cap and Ultra 392611981 GC MS septa 392611982 5 mL Vials i 5 mL 20 mm x 38 mm solvent vials and CP 8410 pelea sample vials w snap cap and septa 392611974 10 mL Ultra GC MS vials 22 mm x 45 mm sample 392612006 50 pk 40 mL Vials vials for CP 8410 w
53. eees 73 FIGURE 18 EFC23 FLOW DIAGRAM sociated Siete A E e ued item abies 15 FIGURE 192 EEC24 FLOW DIAGRAM cuasan a eesti d etd me eet 76 FIGURE 207 FID EXPLODED VIEW sist sitesi ates E A A E E leneece nea 80 FIGURE ZIZFID TOPVIEW corie A A E E ne eae 83 FIGURE 22 TCD SENSITIVITY AND AMPLIFICATION ruri oinin naa A 90 Tables TABLE 1 GENERAL TIGHTENING AND RETIGHTENING FOR COMMON FERRULEG 18 TABLE 2 MAINTENANCE SCHEDULE icc icatcots bacteriuria tnt taeda bieteatinse tel hi E 43 TABLE 3 SPLIT INJECTION TYPICAL CONDITIONS srinaranata 63 TABLE 4 SPLITLESS INJECTION METHOD PARAMETERS ccccccccseececeeeeseeeeeseeeeeeees 64 TABLE S V77 COLUMN FERRULE S T160 erpai sot eee seer A a banc anaes 65 TABLE 6 1041 COLUMN FERRULES 1 16 X 0 8 MM aannnannnnannnnnnnnnnnnnnnnnnnnnnnnennnnnnnsnnnnennnnnne 73 TABLE 7 CARRIER GAS FLOW RATES FOR 104 4teeiccc dcccciicecehetacitees liwiaesdchoinel l nedaseeteeneesdiiia 7 TABLE S 1041 TEST COMPOUNDS iiciin ahs E when asa oats ethane N cece 7 Varian Inc User Manual 430 GC and 431 GC Page 5 Introduction ABOUT YOUR 431 GC The 431 GC is sold with Varian Mass Spectrometers and is controlled through the MS Workstation Since the 431 GC is part of an integrated GC MS the Local User Interface LUI and keyboard are not required The information in the manual regarding the 430 GC also applies to the 431 GC with the exception of the sections describing the LUI or keypad ABOUT YOUR 430
54. er remove the Injector access plate by removing the two retaining screws and firmly lifting the plate It may be hot if another injector is also installed and powered The plate may be a little tight do not force it off Lift straight up a slight back and forth rocking may help remove it 4 Use a laboratory tissue to grasp the glass y insert and remove it from the injector body l Replace the Glass Insert Follow these steps to replace the glass insert in the 1177 Injector 1 Using tweezers or clean lab tissue carefully slide the new insert into the injector body Place a new seal over the insert 2 Carefully place the top of the injector over the insert Tighten the two captive screws alternately for uniform sealing Note that placing the top piece onto the body may take some care since the gas supply line and septum purge lines may have minor resistance to movement 3 Install a new septa place the injector nut on the injector and tighten by hand until you feel some resistance then tighten an extra 1 4 turn using the injector nut wrench After the injector nut has been replaced check the split vent and septum purge flow rates to ensure these values have not changed Varian Inc User Manual 430 GC and 431 GC Page 67 Injectors 1177 Split Splitless Capillary Injector 4 Condition the insert by setting the 1177 Injector to the split mode and purging with carrier gas for 30 min at 300 C Injector body cleani
55. essssssssscceessoooess 101 Page 4 User Manual 430 GC and 431 GC Varian Inc Table of Contents Figures FIGURE 1 AUTOSAMPLER CP 8400 8410 ON THE 430 GC SCREW LOCATIONS 11 FIGURE 2 430 GC REAR PANEL SHOWING CP 8400 8410 CABLING cece ee eeees 12 FIGURE 3 430 GC REAR PANEL CONNECTIONS ccc ccccceccccceeceeseeeceeeeetaeeeeseeeeesaeeesaeees 13 FIGURE 4 CONNECTOR J2 SYNC ANALOG OUT 0 0 0 ccccceccccceccecceeeeeeeeeaeeeesaeeeesaeeeesaeeesaeees 14 FIGURE 5 CONNECTOR J22 EXTERNAL EVENTS 1 00 0 ccccceccceeceeceeeeeeeeesaeeeeseeeeeseeeeseeeenas 15 FIGURE 6 COLUMN INSERTION DEPTHS cc ceccccceccceeeeecee cesses eeeseesesseeeeseeeeseeeeseeeeeas 16 POYRE Z COCUMN Sorea a E A 17 FIGURE 8 PROPER FERRULE ORIENTATION riain ea tant aaa ia 19 FIGURE 9 430 GC DIRECT CONNECTED TO THE WORKSTATION cccccecceeeeeeeeeees 20 FIGURE 102 ISOLATED NETWORK crre earo a ee eases 21 FIGURE Te COMPANY NETWORK erna E a NE 22 FIGURE 12 TABLE OPERATIONS WITH LOCAL USER INTERFACE cccccceeeeeeeeees 32 FIGURE 13 EFC21 AND 1177 IN SPLIT MODE FLOW DIAGRAM cccccccccceeeeeeeeeeeeeees 56 FIGURE 14 EFC21 AND 1177 IN SPLITLESS MODE FLOW DIAGRAM cccccceeeeeeeees 57 FIGURE 15 EFC25 FLOW DIAGRAM o2 lt wee sedans ae a oe ee 58 FIGURE 16 1177 INJECTOR ASSEMBLY ya ie A S 65 FIGURE 17 1041 UNIVERSAL INJECTOR WITH INSERT ccccccecccceeceseeeeeeaeeeeseeeeeee
56. essure 0 1 to 100 0 psi Default 10 0 Pressure Pulse Duration 0 01 to 10 00 min Default 0 25 Initial Split Ratio On Off Split ratio 1 to 10 000 Time On Off Split ratio 1 to 10 000 Time On Off Split ratio 1 to 10 000 Time On Off Split ratio 1 to 10 000 Time On Off Split ratio 1 to 10 000 You may add lines to the Injector Split Ratio program by pressing the i key You may delete a line by scrolling so that the desired line is displayed and then pressing the E gt key Varian Inc User Manual 430 GC and 431 GC Page 37 Keyboard and Display THE q INJECTOR KEY This key will give access to the Injector and Pressure Flow settings of the 1041 Injector Injector Outline Injector Oven Injector Temp Mode Pressure Hold Time Total Flow Pressure 0 1 to 100 0 0 1 to 100 0 0 1 to 100 0 Pressure 0 1 to 100 0 Pressure 0 1 to 100 0 Event Time 0 00 to 999 99 Event Time 0 00 to 999 99 0 00 to 999 99 Event Time 0 00 to 999 99 Event Time 0 00 to 999 99 Pressure Pressure Event Time On Off 50 to 450 C lsobaric Constant Flow 0 1 to 100 0 psi 0 00 to 999 99 0 1 to 100 00 Ramp rate 0 1 to 400 0 Ramp rate 0 1 to 400 0 Ramp rate 0 1 to 400 0 Ramp rate 0 1 to 400 0 Ramp rate 0 1 to 400 0 Total Flow 0 1 to 100 0 Total Flow 0 1 to 100 0 Total Flow 0 1 to 100 0 Total Flow 0 1 to 100 0 Total Flow 0 1 to 100 0 Default Isobaric Default 10 0 Default
57. et address can not be changed and is the permanent way of identifying a particular hardware device The Ethernet address consists of 4 pairs of hexadecimal numbers Gateway This is one of several settings within the TCP IP configuration that identifies paths that are used to establish connections with Ethernet devices The Gateway is assigned an IP Address Host Name The host name is an alternate way of identifying a device that is friendlier to people Frequently the host name and the IP Address may be used interchangeably although both must be specified in the BOOTP server Hub A device that allows many Ethernet devices to be interconnected Several hubs may be interconnected depending on the manufacturer to increase the number of Ethernet connections IP Address This is a unique number for each Ethernet device within the set of connected devices Two PCs may have identical IP Addresses so long as they are not interconnected to each other either through a hub or through the internet The IP Address consists of a series of four sets of decimal digits between 1 and 3 characters typically which encodes gateway and routing information that is used by the TCP IP protocol to establish the most efficient and reliable connection Without the IP Address communications would be bogged down trying to establish connections to just the Ethernet address Varian Inc User Manual 430 GC and 431 GC Page 23 Installation Patch Cable A cable that is
58. g the column A Do not heat the column oven above 50 C without carrier gas flowing through the column The column phase can be irreversibly damaged CAUTION EFC Pneumatics Type EFC21 or EFC25 used with the 1177 injector allows the user to seta constant column head pressure build a pressure program or set a constant column flow In addition a split ratio can be set or time programmed A pressure program is typically used to maintain the column flow at a constant value while temperature programming the column oven When Constant Flow Programming is enabled the pressure program needed to maintain constant flow is derived whenever the method is activated 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 CONFIGURATION SETUP oC key on the 430 GC keyboard The Type EFC21 status field displays the actual column pressure in the units chosen in Setup calculated column flow rate calculated column linear velocity and the split ratio The split ratio status is either off if the split state is set to OFF or a whole number The lower part allows you to view edit constant flow mode Page 60 User Manual 430 GC and 431 GC Varian Inc 1177 Split Splitless Capillary Injector Injectors Septum Purge Calibration The 430 GC is equipped with a septum purge for the Model 1177 split splitles
59. he column firmly in place and obtain a good seal Remove the syringe from the injector After the column is installed at the injector end make several dry injections to ensure that the needle enters the column easily User Manual 430 GC and 431 GC Varian Inc 1041 On Column Injector Injectors 1041 Electronic Flow Control The Electronic Flow Control module used on a 1041 injector can be type EFC23 or EFC24 The EFC23 is used to control the 1041 Injector under flow control to program the column flow EFC23 sets a required carrier flow into the Injector Column system A leak in the system would be indicated to the user by a drop in inlet pressure The EFC24 is used to control the 1041 Injector in combination with Gas or a Liquid sampling valve Both EFC types are designed specifically for the 1041 injector to support its various modes of operation In simple terms it duplicates the behavior of the 1041 manual pneumatics system in that there is an inlet mass flow controller supplying carrier gas to the injector and a pressure control valve downstream from the injector which sets the injector pressure As injector pressure determines the rate of carrier gas flow through the column this pressure is monitored close to the point of injection The type EFC23 flow diagram shown below is an indication of the control mechanism of this type of EFC module as lI Digital Flow Control z Carrier Gas inlet
60. highest possible sensitivity operate the TCD at the 0 05 mV range with a high filament current In this configuration TCD noise is primarily noise derived from filament vibration and fluctuations in carrier gas flow through the detector However at high filament currents the detector is very susceptible to air leaks into the gas lines improperly conditioned columns imbalanced reference and analytical flow rates or impure carrier gas supply which cause the baseline to drift Baseline drift from any of these sources generally increases as the absolute filament temperature increases Therefore operate the TCD with as low a filament current as practical for your application Also operate the TCD with the lowest filament and detector temperatures appropriate If possible avoid operating the TCD with a filament temperature greater than 390 C To operate the TCD with filament temperatures between 390 C and 490 C set the Filament Temperature Limit to 490 C See Figure 22 on page 90 for an example of the performance of the TCD ata high current Calculate Detector Sensitivity To calculate the sensitivity of the TCD proceed as follows EXAMPLE 1 Known Sample Weight S PF W Where S Sensitivity in mV x mL mg P Integrated peak area in mV x min W Weight of sample in carrier gas in mg Fo Carrier gas flow in mL min corrected to detector temp Fo Fo Tp Ta 1 Pw Pa Where Fo Flow rate measured at detector outlet at ambie
61. ications J12 SERVICE Not in use J2 External Events Timed relay contacts see on page 15 F1 Fuse User accessible fuse 24 volt supply AC Power Input Standard power cable Installation C3 WARNING HOT AIR E Kpop Meee WARNUNG Heilufiuagqeng Haly lemperatinemphmedlicha Ofiruang fern ATTENTION Sorte dalr chaud Eloig ATTENZIONE Usaia Avia Galda hon aWiciare comport sensibili alla empiatur iPRECAUCION pares cenubles al calor ACHTUNG Blockheren Sy es nicht Lefieinlafizur ATTENTION Ne pas obstruer Prise d air pour le Re ATTENZIONE Non Gstruire i passaggio Presa d ana jPRECAUCION Mo cubrir Toma de aire pararefrigeraci Ea PAM AAAI aie tot gt WATENE CAUTION Instrument cooling air intake Figure 3 430 GC Rear Panel Connections Varian Inc User Manual 430 GC and 431 GC Page 13 Installation Connector J2 Sync Analog Out Connection between the 430 GC and External devices Synchronization Analog signals Connector J2 430 GC Sync Analog Out Ready In 2 GND 1 J2 11 SYNC Integrator ID ANALOG OUT 3 9 Start Out 1 Volt default 7 See Analog Out 10 Volt lt 15 Selectable by Jumper gt GND 2 on Main Board Figure 4 Connector J2 Sync Analog Out If an integrator or other device is connected pin 2 and 11 must be connected in order to inform the 430
62. in the capillary mode the following carrier gas flow rates are recommended Carrier Gas Column Flow Rate Column Flow Rate Optimum Typical Nitrogen 1 5 mL min 3 15 mL min 2 4 4 0 mL min RAS Alin Hydrogen 4 0 8 0 mL min 8 20 mL min Table 7 carrier Gas Flow Rates for 1041 Adjust the make up gas flow to give a total of 30 mL min When operating in the packed column mode adjust the carrier gas flow to applicable packed column flow rates 20 to 50 mL min Testing the 1041 Injector The most effective method of testing injector performance is by running a test sample The following procedure describes how to test the performance of the 1041 on column 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 Varian GC detectors Test Sample Part Number Concentrations of Test Compounds TCD 82 005048 01 3 00 ug uL of C14 C15 and Cig in iso octane FID 82 005048 07 30 ng uL of C14 C15 and Cig in iso octane Note if the FID test sample is not available the TCD test sample can be used if first diluted 100 1 Table 8 1041 Test Compounds To run the test sample use the default method for one of the methods in the 430 GC These conditions will give you optimum sensitivity and precision Varian Inc User Manual 430 GC and 431 GC Page 77 Detectors Flame lonization Detector FID DETE
63. ing from one 1177 mode to another involves changing the glass insert A detailed stepwise procedure to carry out this task is given in the Maintenance section of this manual on page 66 In most injection modes the insert is installed with an o ring Split Injection The split mode is used when samples are relatively concentrated and for neat samples This mode of injection involves rapid vaporization of the sample followed by sample splitting Splitting involves directing a portion of the sample into the column while the remainder is vented The split ratio is defined as the proportion of sample vented to the sample entering the column With EFC carrier gas control this parameter can be set automatically in the 1177 method Injector Insert 4 mm ID open insert packed with glass wool Column Installation 3 7 cm from the bottom of the column nut at the base of the injector Injector Temperature Isothermal 250 C Column Temperature 50 C initial for 0 1 min ramp to 250 C at 20 C min hold 5 min Carrier Gas Control Set the split mode to ON for the duration of the run in the 1177 method section and set the split ratio to 100 The sample is split upon injection and a representative portion representing 1 100 of the amount injected enters the column 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
64. inject to correct this Page 94 User Manual 430 GC and 431 GC Varian Inc Errors ADC CALIB FAILURE Fatal The DAC Digital to Analog Converter that supplies the analog output signal failed to calibrate within its set tolerance Turn off the power and then turn it back on If the problem is observed again either immediately or within a short period of time call your Varian Service Representative COL RESPNSE TOO FAST Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative COL RESPNSE TOO SLOW Fatal Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative COL TEMP PROBE OPEN Fatal Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative COL TEMP PROBE SHORT Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative COL TEMP TOO LOW Fatal Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative COL THERMAL RUNAWAY Fatal Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative DAC CALIB FAILURE Activate a method to clear this Error If the Error recurs turn the GC off and then on If the Error persists call your Varian Service Representative DET RESPNSE TOO FAST Fatal Turn off instrument and turn it back on If the Error recurs call your Varian Servic
65. is used in a manner not specified by the manufacturer the protection provided by the equipment may be impaired It is the responsibility of the Customer to inform Varian Customer Support Representatives if the instrument has been WARNING used for the analysis of hazardous biological radioactive or toxic samples prior to any instrument service being performed or when an instrument is being returned to the Service Center for repair Page VI User Manual 430 GC and 431 GC Varian Inc Safety Information ELECTRICAL HAZARDS Disconnect the instrument from all power sources before removing protective panels to avoid exposure to potentially dangerous voltages When it is necessary to use a non original power cord plug make sure the replacement cord adheres to the color coding and polarity described in the manual and all local building safety codes Replace blown fuses with fuses of the size and rating stipulated on the fuse panel or in the manual Make sure that voltage sources and line voltage match the value for which the instrument is wired Replace faulty or frayed power cords immediately with the same type and rating COMPRESSED GAS CYLINDERS Varian Inc Store and handle compressed gases carefully and in strict adherence to safety codes Secure cylinders to an immovable structure or wall Store and move cylinders in an upright vertical position Before transport remove regulators and install cylinder cap
66. l Injector with Insert Teflon 40 Graphite Column ID 60 Vespel Max 250 C Max 350 C Max 400 C 1 Injector Nut 390812700 Injector Nur Wrench 390842300 Automatic Start Switch 390820601 BTO lowest bleed CR298705 Marathon Autosampler CR239188 Advanced Green 3 general purpose CR246124 Septum pick 7200008400 EFC23 type 392548201 Injector Body Ferrule 40 Graphite 60 Vespel up to 400 C CR213400 Graphite up to 450 C CR211400 Injector Body Nut Stainless Steel SWSS4021 Injector Insert Stainless Steel 392543101 Column Ferrule see table below Capillary Nut 394955100 Graphite silTite Max 450 C Metal GC MS 0 53 mm ID CR214108 CR212108 CR213108 Table 6 1041 Column Ferrules 1 16 x 0 8 mm Replacement parts on page 101 or click here Varian Inc User Manual 430 GC and 431 GC CR211108 SG073302 Page 73 Injectors 1041 On Column Injector Column Installation The following instructions apply to installing a 0 53 mm ID capillary column in the 1041 injector Fused silica columns are somewhat fragile and must be handled with care During operation the 0 53 mm ID capillary column hangs on the capillary column holder in the column oven To prevent the column from unwinding weave both of the column ends through and around the column loop several times This is particularly useful if your column is not mounted in a cage Hang the coiled column on the capillary column holder or
67. led areas have returned to room temperature or wear adequate hand protection before you touch potentially hot or cold surfaces Page VIII User Manual 430 GC and 431 GC Varian Inc SPARE PARTS AVAILABILITY It is the policy of Varian to provide operational spare parts for any instrument and major accessory for a period of five 5 years after shipment of the final production run of that instrument Spare parts will be available after this five 5 year period but on an as available basis Operational spare parts are defined as those individual electrical or mechanical parts that are susceptible to failure during their normal operation Examples include relays lamps temperature probes detector elements motors etc Sheet metal parts structural members or assemblies and castings printed circuit boards and functional modules are normally capable of being rebuilt to like new condition throughout their useful life and therefore will be supplied only on an as available basis after the final production run of the instrument Varian Analytical Instruments Sales Offices For Sales or Service assistance and to order Parts and S Safety Information SERVICE AVAILABILITY Varian provides a variety of services to support its customers after warranty expiration Repair service can be provided by attractively priced service contracts or on a time and material basis Technical support and training can be provided by qualified personnel on both a
68. les to connect the GCs and the Workstation PCs to the Ethernet hub or switch If you want to connect your 430 GC to the same Workstation as your other Varian GC you will need a hub We refer to this type of special purpose network as an isolated network one that does not have IP Addresses provided by the Network Administrator Workstation Ethernet Patch Cables p n 03 926129 01 or 02 Ethernet 430 GC hub or switch 430 GC Other Varian GC Workstation Figure 10 Isolated Network User Manual 430 GC and 431 GC Page 21 Installation You may also connect your Workstations and 430 GC to a company Ethernet network used for purposes other than instrument control such as Internet access or file server access We refer to this type of multi purpose network as a company network and it will typically be managed by a Network Administrator in your company If this is the case then some of the settings needed to configure your 430 GC and Workstation PC will need to be provided by your Network Administrator If you are connecting your 430 GC and Workstation to a company network your Network Administrator should be made aware that the 430 GC requires a BOOTP Server for IP Address assignment Ethernet Patch Cables p n 03 926129 01 or 02 Star 800 Box Other Varian GC Ethernet hub or switch BEEBE gut shay os 6 Other Varian GC Workstation er z 6 Uplink connection to aah en cilia
69. librium always exceeds the time it takes for the detector oven to reach its temperature When the baseline is stable you can begin your analysis Autozero is automatically disabled when the GC method is in RUN Change Initial Autozero back to YES This allows the system to balance the bridge automatically before each run for maximum dynamic range The current status of the balance control from 99 to 99 is shown on the display A continuous drift in the balance value over time may indicate you have an air leak which is causing one set of filaments to oxidize changing their resistance and unbalancing the detector bridge Range Setting Use the 0 05 mV range in the following cases e Low currents 100 150 mA e High Currents 300 mA e Output Signal Fed to Computer or Integrator Varian Inc User Manual 430 GC and 431 GC Page 89 Detectors Thermal Conductivity Detector TCD Low Currents 100 150 mA Analyses that had required a high filament current and a less sensitive range can often be performed at lower currents and a more sensitive range For example a filament current of 120 mA and a range of 0 05 mV yields about the same output signal as a filament current of 300 mA and a range of 0 5 mV At the lower current the detector noise is lower the stability is higher and the filament lifetime is extended Thus Varian recommends that whenever possible you operate the TCD at the lowest practical filament current The chrom
70. lit flow controller Adjust the Back Pressure Regulator on the GC pneumatics panel to establish a positive column head pressure monitored on the pressure gauge Set the column head pressure based on the column installed in the GC For example for a 30m x 250 um ID column set the column head pressure to 12 15 Psig to achieve 1 mL min column flow rate at 50 C oven temperature helium Connect the flowmeter to the split vent on the left side of the GC and measure the split vent flow rate Turn the Split Flow Controller valve to adjust the split vent flow rate to 50 mL min Adjust the Septum Purge Needle valve to adjust the septum purge flow rate to 3 5 mL min Readjust the split vent flow rate to 50 mL min Before heating the column purge the system with carrier gas for 10 15 minutes User Manual 430 GC and 431 GC Varian Inc 1177 Split Splitless Capillary Injector Injectors 1177 Modes of Operation The 1177 can be operated in several modes depending on the nature of the sample and requirements of the analysis When designing an injection method the most important parameters are e the injector insert used e the injector and column temperature when the injection is made e the carrier gas flow profile through the injector The following is a brief description of the method parameters used for each injection mode In all cases Electronic Flow Control EFC is used for carrier gas control In many cases switch
71. n glass injector RT207732145 5 pk inserts 4 mm ID wool plug single gooseneck glass injector inserts Ko 392611936 5 pk 4 mm ID unpacked single gooseneck glass injector inserts 392611927 5 pk 4 mm ID wool plug open glass injector inserts 392611937 5 pk 4 mm ID unpacked open glass injector inserts 392611925 5 pk __ 2mm ID wool plug open glass injector inserts 392611938 5 pk m 2 mm ID unpacked open glass injector inserts 392611924 5 pk E SPME insert 0 75 mm ID for SPME fiber injections 392611998 5 pk Septa 9 0 mm Advanced Green 3 Centerguide septa CR246713 50 pk Viton O ring standard injector insert seals 8850103100 25 pk Insert Seals Varian Inc User Manual 430 GC and 431 GC Page 103 Replacement Parts Page 104 User Manual 430 GC and 431 GC Varian Inc
72. nc User Manual 430 GC and 431 GC Page 65 Injectors 1177 Split Splitless Capillary Injector Page 66 Maintenance Before maintaining the 1177 injector please read the common Injector septum maintenance information in the section Maintenance on page 46 The 1177 is a Split Splitless capillary injector Typically to change from Split operation to Splitless involves changing the injector insert Also replace the insert on routine base This is especially important when dirty samples are analyzed Tools Required Tweezers or septum pick P N 72 000084 00 Injector nut wrench P N 03 908423 00 Flat blade screwdriver long handle Clean laboratory tissue The injector nut may be hot Lower the injector WARNING temperature to 50 C and permit the injector nut to BURN HAZARD cool before proceeding Remove the Glass Insert 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 User Manual 430 GC and 431 GC Varian Inc 1177 Split Splitless Capillary Injector Injectors 3 Unscrew the two captive screws holding the top of the injector to the base Carefully move this assembly to one side The Septum purge line and carrier gas supply lines may hinder movement of the top piece somewhat When using a CP 8400 AutoSampl
73. ng To clean the injector body proceed as follows 1 Set the column oven temperature to 45 C and the 1177 injector temperature to 50 C Wait for the zones to reach their set temperatures and then turn the column oven off by hl the TURN OVEN OFF button located in the Column Oven section 2 Use the 5 16 open end wrench to loosen the capillary column nut 3 By hand carefully withdraw the fused silica column and nut from the injector assembly Set the column nut and column end on the floor of the GC oven WARNING CHEMICAL 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 4 Remove the injector nut septum and top of injector 5 Moisten a cotton swab and a stick with methanol and gently swab center of the injector body 6 Moisten a cotton swab on a stick with iso octane and gently swab the center of the injector body 7 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 8 Gently twist the column nut in the opposite direction used to tighten the nut Place the column nut on the end of the injector and tighten the nut This procedure minimizes twisting the column Page 68 User Manual 430 GC and 431 GC Varian Inc 1177 Split Splitless Capillary Injector I
74. njectors 9 Use the 5 16 open end wrench and tighten with 1 6 turn to secure the column in place 10 Replace the insert seal injector top septum and injector nut 11 To check whether the injector is leak tight connect a flow meter to the split vent 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 pressing the TURN OVEN ON button in the column oven section Varian Inc User Manual 430 GC and 431 GC Page 69 Injectors 1177 Split Splitless Capillary Injector Page 70 User Manual 430 GC and 431 GC Varian Inc 1041 On Column Injector Injectors THE 1041 ON COLUMN INJECTOR Designed for On Column sample injection onto 530 micron D fused silica columns 1 4 inch and 1 8 inch O D packed columns glass or metal On Column injection provides complete sample transfer from injector to column results in good quantitation The fused silica column or glass column extends all the way from the injector septum to the ionization detector providing a clean inert system without cross overs Quick and easy to switch from megabore to packed column or vise versa by changing an adaptor The 1041 is supplied with capillary mounting hardware as standard If you wish to operate the injector in the packed column mode then a packed column adapter kit must be ordered 03 925588 91 This kit contains injector and detector h
75. nsive supply of quality maintenance parts for your 430 GC and all of your chromatography needs including a comprehensive selection of the highest quality capillary columns available to chromatographers Please visit the Varian internet site www varianinc com contact your Varian sales representative or call your local Varian distribution center PREPARING FOR INSTALLATION A Refer to the Pre Installation Instructions CP501405 for site preparation and unpacking information CAUTION The instrument has been protected during shipment by various caps plugs and restraints Prior to operating Remove the tape restraining the column oven door Remove any plastic plugs or caps inside the column oven and of FID Cut the tie wrap and remove the shipping dowel for oven fan motor from the hole in the GC left side panel Remove the carrier gas fitting cap on the rear panel Install the septum purge cover by snapping it onto the GC above the oven door Page 10 User Manual 430 GC and 431 GC Varian Inc Installation INSTALLING THE CP 8400 8410 AUTOSAMPLER To install your CP 8400 8410 on a 430 GC first unpack the AutoSampler and verify that all of the parts required are present Contact your Varian representative immediately if you find that any parts are damaged or missing Mounting the CP 8400 8410 onto the 430 GC The CP 8400 8410 has a single mounting position on the 430 GC top cover There are two metal guiding
76. nt Changing a value will not immediately result in a change of the parameter being edited Only after pushing the ENTER key the value will be accepted The keys status and g UP LINE only serve to change the display If you wish to exit a field that you have edited without accepting the edit press the keys and t to escape from that field gt The keys START 0 or ENTER Er NEW LINE and DELETE LINE indicate an action will occur when that key is pressed gt el are two examples of action keys For instance if you press J the 430 GC will immediately begin a run in automatic manual injections you will be prompted for the vial and method before the injection occurs All selections from the keypad are made via scrolling using the T UP and 4 DOWN keys immediately to the right of the display it is not possible to enter an illegal value To accept the value press immediately You may press either or EG to scroll between parameters Varian Inc User Manual 430 GC and 431 GC Page 7 Introduction The display is designed to show you both data and navigational information This is presented to you in two ways 1 An LED will illuminate showing you which section you are working in and displaying 2 The display will provide you direct information on where in a section you are as well as the parameter In the following example the A S indicates you are working on the Aut
77. nt temperature in mL min Tp Detector temperature in K Ta Ambient temperature in K Pw Partial pressure of H20 at ambient temperature in torr Pa Ambient pressure in torr Note The 1 Pyw P expression applies only if using a bubble flowmeter Varian Inc User Manual 430 GC and 431 GC Page 91 Detectors Thermal Conductivity Detector TCD Page 92 EXAMPLE 2 Known Concentration of Sample in Detector S E Cp Where S Sensitivity in mV x mL mg E Detector signal peak height in mV Cp Concentration of test substance in the measured peak volume in mg mL Peak volume Peak width at half height in min x gas flow rate at detector in mL min W e h 2 x FC Calculate Detector Detectivity To calculate the detectivity of the TCD proceed as follows 7 2 x Noise Detectivity Sensitivity Reverse Polarity If you inject a standard or sample into the reference side of the TCD peaks appear in the negative direction If you want to integrate or process these peaks with a data system you must convert the polarity of the peaks from negative to positive Reference the TCD section to set initial detector polarity either Positive or Negative You can also time program when you would like the polarity to be automatically reversed during a chromatographic run Set a time programmed polarity reversal in the detector method section Adjust TCD Carrier Gas Flow Rates All 430 GCs equipped with TCDs are factory tested
78. ntry Page 32 User Manual 430 GC and 431 GC Varian Inc Display and Keyboard THE x SETUP KEY The parameters available from the key are summarized in the Setup Outline below if NO CP 8400 or CP 8410 is installed you will not see the AutoSampler Setup section Language EFC type 1 for 1177 Injector EFC type 4 for 1041 injector Varian Inc English French Spanish Italian German Japanese Katakana Gas Type He No H2 Outlet Atm Vacuum Units psi kPa Barr Gas Saver Timeout 0 off to 999 99 min If the GC is idle for the set period of time the Gas Saver flow rate is implemented and an advisory Error is created Activate a Method to clear the Error Gas Saver Flowrate O to 100 mL min Splitless Vent Flow O to 100 mL min Septum Purge Calibrate Gas Type He N2 H2 Outlet Atm Vacuum Units psi kPa Barr Gas Saver Timeout 0 off to 999 99 min If the GC is idle for the set period of time the Gas Saver flow rate is implemented and an advisory Error is spawned Activate a Method to clear the Error Gas Saver Flowrate O to 100 mL min Splitless Vent Flow O to 100 mL min User Manual 430 GC and 431 GC Page 33 Keyboard and Display Column Temperature Limits AutoSampler Date Time Password Page 34 Length I D Standby Temperature Standby Time out 0 01 to 200 00m 20 to 530 um packed 50 to 450 C 0 00 off to 999 99 min Column Temperature zone upper limi
79. oSampler method section the 2 represents the current line number and the 31 indicates the total number of lines in the A S User Defined section The rest of the display is composed of the parameter and its current setting An LED next to the A S method section will be illuminated to further affirm that you are working in the A S method section A S 2 3l SAMPLE PENETRTN DEPTH 1007 While not all displays will show current line out of a total number of lines they all follow the principle of informing you with a LED that indicates which key was selected The information above represents all of the fundamental interactions with the keypad If you are controlling your 430 GC from a WorkStation you will need to establish Ethernet communications with the GC as described in this manual on page 20 and use your Workstation according to its instructions Page 8 User Manual 430 GC and 431 GC Varian Inc Introduction Varian Inc User Manual 430 GC and 431 GC Page 9 Installation INSTALLATION NOTES ABOUT SETTING UP AND USING YOUR 430 GC The purity of the gases used with your 430 GC are essential for optimum operation A Varian Gas Clean Filter Kit CP736530 must be installed All GCs require regular maintenance in order to operate at their highest efficiency You will want to change the injector septum injector liner FID flame tip gas filters and AutoSampler vials wash bottle septa and solvents regularly Varian has an exte
80. of Contents VARIAN ANALYTICAL INSTRUMENT WARRANT Y ccccscccssccccsccccsccccccccccsccccsccccecsces Ill HAROMA I Sil el OUO Bi em eee aeRO eee ee Ul OPT WARE PRODUCTS aise a aia a ci N cals ed oes ea II KEN DE a a ae EN at te Ul LIMITATION OF VW ARRAN TY oe teinetalel eit vaceratavetin A oe he ea el Ul LIMITATION OF REMEDIES AND LIABILITY ctecscaschestensda suc A E II L neeoosesesesososseecsseessscessscessseessseessseessseessscessseessscessseessscessseessseessseessseessseessse IV ROI a FA U A en EREE EER RENE E EE Ro EE IE EOI EAEE A Ce Re E E IV OPERATING ENS TRUCTIONS i a a a sae vente a aa EAA IV GENERAL SAFETY PRECAUTIONS aa e aaa r aA a aa ia a ae aidaa VI IGE BAR AON o VAN ID ET E EEE I A EEE A BEA E EA A ET E EEA VII COMPRESSED GAS CYLINDER S iectcass ca esen erie ien a sede a ra e i arera iria Enan Enia VII GC SABE TY PRACTIC S ER A a uae aaa A ede ea et a VII E OUST ST OEE E T a a a E A a eget ete VIII Radi achye source TICLE CL ONS ueuemace inanan aan a aa a a aan a VIII BOTAL a a a a nen Cae VIII SPARE PARIS AVAMA BIEN Y naea a a a A E a N aa IX SPERVICRAVANARIEI T Y aeie R A E A A ET IX ABOUT YOURI GCO ioaea e a nae ae o aa eaa O aaea aa a SEOC 6 ABOUTI OUR II GO aiaia o i aod E ai 6 KEYPAD areia A E E a O EAE EET f O EEO 10 NOTES ABOUT SETTING UP AND USING YOUR 430 GC sisoseeesseensseensseersseerssecrsseersserrsseersseersseersserrsseee 10 PREPARING FOR INSTALLATION jiscssses des ianiisehs toca io e
81. ol E See pn se E RR eee column Split Vent CL v A Figure 14 EFC21 and 1177 in Splitless mode Flow Diagram See Pencil Filters on page 51 Varian Inc User Manual 430 GC and 431 GC Page 57 Injectors 1177 Split Splitless Capillary Injector The EFC25 is almost identical as the EFC21 the only exception is that the pressure is monitored at the module itself rather than at the Injector This allows the EFC25 to be used with Gas or Liquid Sample Valve s and Purge and Trap devices upstream from the Injector I l l L l l I Digital Flow Control Carrier Gas inlet Fencil Headspace p Flow sensor Be i k sampler or Filter other devices Molsiave Charcoal CP742210 silver color P Sensor i CP742211 gold color Digital Pressure Control Pressure aa a a a column Split Vent Figure 15 EFC25 Flow Diagram See Pencil Filters on page 51 Page 58 User Manual 430 GC and 431 GC Varian Inc 1177 Split Splitless Capillary Injector Injectors 1177 Manual Pneumatics The total flow into the system is adjusted using a 0 800 mL min manual flow controller The 1177 Injector uses a flow controller to supply the total flow into the system with a back pressure regulator to control the column head pressure When the injector is operated in the split mode the flow out the spilt vent relative to the flow through the column is defined as the split ratio In
82. pins in the bottom of the AutoSampler that fit into corresponding holes in the 430 GC top cover The CP 8400 8410 is attached to the top cover by securing two screws on the AutoSampler base underneath the sample tray and two more screws on a tab at the rear of the AutoSampler Figure 1 AutoSampler CP 8400 8410 on the 430 GC screw locations Varian Inc User Manual 430 GC and 431 GC Page 11 Installation Connecting AutoSampler Power and Communication Cables The CP 8400 8410 is connected with a three connector cable included with the Sampler to the 430 GC e The 25 pin D shell connector attaches to the S I D port J4 connector e The small white power connector to the A S POWER connector J7 e The 15 pin D shell connector is plugged into the back of the CP 8400 8410 It is important that the CP 8400 8410 is switched on prior to powering up the GC A flashing green LED at the rear of the AutoSampler is indicating that there is communication between 430 GC and the Sampler bi A Figure 2 430 GC Rear Panel Showing CP 8400 8410 Cabling Page 12 User Manual 430 GC and 431 GC Varian Inc 430 GC REAR PANEL CONNECTORS J2 SYNC Analog Out synchronization signal connector between the GC and External devices see on page 14 J4 S 1 D Serial port for CP 8400 8410 AutoSampler control J7 A S POWER Power Connector for CP 8400 8410 AutoSampler J10 COMM RJ45 connector for 10 base T cable for Ethernet commun
83. ports plugged pressurize the system to 80 psi Setting the isobaric pressure to 80 psi either at the 430 GC Keypad or via downloaded Workstation Method Shut off the carrier supply at the source and monitor the displayed pressure at the GC for five minutes The pressure should not drop more than 4 psi in five minutes Leak checking ensures that there are no leaks in the GC system up to and including the injector assembly If the indicated pressure on the GC drops by more than 4 psi during the five minute test period this indicates that there is a leak in the system Finding such a leak particularly if it is a small leak can be very difficult In general the best approach is to systematically go through the pneumatic system from the source and tighten each fitting until the leak is eliminated It is important to note that leaks are most often found in the carrier gas supply to the GC Varian Inc User Manual 430 GC and 431 GC Page 45 Maintenance Parts and Supplies Locate leaks with an electronic leak detector only An electronic helium leak detector is available from Varian www varianinic com 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 leak from a GC system Gas Filter Cartridge Replacement The 430 GC requires high grade pure gas for optimal performance Make sure you use gas filters for best operation If you are using the recommende
84. r inserts are deactivated for maximum inertness Page 54 User Manual 430 GC and 431 GC Varian Inc 1177 Split Splitless Capillary Injector Injectors 1177 Modes of Injection The 1177 injection mode is defined by the Split Vent program and by the choice of insert The Split Vent is controlled differently based on the pneumatics installed if EFC the split valve is controlled from the Injector section or if manual pneumatics the external events control the split valve The following are brief descriptions of the various modes of injection More detailed information on each mode is given later in this section Split Mode The split injection mode is preferred for the analysis of relatively concentrated samples The sample is split in the injector with a representative portion entering the column The split injection mode provides the shortest sampling time which leads to sharp chromatographic peaks Use the 4 0 mm open insert or the packed 4 0 mm ID insert when operating in the split mode In the split injection mode the sample volume is typically 2 uL or less Early eluting compounds usually appear as very sharp peaks In some cases the peak width is less than one second 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 CP 84
85. re in the GC operates through the detection of air or N2 in the detector cells the filament protection feature is disabled when you use nitrogen or argon as the carrier gas Set the Filament Temperature Limit to 390 C or 490 C according to the highest filament temperature setpoint required With the Limit set to 390 C the peak sample filament temperature is limited to approximately 450 C The temperature limit is approximately 550 C at the 490 C setting The 450 C limit protects filaments from oxidation when exposed to air over an extended period of time However at the 550 C temperature limit the filament can degrade after only a few minutes Varian Inc User Manual 430 GC and 431 GC Page 87 Detectors Thermal Conductivity Detector TCD If you select N2 Ar as the carrier gas the filament protection feature is filaments can rapidly oxidize if you operate the TCD filament temperature A disabled Because the GC does not turn off the filament current the TCD above 390 C without carrier gas flowing through the TCD cells If you plan to CAUTION operate the TCD after the carrier gas has been turned off purge the air from the TCD cells with carrier gas for five minutes before operating the TCD Operation To operate the TCD requires only carrier gas Helium or hydrogen is recommended as carrier gases You can use nitrogen as a carrier gas but you may lose some sensitivity and see an increase in the detec
86. re may be present Follow manual instructions for safe operation The potential for explosion may exist because of type of gas or liquid used lonizing radiation source is present Follow manual instructions for safe operation Keep hands and fingers away Varian Inc User Manual 430 GC and 431 GC Page V Safety Information GENERAL SAFETY PRECAUTIONS Follow these safety practices to ensure safe equipment operation Perform periodic leak checks on all supply lines and pneumatic plumbing Do not allow gas lines to become kinked or punctured Place lines away from foot traffic and extreme heat or cold Store organic solvents in fireproof vented and clearly labeled cabinets so they are easily identified as toxic and or flammable materials Do not accumulate waste solvents Dispose of such materials through a regulated disposal program and not through municipal sewage lines This instrument has been tested per applicable requirements of EMC Directive as required to carry the European Union CE Mark As such this equipment may be susceptible to radiation interference levels or frequencies which are not within the tested limits This instrument is designed for chromatographic analysis of appropriately prepared samples It must be operated using appropriate gases and or solvents and within specified maximum ranges for pressure flows and temperatures as CAUTION described in this manual If the equipment
87. rts on the TCD Once the carrier gas is flowing through the TCD set up the TCD for operation as follows 1 Set the TCD oven to the desired temperature and allow it to come to the setpoint Usually set the TCD temperature at least 20 C higher than the maximum temperature the column oven reaches in your analysis 2 Set TCD filament temperature in the detector section A filament temperature 50 C above the detector temperature should provide a good starting point for most applications Turn the TCD Electronics ON to begin heating the filaments 3 Allow system to equilibrate 10 to 15 minutes 4 Monitor the filament current through the detector status display Initially the current is greater than the final operating current Gradually however the current decreases as the detector thermally equilibrates For best performance of the detector do not permit the filament temperature to exceed the detector temperature by more than 200 C Generally use the lowest detector current possible for the sensitivity your application requires 5 Set the initial Autozero to OFF Set Autozero to NO then select the Command icon followed by Autozero Now Monitor the signal on the detector status display A continuous drift either positive or negative may indicate an air leak in either the carrier or reference gas stream 6 Note that it is normal for the TCD baseline to drift until the detector thermally equilibrates The time it takes to reach equi
88. ructions provided in the Accessory Kit 10 Leak check all fittings see page 44 11 Repeat this process as necessary for detector gases However use a secondary pressure of 60 psi for air and 40 psi for Ho SETUP INFORMATION Enter oC and enter essential parameters such as column diameter length and carrier gas ETHERNET COMMUNICATIONS Page 20 The 430 GC uses Ethernet as the means of external instrument control and to transfer digital data to a data system to which it is attached When running with Ethernet the 430 GC will have its IP Address assigned by either your company network or by a connected Workstation If you are using a workstation from another vendor that supports Varian GC products refer to that vendor s documentation to determine how it should be configured to work with Varian GCs 430 GC may be connected in three basic configurations If you have one 430 GC to connect directly to the Workstation PC and the Workstation PC is NOT connected to a company network then you may connect using the Ethernet crossover cable supplied with the 430 GC _ Workstation dc nananana 430 GC Ethernet Crossover Cable p n 03 933511 01 Figure 9 430 GC direct connected to the Workstation User Manual 430 GC and 431 GC Varian Inc Varian Inc Installation When connecting several 430 GCs to one or more Workstations you will need to use an Ethernet 10BaseT hub or switch and Ethernet Category 5 patch cab
89. s a negative pressure If the required pressure is less than 1 atmosphere the system will try to adjust the pressure to the calculated value Since the split vent and septum purge valve vent to the lab the vacuum pump will draw air through your column potentially ruining the column and damaging your MS detector if installed Important Tips Regarding 430 GC and 431 GC Operation After editing the active method it must be re activated before running the next analysis Always remember to activate a method after you have made edits if you intend to run that method next The 431 GC is sold with Varian Mass Spectrometers and is controlled through the MS Workstation Software Since the 431 GC is part of an integrated GC MS the Local User Interface LUI and keyboard are not required The 431 GC supports one active method at a time You may build and edit GC methods using the MS Workstation while the GC is running but you may not change the method that is currently running If you are using the 430 GC you may edit methods locally only when the GC is not in the RUN state executing a method The Status and Control screen for the 430 GC has an extend runtime key that will allow you to extend the runtime by 10 minutes each time you click on the key The extended run time will be used until the method is either re activated or a new method is activated The extend run feature does not change the method stored in your Workstation If a potentially ha
90. s expressly in lieu of and excludes all other express or implied warranties including but not limited to warranties of merchantability and of fitness for particular purpose use or application and all other obligations or liabilities on the part of Varian unless such other warranties obligations or liabilities are expressly agreed to in writing by Varian LIMITATION OF REMEDIES AND LIABILITY The remedies provided herein are the sole and exclusive remedies of the Customer In no case will Varian be liable for incidental or consequential damages loss of use loss of production or any other loss incurred Varian Inc User Manual 430 GC and 431 GC Page Ill Safety Information SAFETY INFORMATION INFORMATION To prevent any injury to the user or any damage to the instrument it is essential that you read the information in this chapter and the GC user manual s If this manual is not in your native language and if you have problems understanding the text we advise you to contact your Varian office for assistance Varian cannot accept responsibility for any damage or injury caused by misunderstanding of the information in this manual OPERATING INSTRUCTIONS This instruction manual is provided to help you establish operating conditions which will permit safe and efficient use of your equipment Special considerations and precautions are also described in the manual which appear in the form of NOTES CAUTIONS and WARNINGS as descri
91. s injector and is controlled by a manual needle valve This is located behind the front cover of the GC The manual needle valve can offer advantages over fixed restriction types as it can be adjusted to suit the more demanding applications For the accurate display of total column flow and velocity it does require calibration when columns of different length and diameter are installed Procedure 1 Download or activate the GC Method and note the pressure required to set the desired flow 2 Press Q and press until IEFC SETUP SEPTUM PURGE CALIBRATE Is displayed 3 Using the T or 4 key to change the entry to YES and press 4 EFC SEPTUM PURGE CALIB PRES Will be displayed and enter the pressure required using the T or 4 key and press 5 EFC MEASURE AND ENTER FLOWRATE will be displayed 6 Adjust the flow rate to approximately 5mls min typical values are from 2 10 mls min by turning the needle valve 7 Note the flow rate and enter this value using the 4 or T keys and press to accept 8 EFC SEPTUM PURGE CAL DONE PRESS ENTER is displayed 9 Septum Purge Calibration is complete Varian Inc User Manual 430 GC and 431 GC Page 61 Injectors 1177 Split Splitless Capillary Injector Manual Pneumatics Tools and equipment needed e Bubble or electronic flowmeter e g Digital Flowmeter 1 Page 62 Turn the 1177 Split Flow Controller on the GC pneumatics panel counterclockwise to open the sp
92. stomer shall be responsible for loss or damage in transit and shall prepay shipping cost Varian will return the accessory or instrument to the Customer prepaid and insured Claims for loss or damage in transit shall be filed by the Customer To correct software operation anomalies Varian will issue software revisions where such revisions exist and where in Varian s opinion this is the most efficient remedy LIMITATION OF WARRANTY This warranty does not cover software supplied by the Customer equipment and software warranted by another manufacturer or replacement of expendable items and those of limited life such as but not limited to Filters glassware instrument status lamps source lamps septa columns fuses chart paper and ink nebulizers flow cells pistons seals fittings valves burners sample tubes probe inserts print heads glass lined tubing pipe and tube fittings variable temperature dewars transfer lines flexible discs magnetic tape cassettes electron multipliers filaments vacuum gaskets seats and all parts exposed to samples and mobile phases This warranty shall be void in the event of accident abuse alteration misuse neglect breakage improper operation or maintenance unauthorized or improper modifications or tampering use in an unsuitable physical environment use with a marginal power supply or use with other inadequate facilities or utilities Reasonable care must be used to avoid hazards This warranty i
93. t 0 0 to 99 Default 5 0 to 5 or 10 or 100 Default 0 0 to 99 9 Default 5 0 1 to 25 or 50 Default 50 0 1 to 25 or 50 Default 0 0 to 99 9 Default 0 0 to 99 9 Default No Yes No Default 2 1 2 3 Default 1 0 to 4 9 or 0 to 9 0 Default 5 0 1 to 25 or 50 Default 0 0 to 9 9 Default Yes Yes No Default 1 1 2 3 Default O 0 to 5 or 10 Default 5 0 1 to 25 or 50 Default 0 0 to 9 9 Default No Yes No Varian Inc Display and Keyboard External Events Initial 1 On Off 2 On Off Default Off 0 01 999 99 1 On Off 2 On Off Default Off External Events are 24 Vac 200 mA max current 0 01 999 99 1 On Off 2 On Off Default Off You may add lines to the External Events program by pressing the Ey key You may delete a line by scrolling so that the desired line is displayed and then pressing the key If your 430 GC is equipped with a sampling valve you will use the external events to operate toggle the valve s position Note that the initial state of the valve will depend on whether the external event s initial state is energized on or de energized off THE q INJECTOR KEY This key will give access to the Injector and Pressure Flow settings 1177 Injector Injector Outline Injector Oven On Off Injector Temp 50 to 450 C Mode lsobaric Constant Default Isobaric Flow Pressure 0 1 to 100 0 psi Default 10 0 Pressure Pulse Yes No Default No Pressure Pulse Pr
94. t 50 to 450 C Detector Temperature zone upper limit 50 to 450 C Injector Temperature zone upper limit 50 to 450 C Calibrate Syringe Volume Date Time Set keypad Password Enter Password Vial 0 1 Injector 5 10 100 250 uL MM DD YY DD MM YY Locked Unlocked kkkkkkkk User Manual 430 GC and 431 GC Varian Inc Display and Keyboard THE 0 COMMAND KEY the D key gives you access to a variety of operations that are not properly associated with either method program execution or the GC configuration Method Actions Activate Method Methods 1 2 3 4 or 5 Copy Method Methods 1 2 3 4 5to1 2 3 4 5 Set Method to Defaults Methods 1 2 3 4 or 5 AutoSampler Actions Change Syringe Beeper On Off Move Tower Home Reset Plunger Stroke Counter Plunger Stroke Warning Limit Syringe Penetration Speed into Injector Syringe Depth into Injector Detector Actions AutoZero Now Clear AutoZero Ignite Flame Now FID only Remote Control Enable Disable a remote Workstation Varian Inc User Manual 430 GC and 431 GC Page 35 Keyboard and Display The following sections outline the parameters that are available under each method icon THE 000 AUTO KEY This key will give access to the AutoSampler and External Events Method section The following section lists the parameters for the CP 8400 AutoSampler and CP 8410 Autolnjector If no AutoSampler is connected the parameters will not be displayed
95. tectors TCD Adjustments Select Setup and set EFC Gas Type to the same type Setting the Filament Temperature Limit To protect the filament always operate the detector with the 390 C limit selected unless you require the maximum dynamic range available to the CAUTION With prolonged use the filaments slowly oxidize and their resistances increase At some point this will cause the largest peaks in your chromatogram to become flat topped indicating that the filament protection software has been activated Note that if the TCD signal is sufficiently large the output may go to zero and become unresponsive If this occurs adjust your injection site and conditions to avoid over range conditions To adjust for this increase in resistance set the Filament Temperature Limit to 490 C even for filament temperature set points below 390 C The TCD filament is automatically protected in the 430 GC The GC turns off the filament current after four minutes if it detects that the carrier gas flow has stopped or that the filament current is low Also the GC turns off filament current when it detects that carrier gas is flowing through one side of the detector cell but not through the other e g a septum or column is not installed or a leak exists in one cell and not the other If you select Helium or H2 as the carrier gas the GC operates in the standard way to protect the TCD filament However because the filament protection featu
96. teway 255 0 0 0 Domain 0 0 0 0 DNS Disabled WNS Configuration Disabled Your Ethernet card will need to have an IP Address assigned to it If your PC will not have any other Ethernet communications there are no problems with IP Address conflicts and you can set the IP Address to any value for example 10 128 70 10 Page 24 User Manual 430 GC and 431 GC Varian Inc Installation Connecting Cables Power down both your PC and 430 GC The optional Ethernet connection is made at the back of the 430 GC J10 on page 13 There are two types of cables crossover and patch which are used as shown in the figures in the introduction to this section If you will be connecting a single GC to a single Workstation PC you should use the crossover cable to make the direct connection Use the patch cable to connect the 430 GC to a hub or to your company network Varian Inc User Manual 430 GC and 431 GC Page 25 Installation CONNECTING POWER Plug the GC power cord into an appropriate power source Switch on the AutoSampler Switch on the 430 GC Power Switch located at the bottom left of the GC Confirm that the GC Power LED is on FACTORY DEFAULT STATES AND SETTINGS e When the GC is switched on first time all five methods will be set to default conditions appropriate for running the FID Test Mix e The column oven defaults to power ON and a set temperature of 80 C It will have a ramp that ends at 160 C
97. that you have free movement of the plunger Replace the syringe if required If the condition persists contact your Varian Service Representative Varian Inc User Manual 430 GC and 431 GC Page 93 Errors A S PLUNGER SENS ERR Fatal The AutoSampler plunger sensor has failed to conform to its expected operation Turn off the GC and then on again If the problem persists call your Varian Service Representative A S SYR SENSOR ERR Fatal The AutoSampler syringe sensor has failed to conform to its expected operation Turn off the GC and then on again If the problem persists call your Varian Service Representative A S SYR VOL EXCEEDED Soft The total volume of the sample air gaps if any solvent plugs if any and internal standards if any exceeds the capacity of the configured syringe Note that this error is only sensed at the time of injection Check your method and correct any volumes that are excessive A S SYRINGE MISSING Soft The AutoSampler has sensed that the syringe is not installed Check that you have a syringe installed If the condition persists contact your Varian Service Representative A S SYRINGE SLED ERR Soft The syringe sled is either jammed or miscalibrated Recalibrate your vial and injector positions making certain that the syringe sled has a small clearance consult your manual above vials and does not compress the injector switch on the injector If after adjusting the syringe sled height you still
98. the Customer and Varian any warranty shall be strictly in accordance with the terms of such agreement In the absence of a license agreement and unless an alternate warranty period is agreed upon in writing between Varian and the Customer the warranty period is as specified on the face of Varian s quotation Varian warrants such software products if used with and properly installed on Varian hardware or other hardware as specified by Varian to perform as 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 does not warrant uninterrupted or error free operation REMEDIES The sole and exclusive remedy under hardware warranty shall be repair of instrument malfunctions which in Varian s opinion are due or traceable to defects in original materials or workmanship or at Varian s option replacement of the respective defective parts provided that Varian may as an alternative elect to refund an equitable portion of the purchase price of the instrument or accessory Repair or replacement under warranty does not extend the original warranty period Repair or replacement under warranty claims shall be made in Varian s sole discretion either by sending a Customer Support Representative to the site or by authorizing the Customer to return the defective accessory or instrument to Varian or to send it to a designated service facility The Cu
99. the splitless mode gas does not flow through the split line from the injector to the 3 way solenoid Rather gas from the flow controller by passes the injector to pass through the 3 way solenoid valve The back pressure regulator uses this flow to control column head pressure which in turn controls carrier gas flow through the column Operation of the 1177 Injector The following section describes how to operate the 1177Split Splitless Capillary Injector with the Varian 430 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 the various modes of injection Column Installation The Column Installation on page 16 procedure describes the installation of a capillary column in a Varian 430 GC equipped with an 1177 injector Each step of the procedure is described in detail Condition the Column For conditioning the capillary column see information manufacturer Column Installation in Detector For connecting a capillary column into a detector see Column Installation on page 16 Varian Inc User Manual 430 GC and 431 GC Page 59 Injectors 1177 Split Splitless Capillary Injector Setting 1177 Gas Flow Rates The gas flow rates for the 1177 Split Splitless Capillary Injector can be set using manual pneumatics or Electronic Flow Control Note that a positive flow through the column must be set before heatin
100. tics system in that there is an inlet mass flow controller supplying carrier gas to the injector and a pressure control valve downstream from the injector which sets the injector pressure As injector pressure determines the rate of carrier gas flow through the column this pressure is monitored close to the point of injection Type EFC21 allows the user to set constant injector pressure or constant flow In addition the split ratio can be programmed Needle Valve poe SSS See a era 7 EFC21 i x GC Control Septum Purge I l l I l I l l Digital Flow Control z Carrier Gas inlet Pencil Filter Molsieve tharcoal CP742210 silver color Pencil a split Line Filter harcoal CP742211 gold color Pressure troller lee een cies column Split Vent Figure 13 EFC21 and 1177 in Split mode Flow Diagram See Pencil Filters on page 51 Page 56 User Manual 430 GC and 431 GC Varian Inc 1177 Split Splitless Capillary Injector Injectors Needle Valve ioe eee l l l Digital Flow Control Carrier Gas inlet i gt lt Molsieve Charcoal CP742210 silver color Pencil Split Line Filter I Charcoa CP 42211 gold color P Sensor ressure troller Digital Pressure Contr
101. tor noise A If hydrogen is used as a carrier gas vent the hydrogen from the TCD to a safe place Hydrogen is very flammable WARNING Page 88 Before Operating the TCD Do not operate the TCD until you have connected carrier gas to both inlets of the TCD The TCD accommodates two columns a column for the reference cell and a column for the detector cell or a column and a reference line The columns can be packed or capillary columns and you can combine a capillary column with a packed column To avoid contaminating the detector condition all packed columns before you connect them to the TCD For the following discussion assume that the analytical column is attached to the right side of the TCD and the reference column or reference gas supply to the left side of the TCD However you can configure the GC with the analytical column connected to the left side of the TCD simply reverse the TCD polarity If you plan to operate the TCD after the carrier gas has been turned off for an extended period of time turn on the carrier gas for five minutes before turning on the filament current to purge air from the system This prevents oxidation of the TCD filaments User Manual 430 GC and 431 GC Varian Inc Thermal Conductivity Detector TCD Detectors At the factory the carrier gas flow rate for TCD is set at 30 mL min Carrier gas He through both sides of the detector The carrier gas flow rate is measured at the two exit po
102. tween the jet and the electrode and when a carbon containing solute is burnt in the jet the electron ion pairs that are formed are collected at the jet and cylindrical electrode The following instructions refer to the operation of a 430 GC Flame lonization 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 back right of the instrument The electronics of the FID are controlled from the 430 GC Display Keyboard the gas flows are set and controlled either from the 430 GC Display Keyboard if detector EFC is installed or at the pneumatics panel User Manual 430 GC and 431 GC Page 79 Detectors Flame lonization Detector FID OONDORWDNDM Installation Disassembly At times it is necessary to remove the detector components to inspect to clean to replace parts or to install another detector Follow the disassemble reassemble instructions on the next pages for both the FID and the detector oven Exploded View Signal Cable 200187700 Signal Probe 200187300 Ignitor Cable 392548701 Ignitor Probe 200187200 Screws 8 32 x 1214200804 Collector Tube 394958700 Tower Screws 8 32 x 3 391866301 Ceramic Insulator 2100003200 Tower Top Plate 3400073100 Detector Tower Body 100099300 Flame Tip 0 010 in Capillary Tip 200187500 Flame Tip 0 010 in Standard Tip 200193800 Ferrule Vespel 100
103. used User Manual 430 GC and 431 GC Page 53 Injectors 1177 Split Splitless Capillary Injector Features of the 1177 injector The 1177 operates isothermally from 50 to 450 C Changing from one injection mode to another typically involves a change of injector insert and a modification to the injector and EFC program Glass inserts can be easily changed from the top of the injector The internal injector temperature profile keeps the septum cool while maintaining the point of injection at the setpoint temperature The 1177 uses positive septum purge to minimize the adsorption of sample onto the injector septum and to prevent contaminants from the septum entering the column The 1177 uses a unique dual split vent that allows effective sweeping of the entire injector body Automatic Start Switch The automatic start switch is a spring loaded actuator that fits over and is aligned with the injection port of the 1177 injector nut The GC run is started when the actuator is depressed by the syringe barrel or manually pressed at the moment of sample injection The GC run can also be manually started by pressing the START key on the keyboard The injector nut and automatic start switch assembly may WARNING be very hot during instrument operation and should not be BURN HAZARD touched with unprotected hands 1177 Injector Inserts Click here to see the 1177 Injector Inserts on page 103 Note that all 1177 injecto
104. vent and septum purge flow rates to ensure these values have not changed 6 Condition the insert by setting the 1177 Injector to the split mode and purging with carrier gas for 30 minutes at 300 C User Manual 430 GC and 431 GC Varian Inc Maintenance Parts and Supplies Pencil Filter The Pencil filters are used to protect the Injector and or EFC injector depending The Pencil Filter s are located underneath the Top cover Both pencil filters must be replaced on a yearly base It is advised to replace the filters by a Varian service engineer on a regular maintenance visit Pencil Filters Two types of Pencil Filters are available 1 Molsieve Charcoal filter CP 742210 silver color Varian Inc User Manual 430 GC and 431 GC Page 51 Maintenance Parts and Supplies Page 52 User Manual 430 GC and 431 GC Varian Inc 1177 Split Splitless Capillary Injector Injectors THE 1177 SPLIT SPLITLESS CAPILLARY INJECTOR Varian Inc MA oi The 1177 is a dedicated Split Splitless Isothermal Capillary Injector which operates in two modes e Split Isothermal e Splitless Isothermal The 1177 Injector can be used with a wide range of narrow bore to large bore 100 to 530 um 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
105. while you pull off the O ring Note The glass inserts can be cleaned and reused We recommend that you use a new O ring each time you remove the insert for cleaning or replacement Varian Inc User Manual 430 GC and 431 GC Page 49 Maintenance Parts and Supplies Page 50 Inserting the Glass Insert Follow these steps to replace the glass insert in the 1177 Injector 1 Using tweezers or clean lab tissue carefully slide the new insert into the injector body Place a new o ring over the insert and gently work it down until it sits over the o ring seat at the top of the injector body Use tweezers to work the o ring down the insert Avoid touching either the o ring or the insert 2 Carefully place the septum purge head over the insert Tighten the two captive screws alternately for uniform seating of the purge head onto the body and uniform seal of the o ring Note that placing the purge head onto the body may take some care since the gas supply line and septum purge lines may have minor resistance to movement 3 Reinstall the injector switch and retaining nut 4 Use tweezers to place a new septum in the purge head Note If the septum has a Teflon face place the Teflon face down toward the column 5 Place the injector nut on the injector and tighten by hand until you feel some resistance then tighten an extra 1 4 turn using the injector nut wrench Note After the injector nut has been replaced check the split
106. with a graphite ferrule Install a new aluminum seal washer onto the shoulder of the detector base To ensure a reliable tower seal use a NEW aluminum washer each time you install the detector Place the detector tower on the detector base and secure it with the two 8 32 x 2 3 4 inch tower mounting screws do not exceed 20 inch pounds of torque Alternately tighten these screws a 1 2 turn as the tower tightens into place following the torque specification above Handle the ceramic insulator and probes with tweezers to avoid contamination Carefully insert the ignitor probe into the lower arm of the detector tower Align the probe key with the tower arm slot Check the orientation of the ignitor elements by looking down through the top of the detector tower The spring clip should slip around the flame tip and make good contact see Figure 21 on page 83 The ignitor coil must not touch the flame tip assembly nor be positioned directly above it Tighten the knurled nut to secure the probe Make sure the notch in the detector tower arm does not cut the O ring seal Insert the insulator into the detector tower then insert the collector tube into the tower The collector tube must not touch the ignitor coil Insert the signal probe into the upper arm of the detector tower The probe clip should fit around the tapered section on the collector tube tightly enough to exert a User Manual 430 GC and 431 GC Varian Inc Detectors downward for
107. your Varian Service Representative TEMP gt MAX DET SETUP Soft Change either temperature limit or the programmed temperature and re activate the method TEMP gt MAX DET TEMP Fatal Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative TEMP gt MAX INJ SETUP Soft Change either temperature limit or the programmed temperature and re activate the method TEMP gt MAX INJ TEMP Fatal Turn off instrument and turn it back on If the Error recurs call your Varian Service Representative Varian Inc User Manual 430 GC and 431 GC Page 97 Errors Page 98 User Manual 430 GC and 431 GC Varian Inc Shipping Cleaning and Disposal Instructions SHIPPING CLEANING AND DISPOSAL INSTRUCTIONS SHIPPING INSTRUCTIONS subsidiary or Varian Inc representative it is very important to follow these additional preparation instructions A If your 430 GC for any reason must send back to the nearest Varian Inc CAUTION 1 Place the shipping restrain pin back 2 Put protection plugs on the sample and or carrier gas inlets 3 Remove columns CLEANING INSTRUCTIONS To keep the 430 GC surface clean refer to the remarks given below Switch the 430 GC off Remove the power cable Put protection plugs on the sample and carrier gas inlets Put protection plugs on the Column vents Use a soft no hard or abrasive brush to carefully brush away all dust and dirt e lf the outer cas
108. zardous Error is detected such as a thermal runaway the 430 GC shuts down the affected component and reports the Error After correcting the Error normal operation is restored by powering the 430 GC OFF then ON Page ll User Manual 430 GC and 431 GC Varian Inc Warranty VARIAN ANALYTICAL INSTRUMENT WARRANTY HARDWARE PRODUCTS All analytical instruments sold by Varian are warranted to be free from defects in material and workmanship for the periods specified and in accordance with the terms on the face of Varian s quotation or as otherwise agreed upon in writing between Varian and the Customer The warranty period begins on the date of shipment from Varian to the original Customer However where installation is paid for by the Customer or included in the purchase price the warranty period begins upon completion of installation If the Customer schedules installation to start later than 30 days after delivery or if such delay is caused through the Customer s inability to provide adequate facilities or utilities or through failure to comply with Varian s reasonable pre installation instructions or through other omissions by Customer then the warranty period starts on the 31st day from date of shipment Moreover Varian will charge the Customer for labor and other expenses involved in making multiple or follow up installation service calls SOFTWARE PRODUCTS Where software is provided within the frame of a license agreement concluded between

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