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1177 Split/Splitless Capillary Injector - Injectors

Varian, Inc.

User Manual 450-GC

Page: 169

Testing the 1177 Injector Performance

The following procedure describes how to test the performance of the 1177
Capillary Injector. This is best done with a test sample containing an
appropriate set of components for the installed detector. The following table
lists the series of test samples available for 450-GC.

Test Sample

Part Number

Concentrati ons of Test Compoun ds

TCD

82-005048-01

3.00

μ

g/

μ

L of C

14

, C

15

and C

16

in iso-octane.

ECD

82-005048-02

33.0 pg/

μ

L of lindane and aldrin in iso-octane.

PFPD

82-005048-03

20.0 ng/

μ

L of n-dodecanethiol, tributylphosphate,

methyl parathion; 4000 ng/

μ

L of n-pentadecane in

iso-octane.

TSD

82-005048-04

2.00 ng/

μ

L of azobenzene, methyl parathion; 4.00

ng/

μ

L malathion and 4.00

μ

g/

μ

L C

17

in iso-octane.

FID

82-005048-07

30 ng/

μ

L of C

14

, C

15

and C

16

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 31: Detector Test Samples

To run one of these test samples, use the chromatographic conditions listed
previously for the injection technique you are currently using. The detector
should be operated at the most sensitive range, e.g., 12 for FID and TSD, 0.05
for TCD, 10 for PFPD and 1 for ECD. The resultant chromatogram on page 419
should approximate that shown in the detector section of this manual.

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Содержание 450-GC

Страница 1: ...1 9259452344 Europe Europe P O Box 8033 P O Box 8033 4330 EA Middelburg 4330 EA Middelburg The Netherlands The Netherlands Tel 31 118671000 Tel 31 118671000 Fax 31 118623193 Fax 31 118623193 Australi...

Страница 2: ...Similarly determine the physical location of the Electronic Flow Control Similarly determine the physical location of the detector you want to use and identify t detector you want to use and identify...

Страница 3: ...ernative elect to refund refund an equitable portion of an equitable portion of the purchase price of the instrument or accessory the purchase price of the instrument or accessory Repair or replacemen...

Страница 4: ...ian cannot accept responsibility for any damage or injury caused by misunderstanding of the information in responsibility for any damage or injury caused by misunderstanding of the information in this...

Страница 5: ...d panels attached panels Hazardous chemicals may be present Avoid Hazardous chemicals may be present Avoid contact contact especially when replenishing reservoirs Use proper eye especially when replen...

Страница 6: ...M EMC Directive as requir C Directive as required to carry ed to carry the European Union CE Ma the European Union CE Mark rk This instrument is designed for chromatographic ana This instrument is des...

Страница 7: ...d r frayed power power cords i cords immediately mmediately with the with the same same type a type and ratin nd rating g COMPRESSED GAS CYLINDERS COMPRESSED GAS CYLINDERS Store a Store and h nd handl...

Страница 8: ...dioactive Source Detectors Radioactive Source Detectors Read carefully and comply with all NOTES CAUTIONS and WARNINGS in Read carefully and comply with all NOTES CAUTIONS and WARNINGS in the Ni the N...

Страница 9: ...by qualified personnel on both a contractual or as on both a contractual or as needed basis needed basis Varian Analytical Instruments Sales Offices Varian Analytical Instruments Sales Offices For Sa...

Страница 10: ...Safety Information Safety Information Page Page X X User User Manual Manual 450 GC 450 GC Varian Varian Inc Inc CE DECLARATION OF CONFORMITY CE DECLARATION OF CONFORMITY...

Страница 11: ...RS VII GC SAFETY PRACTICES VIII Exhaust System VIII Radioactive Source Detectors VIII Burn Hazard VIII SPARE PARTS AVAILABILITY IX SERVICE AVAILABILITY IX CE DECLARATION OF CONFORMITY X TABLE OF CONTE...

Страница 12: ...te to Condition Column 22 Injector Conditioning 22 Column Conditioning 23 New Columns 23 Used Columns 23 Connect Capillary Column to Detector 24 Column Insertion Depths for Varian Detectors 24 Connect...

Страница 13: ...ECTOR 205 205 Automatic Star Automatic Start Switch t Switch 206 206 1041 Injector Insert 1041 Injector Insert 206 206 Injector A Injector Assembly and ssembly and Insert Insert 207 207 1041 Electron...

Страница 14: ...lass Insert 237 237 Syringe Syringe 237 237 Mounting the Column Mounting the Column 238 238 Column Column Installation Installation 238 238 Condition Condition the Colum the Column n 238 238 Column In...

Страница 15: ...T 262 262 Building an SPT metho Building an SPT method d 263 263 Replacing the Trap Assembly Replacing the Trap Assembly 264 264 SPT System SPT System Compon Components ents 265 265 Remove the SPT Cov...

Страница 16: ...ogen Flow 309 309 Maintainin Maintaining Optimum Cond g Optimum Conditions itions 310 310 Column Bleed Column Bleed 311 311 Solvent Solvent Consideratio Considerations ns 311 311 Chlorinated Chlorinat...

Страница 17: ...n Stages of Flame Pulsation 347 347 How Does the PFPD Achieve its How Does the PFPD Achieve its Greater Detectivity and Selectivity Greater Detectivity and Selectivity 348 348 Background Emission in a...

Страница 18: ...and Gate Width Parameters 388 388 Setting the Trigger Level Setting the Trigger Level 390 390 Setting Gate Delay and Gate Setting Gate Delay and Gate Width Width 392 392 Set Gate Width Set Gate Width...

Страница 19: ...Not Ign Flame Does Not Ignite ite 414 414 Baseline Noise is Too High Baseline Noise is Too High 415 415 Baseline Baseline is Erratic is Erratic tick tock tick tock 417 417 DETECTOR TEST DETECTOR TEST...

Страница 20: ...0 470 Programmed Temperature Vaporizer PTV Programmed Temperature Vaporizer PTV 470 470 Desc Descripti ription on 470 470 Cold Split Injection Cold Split Injection 471 471 Cold Sp Cold Splitless Injec...

Страница 21: ...Table of Contents Table of Contents Page Page XXIV XXIV User User Manual Manual 450 GC 450 GC Varian Varian Inc Inc...

Страница 22: ...177 F FIGURE IGURE 24 24 EFC21 EFC21 AND AND 1079 1079 IN IN S SPLIT MODE PLIT MODE F FLOW LOW D DIAGRAM IAGRAM 181 181 F FIGURE IGURE 25 25 EFC25 EFC25 AND AND 1079 1079 F FLOW LOW D DIAGRAM IAGRAM...

Страница 23: ...ROSS SECTIONAL VIEW 316 FIGURE 54 TCD SENSITIVITY AND AMPLIFICATION 326 FIGURE 55 ECD EXPLODED VIEW 335 FIGURE 56 RADIOACTIVE CAUTION LABEL GENERAL LICENSE DEVICE 338 FIGURE 57 RADIOACTIVE CAUTION LAB...

Страница 24: ...ODULES 63 TABLE 21 SAMPLER INJECTOR POSITION 69 TABLE 22 VALVE TYPE NAMES 72 TABLE 23 ANALOG CABLES 95 TABLE 24 INJECTION MODE PARAMETERS FOR ON COLUMN 125 TABLE 25 INJECTION MODE PARAMETERS FOR SPLIT...

Страница 25: ...SPT REPLACEMENT PARTS 275 TABLE 52 ECD GASES PRESSURES PURITY AND FLOW RATES 334 TABLE 53 SPECIFICATIONS PFPD 352 TABLE 54 SPECIFICATIONS NITROGEN MODE PFPD 353 TABLE 55 ACCESSORY KIT PFPD 354 TABLE...

Страница 26: ...n this Manual AC alternating current DC direct current ECD Electron Capture Detector EFC Electronic Flow Control FID Flame Ionization Detector PFPD Pulsed Flame Photometric Detector TCD Thermal Conduc...

Страница 27: ...Hydrogen burns Hydrogen burns with a with a no no luminous flame luminous flame which can which can be be invisible under invisible under bright light bright light Hydrogen is potentially explosive Ta...

Страница 28: ...at can spark sources of static electricity etc flames devices that can spark sources of static electricity etc Do n Do not all ot allow h ow hydrogen ydrogen from from a h a high p igh pressure ressur...

Страница 29: ...rking EFC s 2 Bar 30 psi for well working EFC s Example Column pressure neede Example Column pressure needed 100 kPa d 100 kPa 200 kPa pressure drop Inlet 200 kPa pressure drop Inlet pressure needed a...

Страница 30: ...s to the GC Watch e GC Watch the the pressure gauge closely and adjust the pressure gauge closely and adjust the pressure according to pressure according to Table 2 Table 2 on on page 10 page 10 8 8 L...

Страница 31: ...verify the the 450 GC 450 GC configuration configuration Your GC is shipped from the Your GC is shipped from the factory with default settings The following is factory with default settings The follow...

Страница 32: ...n Factory installed Injectors other than the 1041 have a glass other than the 1041 have a glass insert suitable for a variety insert suitable for a variety of applications If of applications If your a...

Страница 33: ...re co Three types of ferrules are common mmon graphite Vespe graphite Vespel or polyimide and l or polyimide and graphite Vespel graphite Vespel Do Do not not use use graphite graphite with with ECD E...

Страница 34: ...thly as possible To achieve this a smoothly as possible To achieve this a proper proper scoring tool is required A scoring tool is required A ceramic scoring wafer 01 900158 0 ceramic scoring wafer 01...

Страница 35: ...o a firm stop This correctly positions the column against the upper stop This correctly positions the column against the upper end of the Injector insert The column must go in the full distance If it...

Страница 36: ...variety of with a variety of ferrule types Do not over ferrule types Do not over tighten capillary column nuts use a tighten capillary column nuts use a new ferrule if the column does not new ferrule...

Страница 37: ...rted for packed column use by installing the appropriate adapters Place nuts and ferrules on both ends of column as shown If your column is metal insert it into the Injector fitting and gently push un...

Страница 38: ...onically controlled EFC or manually controlled and are different for each Injector system If your Injector model is a Carrier gas flow is regulated by a 1041 1061 Type EFC23 or type EFC24 with valving...

Страница 39: ...e with EFC installed For either a 1177 or 1079 PTV with manual pneumatics see the Injector section of the Operator s Manual on page 97 for further information 1 Press the FLOW PRESSURE key and set the...

Страница 40: ...ion front middle or rear or type Press the Calibrate button You will be prompted to enter the Column Head Pressure and Adjusted Septum Purge Flow Rate Fill in the column head pressure and adjust and m...

Страница 41: ...E key select the appropriate Injector by location and set the pressure according the table Table 9 Column condition head pressure For capillary columns the gasflow through the column is verified by di...

Страница 42: ...ine retention of extra peaks etc For fused silica columns it is recommended that 1 to 2 turns at the beginning of the column approximately 1 2 meter be cut off prior to reconditioning as this is the e...

Страница 43: ...er PN 03 925605 01 is used on the TCD inlet DO NOT use graphite ferrules with the ECD Uncoil about 20 cm from end of column Move the column nut and ferrule to within 5 cm of the column end Find the co...

Страница 44: ...her than TCD locate the packed column detector adapter in the Packed Column Kit and install on the inlet to the detector The TCD inlet is designed for packed column installation Insert the open end of...

Страница 45: ...Make Up Carrier Gas Flow Rate mL min Detector Gas Air 1 mL min Detector Gas Air 2 mL min Detector Gas H2 mL min FID N2 H2 or He 20 1 1 15 N2 or He 30 1 300 10 30 1 PDHID For more details see Installat...

Страница 46: ...counter clockwise or until the turns counting dial reads zero Observe reading on flowmeter Ensure it is within the range described in the table for carrier gas flow rates Adjust the carrier gas flow...

Страница 47: ...t ratio to 100 Press the COLUMN OVEN key and set the initial column oven temperature to 250 C Press the DETECTOR key and set the detector oven temperature to 300 C If the detector is an FID wait for t...

Страница 48: ...s for your column For 1041 and 1061 Injectors ECD FID TCDa TSD PFPD Initial column oven temp C 80 80 80 80 80 Initial column oven hold time min 1 1 1 1 1 Program 1 ramp rate C min 20 20 20 20 20 Final...

Страница 49: ...t Sample You are now ready to prepare your sample For preparation of samples for automated injection please refer to the CP 8400 AutoSampler section on page 121 You may inject your sample neat or dilu...

Страница 50: ...e 69 0 5 Phenyl 95 Methyl Cyclohexane 80 7 Iso octane 99 3 Benzene 80 1 Toluene 110 6 Ethyl Ether 34 6 Methyl tert butyl ether 55 2 Methylene Chloride 39 8 Chloroform 61 2 Carbon Disulfide 46 5 Interm...

Страница 51: ...D make a 1 20 dilution of the test sample in iso octane With the READY light on at the GC and the appropriate volume of test sample in your injection syringe you are ready to make your injection For a...

Страница 52: ...ECTORS The 450 GC Gas Chromatograph is equipped with various connectors on the rear panel and top of the instrument intended for use with peripheral equipment such as AutoSamplers and data handling de...

Страница 53: ...VAC output see on page 38 J44 Cryo Valves 3 24 VDC Cryo valve connection See on page 39 J42 J43 External Events Timed Events contacts See on page 40 J41 Heater Connections Line Voltage Heater connect...

Страница 54: ...User Manual 450 GC Page 35 J504 J505 S I D 1 AND 2 Sample Introduction Device used for AutoSampler control AutoSampler CP 84XX ONLY on connector S I D 2 CombiPal on connector S I D 1 or S I D 2 Figur...

Страница 55: ...ator or other device is connected the 450 GC is waiting not ready on display for Ready In signal pin 1 to start In the Setup tab Configuration on page 67 the Ready In Closed Contact checkbox must be c...

Страница 56: ...Peripheral Connectors Varian Inc User Manual 450 GC Page 37 J302 TEMPERATURE PROBES Temperature probe connectors for Heaters Figure 6 Connector J302 Top View...

Страница 57: ...Connectors Page 38 User Manual 450 GC Varian Inc J45 J46 AUXILIARY 1 AND 2 24 VAC output used for power supply AutoSampler CP 8400 or AutoInjector CP 8410 Figure 7 Connector J45 J46 Top View See Fuses...

Страница 58: ...Peripheral Connectors Varian Inc User Manual 450 GC Page 39 J44 CRYO VALVES 3 24 VDC Cryo valve connections Figure 8 Connector J44 Top View See Fuses on page 44...

Страница 59: ...40 User Manual 450 GC Varian Inc J42 J43 EXTERNAL EVENTS Timed 24 Volt DC contacts 7 connector for more optional contacts see Option Board on page 43 Figure 9 Connector J42 J43 Top View See Fuses on p...

Страница 60: ...by incorrect choice of certain parameters The SPME mode requires different hardware optional If the SPME mode is selected the other injection modes will not be available This section will cover AutoS...

Страница 61: ...ain power switch and unplug the power cord Use the correct included screws metric to mount the sampler 1 Before installing the CP 8400 or CP 8410 AutoSampler make certain your 450 GC is equipped with...

Страница 62: ...ver by lifting up and removing the Detector cover Remove the Detector cover by lifting the rear of the cover and sliding it towards the rear of the GC and up Remove the 4 screws holding the Injector c...

Страница 63: ...he retaining screws on the Injectors You may need to unscrew the Injector nut and remove the inject switch to have unimpeded access to the Injector retaining screws replace the Injector nut if removed...

Страница 64: ...t with either the front or rear mounting position See Figure 14 as appropriate 12 The base is secured to the Top Cover via 2 short screws at the rear and 3 long screws underneath the AutoSampler AutoI...

Страница 65: ...ent Wash on page 111 vial 18 Place a capped vial into the Vial 0 location if you have a CP 8400 or the Vial 1 location if you have a CP 8410 19 Place the CP 8400 sample carrousel onto the base or plac...

Страница 66: ...tion process 5 The GC Sampler combination must be calibrated now proceed with the next calibration chapter It is important that the CP 8400 8410 is switched on prior to power up the GC A flashing gree...

Страница 67: ...he large wash vial the capacity is increasing by a factor of 60 The Large Wash Vial is a 120 mL stainless steel vial and has 2 openings Both use a snap cap The vial replaces the 5 mL solvent vial The...

Страница 68: ...Sampler has been removed from the GC and after maintenance repair back on the GC Bending Sample needles Other Injector positions used back or front If the Injector has been removed calibration is man...

Страница 69: ...that you recalibrate the Vial 0 Position to avoid bent needles and other minor problems In order to accurately calibrate Vial positions use the calibration tool P N CP740889 The calibration tool simu...

Страница 70: ...CP 8400 Vial 0 position involves manipulating the positions of 3 different components Tower Syringe and Carrousel Calibrating the CP 8410 Vial 1 position involves manipulating the positions of 2 diff...

Страница 71: ...ween the tower and sample carrousel one or more times to determine the optimum rotational positions 7 Adjust the syringe sled height so that the needle is just barely above the calibration tool top Yo...

Страница 72: ...n will be visible 3 Before starting the calibration identify Injector 1 and Injector 2 Injector 1 is the first Injector the Tower will encounter when it rotates clockwise to reach the Injector s The s...

Страница 73: ...otates so that it is over Injector 1 position and lowers the syringe sledge so that it is over the Injector Syringe moves automatically during operation of instrument Keep your hands and fingers out o...

Страница 74: ...ct Switch Locator cone 7 Adjust the height using the Up and Down button of the needle guide such that the sled is just resting on or very slightly depressing the Injector Switch and is covering the lo...

Страница 75: ...e SETUP key and select CALIBRATION select on the next page Sampler Change Syringe 2 The next massage will pop up and the Sampler Tower will go to his Syringe Replace Check Syringe position 3 Check or...

Страница 76: ...YRINGE SIZE CHANGE For changing the syringe size the next procedure MUST be followed 1 Change syringe size in Setup tab SampleDelivery 2 Press OK to leave Setup 3 Follow the Syringe Check Replace proc...

Страница 77: ...n volume vial range GC method within the Automation pages for quick access and change Those parameters that drive the AutoSampler actions such as clean viscosity settings and needle residence times ar...

Страница 78: ...injection In SPME however the plunger is at the top of its travel when it is in the home position and the SPME fiber must be exposed by inserting the plunger into the fiber holder barrel to expose the...

Страница 79: ...124 Standard Split Splitless 3 Neat samples on page 126 Neat 4 Viscous samples on page 128 Viscous 5 Volatile samples on page 129 Volatile 6 User Defined on page 131 User Defined Choosing 1 of these 5...

Страница 80: ...7 5 Plunger Speed Up L s 0 5 1 2 5 5 10 20 50 Plunger Speed Down L s 5 10 25 50 25 50 62 5 2 If used Any Pre Injection Sample Clean Flushes sample waste Volume L 0 75 1 5 3 75 7 5 37 5 75 187 5 Plunge...

Страница 81: ...rd is not permitted with Standard Sampling modes Standard mode parameters are set for samples dissolved in common solvents such as iso octane The Standard sampling mode for Split Splitless performs th...

Страница 82: ...e L 0 1 0 2 0 5 0 5 0 5 2 4 6 Inject Sample Plunger Speed During Injection L s 5 10 25 50 25 50 62 5 Pre Injection Delay s 0 0 0 0 0 0 0 0 0 0 0 0 0 0 Post Injection Delay s 6 0 6 0 6 0 6 0 6 0 6 0 6...

Страница 83: ...stic door and remove the syringe 4 Remove the syringe bracket 3 screws 5 Push the Injector s plunger head holder downwards 6 Push the syringe sled down as far as it will go Once the syringe guide foot...

Страница 84: ...a way that you can see the opening in the barrel Installation of the fiber into the SPME syringe i e the fiber holder is explained in the fiber holder manual 11 Close the cover on the tower and turn o...

Страница 85: ...fiber it is important to use the correct Injector insert Use a straight unpacked insert with an internal diameter of 0 8 mm P N 392611948 for the 1079 Injector Smaller inserts do not allow the fiber s...

Страница 86: ...S To minimize pollution of the analysis by the vial septum special Ultra clean septa are used These vials are included in the SPME kit Replacement parts see here on page 441 Agitation Strokes SPME can...

Страница 87: ...higher than the DOWN position The DOWN position is set at the point at which the fiber is just fully immersed in the sample liquid Typical value for the 2 mL vial P N 392611549 and P N 392611979 Sampl...

Страница 88: ...ime min tAdsorb tagitation nstrokes 1 Whereby tAdsorb is the adsorption time min tagitation is the time per agitation stroke approx 0 01 min nstrokes is the number of agitation strokes For example an...

Страница 89: ...gulations and t he general operating principles including the calibration of the sampler positions To enable the sampler to perform Liquid Sampling 2 basic adjustments of the sampler are required The...

Страница 90: ...may be hot 3 Open de tower s clear plastic door and remove the syringe 4 Remove the syringe bracket 3 screws 5 Push the Injector s plunger head holder downwards Once the syringe guide foot touches th...

Страница 91: ...ringe in the block Lock the plunger head and fix the syringe 10 Close the cover on the tower and turn on the power to the gas chromatograph The gas chromatograph will automatically detect the new conf...

Страница 92: ...AutoSamplers Page 152 User Manual 450 GC Varian Inc...

Страница 93: ...thermal Capillary Injector which operates in 2 modes Split Splitless The 1177 Injector can be used with a wide range of narrow bore to wide bore 100 to 530 m ID capillary columns The basic pneumatics...

Страница 94: ...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...

Страница 95: ...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...

Страница 96: ...he flow of carrier gas through the Injector during the analytical run When the Split State is unchecked most of the sample injected is directed onto the column When the Split State is checked the samp...

Страница 97: ...Splitless 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 Injecto...

Страница 98: ...Injectors 1177 Split Splitless Capillary Injector Page 158 User Manual 450 GC Varian Inc Figure 21 EFC21 and 1177 in Splitless mode Flow Diagram See Pencil Filters on page 437...

Страница 99: ...C25 is almost identical with 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 Purge and Trap device...

Страница 100: ...gulator 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 1177...

Страница 101: ...d with the 1177 Injector allows the user to set a 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 pressur...

Страница 102: ...tric column flow rate constant during temperature programming of the column oven when Constant Flow is selected The same general guidelines should be followed for all injection modes If the column is...

Страница 103: ...ssible Selecting Pressure Pulse gives you the option of enabling a pressure pulse setting the desired pressure and the duration for which the pressure should last Typically the pressure pulse pressure...

Страница 104: ...rect Injector Page 1 or Page 2 or Page 3 A time entry of 0 turns the Gas Saver feature off If a non zero time is entered the Gas Saver timer will start incrementing If a run is not started or a new me...

Страница 105: ...ibration when columns of different length and diameter are installed With type EFC21 the septum purge calibration routine should be carried out when the instrument is first set up or when a new column...

Страница 106: ...t 4 mm ID open insert packed with glass wool Column Position 3 7 cm from the bottom of the column nut at the base of the Injector Injector Temperature Initial temperature isothermal 250 C Column Tempe...

Страница 107: ...82 005048 03 20 0 ng L of n dodecanethiol tributylphosphate methyl parathion 4000 ng L of n pentadecane in iso octane TSD 82 005048 04 2 00 ng L of azobenzene methyl parathion 4 00 ng L malathion and...

Страница 108: ...d de et te ec ct to or r t th he e S Si il lt te ek k l li in ne er r R RT T2 21 10 04 46 62 21 14 45 5 m mu us st t b be e u us se ed d 1 Injector Nut 392597501 Injector Nut Wrench 390842300 2 Knob...

Страница 109: ...n 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 Philips screwdriver long handle...

Страница 110: ...ody 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...

Страница 111: ...e Injector assembly Set the column nut and column end on the floor of the GC oven Use proper eye and skin protection Methanol and acetone are toxic and flammable chemicals Exercise appropriate precaut...

Страница 112: ...n the nut This procedure minimizes twisting the column 11 Use the 5 16 open end wrench and tighten with 1 6 turn to secure the column in place 12 To check whether the Injector is leak tight connect a...

Страница 113: ...pen tubular columns and is capable of isothermal or temperature programmed operation Advanced Performance Five modes of operation split splitless temperature ramped splitless Large Volume Injection LV...

Страница 114: ...minants from the septum entering the column The 1079 PTV combined with the ChromatoProbe on page 198 is an effective tool for chromatographic analysis of dirty samples liquids solids and slurries bloo...

Страница 115: ...3301 0 32 mm ID 2 CR212125 CR213125 CR211125 0 53 mm ID 1 CR214108 CR212108 CR213108 CR211108 SG073302 Table 33 1079 Column Ferrules 1 16 1 Injector Nut 394966601 Injector Nut Wrench 390842300 2 Autom...

Страница 116: ...ixtures e g hydrocarbon mixtures 2 glass inserts are recommended when operating in the splitless temperature ramp mode 1 The 2 mm ID glass wool packed insert is used for non polar compounds at levels...

Страница 117: ...out the split vent to the flow through the column The 1177 Split Splitless Injector on page 153 is optimized for Split application Isothermal Splitless Mode The 3 4 mm insert packed with glass wool i...

Страница 118: ...tion being vented In the example below is a splitless injection The Injector is held in the split state for the initial period with split ratio of 20 When the run is started the split state will switc...

Страница 119: ...s 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 pressu...

Страница 120: ...st 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 Purge and Trap devices upstream fr...

Страница 121: ...uses this flow to control column head pressure which in turn controls carrier gas flow through the column Operation of the 1079 PTV Injector The following section describes how to operate the 1079 PTV...

Страница 122: ...th the 1079 PTV Injector allows the user to set a 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 pressur...

Страница 123: ...g temperature programming of the column oven when Constant Flow is selected The same general guidelines should be followed for all injection modes If the column is operated isothermally then the press...

Страница 124: ...lecting Pressure Pulse gives you the option of enabling a pressure pulse setting the desired pressure and the duration for which the pressure should last Typically the pressure pulse pressure is held...

Страница 125: ...1 or Page 2 or Page 3 A time entry of 0 turns the Gas Saver feature off If a non zero time is entered the Gas Saver timer will start incrementing If a run is not started or a new method is not loaded...

Страница 126: ...columns of different length and diameter are installed With type EFC21 the septum purge calibration routine should be carried out when the instrument is first set up or a new column is installed or wh...

Страница 127: ...pressure gauge Set the column head pressure based on the column installed in the GC For example for a 30m x 250 m ID column set the column head pressure to 12 15 psig to achieve 1 mL min column flow r...

Страница 128: ...eat 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 ve...

Страница 129: ...case of the standard TCD only two can be installed and then no additional detectors can be installed However a dual TCD option is available as a custom solution which allows installation of an additio...

Страница 130: ...onnector contains all 3 analog channels plus status signals for Ready In to the GC and Start Out from the GC In the SETUP page by the detector tab on the second page Page 2 or page 3 the Detector Anal...

Страница 131: ...ult Analog output voltage is 0 1 Volt 0 10 Volt is possible by selectable jumpers on the mainboard contact your local Varian office The right side of the screen is used to time program the signal sour...

Страница 132: ...cable options on page 94 depending on the device to which the cable is connected All cables have a 15 pin D shell connector on one end to attach to J401 on the 450 GC and have the appropriate connect...

Страница 133: ...rogen or other appropriate gas and burn at a small jet situated inside a cylindrical electrode A potential of a few hundred volts is applied between the jet and the electrode and when a carbon contain...

Страница 134: ...ements 2 Press the DETECTOR key on the 450 GC Display Keyboard to display the DETECTOR screen The FID should be listed in position Front Middle or Rear If your GC is equipped with detector EFC verify...

Страница 135: ...temperature to 300 C Verify that the FID electronics is turned OFF Operation 1 Check the detector temperature status on the DETECTOR FID screen Check the FID range setting and set to range 12 if nece...

Страница 136: ...flame is first lit but should drop to 10 mV within 30 minutes To avoid a possible fire or explosion always turn off the flow of hydrogen when the column is removed or when the detector is not being u...

Страница 137: ...el la ay y h he el lp ps s t to o r re ec co ov ve er r f fr ro om m F FI ID D f fl la am me e f fa au ul lt ts s a an nd d a av vo oi id ds s h ha av vi in ng g t th he e f fa au ul lt t a ag ga ai...

Страница 138: ...0 3 Ignitor Cable 392548701 4 Ignitor Probe 200187200 5 Screws 8 32 x 1214200804 6 Collector Tube 394958700 7 Tower Screws 8 32 x 3 391866301 8 Ceramic Insulator 2100003200 9 Tower Top Plate 340007310...

Страница 139: ...e laboratory tissue 5 Remove the 2 tower mounting screws from the top of detector tower 6 Remove the tower assembly from the detector oven lifting straight up until clear of the flame tip Remove the c...

Страница 140: ...shoulder of the detector base To ensure a reliable tower seal use a NEW aluminum washer each time you install the detector 5 Place the detector tower on the detector base and secure it with the 2 tow...

Страница 141: ...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 igniter cable to the igniter probe and the signal cable to the...

Страница 142: ...disassemble the FID on page 289 2 Scrape the deposits from the bore of the collector tube the insulator and the metal part of the flame tip with emery cloth e g SiO2 3 If the flame tip is plugged inse...

Страница 143: ...his situation or when the detector is to be operated at temperatures above 400 C you must replace the ferrule Be sure to select the proper ferrule for the application The Vespel graphite ferrule has a...

Страница 144: ...Detectors Flame Ionization Detector FID Page 294 User Manual 450 GC Varian Inc...

Страница 145: ...ciative 2He 1S 1 ground state This is the well known Hopfield emission The photon energy from the He2 continuum is in the range of 13 5 to 17 7 eV The detector is essentially non destructive 0 01 0 1...

Страница 146: ...er five orders of magnitude with minimum detectable quantities MDQs in the low or sub picogram range The response to fixed gases is positive the standing current increases with MDQs in the low ppb ran...

Страница 147: ...DHID Detectors Varian Inc User Manual 450 GC Page 297 During normal operation the detector produces ultraviolet energy UVA UVB some of which may be emitted Do not watch the arc without eye protection...

Страница 148: ...ual 450 GC Varian Inc Exploded View Figure 50 PDHID Exploded View 1 Ground electrode CP740764 Nut for ground electrode CP914060 Spanner tool CP740760 2 Detector cell CP740765 3 High voltage cable CP74...

Страница 149: ...ector PDHID Detectors Varian Inc User Manual 450 GC Page 299 Gas Connections Figure 51 PDHID Gas Connections Overview Installation The installation of the PDHID detector is normally done at the factor...

Страница 150: ...easily Never use leak detecting fluids on any part of the system Installing and Purging the Helium Purifier 1 If the pressure regulator has a 1 8 male cone type outlet port install the Valco 1 8 exter...

Страница 151: ...Restrictor TGA R 35F80P 3 Connect the outlet end of the restrictor to a flow measuring device Adjust the helium pressure to 80 psi to obtain a continuous flow of 35 mL min 4 After setting the flow rat...

Страница 152: ...til it breaks at the score mark breaks at the score mark 5 5 Examine th Examine the cut with e cut with the magn the magnifying lens ifying lens to decide to decide whether the whether the column was...

Страница 153: ...the remove the 2 Allen scre 2 Allen screws Item 15 ws Item 15 from the from the top of the igniter cap Item 3 Place the Allen screws on a top of the igniter cap Item 3 Place the Allen screws on a cle...

Страница 154: ...r tower with the PMT assembly aside on a clean surface the PMT assembly aside on a clean surface 3 3 Use the Use the metal fo metal forceps to rceps to remove remove the bottom the bottom aluminum alu...

Страница 155: ...ombustor support Tighten the approximately 1 mm above the end of the combustor support Tighten the column nut to secure column in place Next proceed column nut to secure column in place Next proceed o...

Страница 156: ...on 3 3 Continue with Continue with step step 4 4 in in Reassemble the Reassemble the PFPD PFPD Reassemble the PFPD Reassemble the PFPD Refer Refer on page 344 on page 344 Tools and equipment needed to...

Страница 157: ...uminum crunch aluminum crunch washer washer Item 13 on the Item 13 on the detector tower detector tower 6 6 Replace th Replace the igniter ca e igniter cap Item 3 p Item 3 on the d on the detector tow...

Страница 158: ...stor section of the PFPD combustor Follow these directions when adjusting this split valve of the PFPD combustor Follow these directions when adjusting this split valve 1 1 Disconnect Disconnect the o...

Страница 159: ...the following figure when adjusting the flow rates of the gases to rates of the gases to the PFPD the PFPD Item Description Item Description 1 1 Air1 Air1 mass mass flow flow controller controller 2 2...

Страница 160: ...ontroller valve Item 4 Note the current mass flow controller valve Item 4 Note the current dial setting Turn dial setting Turn Hydrogen Hydrogen OFF OFF 5 5 Install the Install the flow measu flow mea...

Страница 161: ...ontroll controllers off f ers off for an extende or an extended period then on d period then on aga again they must in they must equilibrate overnight before the PFPD can achieve optimum equilibrate o...

Страница 162: ...turn the Air1 flow controller counter clockwise until the flow just stops Again write down the dial setting It is recommended that the flow controller dial be set so that it reads zero at this setting...

Страница 163: ...tivity of the PFPD is Selective relative to what In some situations the Sulfur or Phosphorus response is best optimized relative to Carbon the principal background emission in the air hydrogen flame A...

Страница 164: ...as Flow Rate mL min H2 mL min Air1 mL min Air2 mL min Helium 2 13 17 10 5 13 20 10 10 20 34 10 Hydrogen 2 11 17 10 5 9 18 10 10 15 31 10 Nitrogen 2 14 17 10 5 16 21 10 10 24 34 10 Table 57 Flow Rates...

Страница 165: ...tings are recommended for setup and routine operation of the PFPD These adjustments are accessed by pressing the Adjustments button in the PFPD detector section of the 450 GC method Element Gate Delay...

Страница 166: ...sulfur response decreases with increasing detector temperature Set the detector temperature as low as possible while preserving chromatographic peak shape Phosphorus to Carbon selectivity Install wid...

Страница 167: ...ty and Dynamic Range Preliminary results indicate that the tin response is linear and extends over more than three orders of magnitude Other Considerations Tin compounds exhibit tailing in the PFPD pr...

Страница 168: ...ganese emission is not separated in time from the flame background emission a narrow band interference filter is required to provide adequate selectivity against hydrocarbons and other interfering ele...

Страница 169: ...that is to be used Sulfur mode Use the BG 12 deep violet glass filter Phosphorus mode Use the GG 495 yellow glass filter Sulfur Phosphorus mode Use the optional WG 345 glass filter Item Description 1...

Страница 170: ...g free it by using gentle pressure with a capillary pick or other clean utensil Place this filter on a clean surface e g lab tissue or in its storage container Handle the filter holder by its outside...

Страница 171: ...r an analysis the choice of the appropriate diameter narrow bore or wide bore of quartz combustor depends on the detection mode that is to be used Sulfur mode Use the narrow bore 2 mm ID quartz combus...

Страница 172: ...urged with carrier gas before connecting to the GC This will avoid introducing a large amount of air into the GC Flush the GC for a few minutes before heating the Column Detector fuel gases The typica...

Страница 173: ...the 450 GC 1 Set the column oven and the Injector zone temperatures to 50 C and allow them to reach this temperature This allows safe handling of Injector surfaces 2 Remove Injector septum nut and ins...

Страница 174: ...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 Purifier Replacement The most common g...

Страница 175: ...s being used an oxygen trap should also be added For trace analysis the combination of hydrocarbon trap moisture trap and oxygen traps should be used To install or replace the Gas Clean filter cartrid...

Страница 176: ...an autosampler In general the septum should be replaced every 50 100 injections or when symptoms of a septum leak are seen These symptoms include changing retention times reduced detector response or...

Страница 177: ...Maintenance Page 438 User Manual 450 GC Varian Inc...

Страница 178: ...n below Switch the 450 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 carefull...

Страница 179: ...Shipping Cleaning and Disposal Instructions Page 440 User Manual 450 GC Varian Inc...

Страница 180: ...w PTFE rubber septa 392611518 100 pk 100 l polypropylene crimp top vial 12 X 32 mm 11mm caps with PTFE Butyl rubber septa 392611669 100 pk 2 mL Vials Crimping tool 11 mm AL666011 1 pc 5 mL Ultra GC M...

Страница 181: ...vable needle SG005333 1 ea 250 L SGE 250 L syringe SGS006157 1 ea CP 8400 8410 Replacement Carrousel Tray CP 8400 AutoSampler 100 vial Sample Carrousel CP738642 1 ea CP 8410 AutoInjector Sample Tray C...

Страница 182: ...Splitless liner X 11 Splitless liner X 12 Gooseneck Split Splitless liner X 13 Gooseneck Split Splitless liner X 14 Gooseneck Split Splitless with glass wool X 15 Double Gooseneck Splitless liner X 1...

Страница 183: ...column guide for 3400 3500 3600 34 Glass column guide for 3700 450 GC 35 Split Splitless liner with glass wool X 36 Split liner packed with 10 OV 101 on Chromosorb WHP 80 100 X 37 Splitless liner X 3...

Страница 184: ...Splitless liner Gooseneck 2 mm 6 3 mm 72 mm 250 L Glass Yes 6 190010906 Liner for direct injection on narrow bore columns SPI Tapered 0 5 mm 5 mm 54 mm 10 L Glass Yes 7 190010907 Liner for on column...

Страница 185: ...wool plug plug open open glass glass Injector Injector inserts inserts 392611937 392611937 5 pk 5 pk 4 mm ID 4 mm ID unpacked open glass Injector inserts similar unpacked open glass Injector inserts s...

Страница 186: ...focusliner SGE split splitless 2 3 MM fast tapered focusliner inlet liner inlet liner SG092111 5 pk SG092111 5 pk No Picture available No Picture available SGE SGE split splitless split splitless inle...

Страница 187: ...milar to HP 5180 4168 5180 4168 392611935 10 pk 392611935 10 pk 1078 1079 PTV Injector 1078 1079 PTV Injector Parts and Supplies Parts and Supplies Ceramic Ceramic scoring scoring wafer wafer for for...

Страница 188: ...392611953 5 pk 392611953 5 pk 0 5 mm open insert for 0 5 mm open insert for trace analysis and thermolabile trace analysis and thermolabile compounds compounds 392611949 5 pk 392611949 5 pk 1078 107 1...

Страница 189: ...Green 3 3 9 5 9 5 mm mm CR246124 50 pk CR246124 50 pk Inserts Inserts 1041 1041 Insert Insert for for 0 53 0 53 mm mm ID ID columns columns 392543101 392543101 1060 106 1060 1061 Flash Injector 1 Fla...

Страница 190: ...58101 2869458101 10 pk 10 pk Polymide G Polymide Graphite raphite 0 8mm 0 8mm ID ID 2869458200 2869458200 10 pk 10 pk Graphite Graphite 0 5mm 0 5mm ID ID SG072626 SG072626 10 pk 10 pk Column Column Fe...

Страница 191: ...h Wrench 72 000081 00 72 000081 00 Thermal Conductivity Detector TCD Thermal Conductivity Detector TCD TCD Make up Gas Option TCD Make up Gas Option 03 925605 01 03 925605 01 Pulsed Flame Photometric...

Страница 192: ...Replacement Parts Replacement Parts Page Page 456 456 User User Manual Manual 450 GC 450 GC Varian Varian Inc Inc...

Страница 193: ...a a al l l l h h h he e e el l l lp p p pd d d de e e es s s sk k k k E E E Eu u u ur r r ro o o op p p pe e e e M M M Mi i i id d d dd d d de e e el l l lb b b bu u u ur r r rg g g g T T T Th h h he...

Страница 194: ...em based on the system based on the appeara appearance of nce of the chromatogram refer the chromatogram refer to Table Capillary to Table Capillary Chromatograp Chromatographic Interpretations hic In...

Страница 195: ...umn to glass insert See Section 3 Decrease column temperature No sample peak or peak too small Leak at column inlet Syringe is leaking Broken column Injector is leaking Check for leaks Section 4 parag...

Страница 196: ...may be necessary to lift the detector crossover from the ion oven then heat the lines and crossover with a flame while purging with an inert gas Install an uncoated test column and repeat the tempera...

Страница 197: ...d or detector can mean an unstable system for at least a couple hours It can be more effective to have a closer look at the baseline itself first The baseline below 250 C Improvements in column techno...

Страница 198: ...FC Pressure ready time out 44 Front EFC Pressure Ready Time Out Alert Errora Unit not ready for 10 minutes Activated Safety Method 45 Middle EFC Pressure Ready Time Out Alert Errora Unit not ready for...

Страница 199: ...is used Electronics off all H2 flow set to 0 0 mL min Check zone 1 69 Zone 2 Open Sensor Error Zone 2 sensor not in use mis used Electronics off all H2 flow set to 0 0 mL min Check zone 2 70 Zone 3 Op...

Страница 200: ...unaway Error Electronics off all H2 flow set to 0 0 mL min Check zone 1 83 Zone 2 Thermal Runaway Error Electronics off all H2 flow set to 0 0 mL min Check zone 2 84 Zone 3 Thermal Runaway Error Elect...

Страница 201: ......

Страница 202: ...sensor Alert errors not reproducible Electronics off all H2 flow set to 0 0 mL min 429 Sampler Carrousel stuck on sensor Alert errors not reproducible Electronics off all H2 flow set to 0 0 mL min 43...

Страница 203: ...nce Error 455 N15V out of tolerance Error 456 P5V DAC out of tolerance Error 457 VREF1 out of tolerance Error 458 VREF0 out of tolerance Error Out of Tolerance cts_id 459 CTS1 out of tolerance Error 4...

Страница 204: ...c 482 Analogoutput buffer underrun Alert Buffer underrun 483 Analogoutput buffer overflow Alert Buffer overrun Notification Message 484 Analogoutput communication error Alert Notification Message 485...

Страница 205: ...software used in this Gas Chromatograph GNU General Public License is a free copy left license for software and other kinds of works The 450 GC is using version 2 6 18 of the Linux kernel provide by M...

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