D-3 user manual - Valco Instrument Instrument Company
Contents
1. 8 7 cm PACKED COLUMN ADAPTER l 23642 D3 _ 8 A PACKED COLUMN To prevent detector contamination we strongly recommend disconnecting the column from the detector during column bakeout procedures The D3 is optimized for packed columns The column tubing must be thoroughly cleaned and baked before the column is packed Even when the best care is taken in column tubing cleaning and in the support and stationary phase selection a new column will often bleed compounds resulting in a considerable increase in the detector baseline This initial bleed will usually be reduced to acceptable levels after the column is conditioned with clean carrier gas flow for several hours at the recommended bakeout temperature 1 2 Loosen and remove the knurled nut and plug of the capillary column adapter or remove the column ferrule and the column if one has been installed Use a 1 8 wrench to hold the liner that part of the adapter in which the column ferrule sits While the 1 8 wrench keeps the liner from rotating use a 1 4 wrench on the fitting body to loosen the adapter 1 2 turn Installation 15 3 Set aside the 1 8 wrench and completely remove the adapter from the column inlet 4 Screw the packed column adapter into the column inlet by hand Exercise caution as the tip of the adapter is very fragile Then tighten the adapter with a 1 4 wrench using an additional wrench on the flats2. 1 Make sure the on off valve on the helium cylinder is completely closed Screw the CGA fitting nut of the regulator into the helium cylinder Go beyond finger tight but do not tighten the nut all the way some leakage is required for the purging operation 2 Turn the output pressure regulating knob completely counterclockwise 3 Open the cylinder on off valve slightly and quickly close it again 4 Adjust the tightness of the regulator connecting nut to allow a pressure reduction of 690 kPa sec 100 psi sec With a new bottle the gauge should start out at about 14 MPa 2000 psi 5 When the pressure drops into the 1 4 3 4 MPa 200 500 psi range open the cylinder on off valve slightly and quickly close it again 6 Repeat Step 5 eight or ten times to be certain that all the air is purged On the final purge tighten the regulator connecting nut very securely as the pressure approaches the 2 1 3 4 MPa 300 500 psi range Installation 12 7 Open the cylinder valve to pressurize the regulator once again Close the valve and observe the needle of the high pressure gauge for 15 minutes If it doesn t move there is no critical leak on the high pressure side of the regulator CAUTION Never use leak detecting fluids on any part of this 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 external to 1 16 internal re
3. eee eeeeeeeeeeeenneeeeeeeeenaeeeeeeeeaeeeeeeeeenaeeeeeeeeenaeeeeeenenaaees 6 Installing and Configuring the FID Logic Board Agilent 6890 GG riiin A ath ede ell aa ieee eyes 8 Agilent 7890 GC ceeeeeceeecneeeeeneeeeeeeeeeeeaeeeeeeaeeeseeeeeeecaeeeseaeeeseeeeseeaeeete 8 Gas Connections aricii ete eins ena Ae ee eevee 11 Installing and Purging the Gas Regulator cccecceeeeeseeeeeeeeeeneeeteneees 11 Installing and Purging the Helium Purifier aeee 12 Connecting the Discharge Gas to the Detector ccceeeeeeeeeeeeeeeeees 12 Initial PowerUp aiena a diene ET ENE a ASEA 13 Capillary Column Connection c ccceeceeeeeeeneeeeeeaeeeeeeaeeeeenaeeeseaeeeseeaeeesenaeees 14 Packed Column Connection ssssssssessisseitesiresritsrirteirsrirtstntsrrntstnnnernnnnnnene 14 Testing for LEAKS 0 eeceeeeeeeeeeeeneeee eee eeenneeeeeeeeteaaeeeeeeeeeaaeeeeeeensnaaeeeeeeeniaaa 15 Mode Selection and Setup Helium lonization Mode eeceeeceeeeeeeneeeeeeeeeeneeeeeeeeenaeeeeeeeeeaaeeeeeeeeneeeeeeeeeaas 16 Selective Photoionization Mode cccccceeeeeeeeeeeeeeeeeesenaeeeeeeeeseaeeeseneeeee 16 TMWOUDIESHOOUING 2 225 EEEE E T ane eI TEAT E 18 WNA EE AAE A A AAEE EAEE A EE N A 20 Detector Performance Log sssssssrsessserrnnensrrnnnenrirrannenrtnnannennennannennennnnnennennannenna 21 This page intentionally left blank for printing purposes Introduction Description and Operating Principle The D3 is a non rad
4. phosphine nitric oxide carbon disulfide etc can be selectively detected using the appropriate photoionization mode Each dopant gas requires an additional helium purifier which must be purged and conditioned in the same manner as the purifier installed on the discharge gas supply If you are using more than one dopant we recommend use of a Valco multiposition stream selection valve so that no fittings have to be disconnected Not only is this convenient it keeps the system closed minimizing chances of contamination When changing from one dopant to another allow at least one hour for the old gas to be purged from the system 18 Troubleshooting High Background Current Baseline current falls to normal range lt 2000 pA Disconnect the column and cap the column inlet Baseline current is still high gt 2000 pA Check discharge Leaks in the fittings of the PDD plumbing Do a hydrogen leak test described on next page H Tighten leaking fittings The detector isn t leaking Check for column bleed Baseline current falls to snare normal range lt 2000 pA and or leaks in the GC setup gt 2000 pA color gt 2000 pA Leaks inside the detector cell itself Low Sensitivity Check background curr with column removed column inlet plugged Consult Valco No detectable leaks Baseline curr
5. temperature required for the intended analysis When the detector has reached the set temperature read and record the standing current 8 Install the column as illustrated on page 11 leaving the oven at ambient temperature Start carrier flow then read and record the standing current The difference between this reading and the one previous is the ionization of the combined impurities in and eluting with the carrier gas The smaller the difference the better the quality of the gas exiting the column 9 Set the column oven to the temperature required for the intended analysis When the oven reaches the set temperature read and record the standing current The difference with the previous reading is the ionization of the column bleed The smaller the difference the better the column is conditioned NOTE Some stationary phases will have a higher bleed than others but are still suitable for this detector However the lower the bleed the lower the chances of contaminating the detector cell From this point the standing current should be observed and logged after any system change In addition logging the standing current with and without the column on a regular basis is an effective monitor of system integrity leaktightness and cleanliness We also recommend tracking the internal standard quantity on column area count for sensitivity continuity Installation Capillary Column Connection If
6. com Detector Model _D 3 I Serial Number Date of purchase Date Operator Comments Column Detector Noise Sample Standing temp temp level current C C pA Initial power up IPU 100 IPU detector to analysis temp IPU column installed Ambient IPU column to analysis temp 21
7. of the column inlet to support the detector 5 Connect the 1 8 column to the packed column adapter with the EZRU21 reducing union supplied in the fittings kit Testing for Leaks It is critical for the system to be leak tight and an additional check at this point can save many headaches later on To test for leaks 1 Cap the tube and pressurize the entire system with helium to 138 kPa 20 psi 2 If the system does not hold pressure check all the fittings with an electronic helium leak detector DO NOT use leak detecting liquids 3 Tighten fittings as required 16 Mode Selection and Setup Helium Ionization Mode Since the PDHID mode provides a better indication of the cleanliness and the integrity leak tightness of the system that mode is utilized for initial testing and startup If the system is operating according to the parameters described thus far it is ready for operation in the PDHID mode Selective Photoionization Mode To maximize detector lifetime turn off the discharge power when the GC is not actually analyzing samples This is especially important in the Ar Kr PID mode Since the pulsed discharge detector is essentially a windowless helium photoionization detector changing the discharge gas from pure helium to helium doped with argon krypton or xenon changes the discharge emission profile This results in a change in the photon energy due to additional resonance atomic emissions and diat
8. or at the factory If repairs or replacements are to be made at the factory Buyer shall return the goods prepaid and bear all the risks of loss until delivered to the factory If Seller returns the goods they will be delivered prepaid and Seller will bear all risks of loss until delivery to Buyer Buyer and Seller agree that this Limited Warranty shall be governed by and construed in accordance with the laws of the State of Texas The warranties contained in this agreement are in lieu of all other warranties expressed or implied including the warranties of merchantability and fitness for a particular purpose This Limited Warranty supercedes all prior proposals or representations oral or written and constitutes the entire understanding regarding the warranties made by Seller to Buyer This Limited Warranty may not be expanded or modified except in writing signed by the parties hereto Detector Performance Log In addition to the occasions indicated in the Comments area of the table below see nitial Power Up page 13 the standing current should be observed and logged after any system change Logging the standing current with and without the column on a regular basis is also an effective monitor of system integrity leaktightness and cleanliness To check sensitivity continuity we recommend tracking the internal standard quantity on column area count Additional log pages can be down loaded from the support manuals section of www vici
9. rights that vary from state to state For a period of 365 calendar days from the date of shipment Valco Instruments Company Inc hereinafter Seller warrants the goods to be free from defect in material and workmanship to the original purchaser During the warranty period Seller agrees to repair or replace defective and or nonconforming goods or parts without charge for material or labor or at the Seller s option demand return of the goods and tender repayment of the price Buyer s exclusive remedy is repair or replacement of defective and nonconforming goods or at Seller s option the repayment of the price Seller excludes and disclaims any liability for lost profits personal injury interruption of service or for consequential incidental or special damages arising out of resuiting from or relating in any manner to these goods This Limited Warranty does not cover defects damage or nonconformity resulting from abuse misuse neglect lack of reasonable care modification or the attachment of improper devices to the goods This Limited Warranty does not cover expendable items This warranty is VOID when repairs are performed by a nonauthorized service center or representative For infor mation about authorized service centers or representatives write Customer Repairs Valco Instruments Company Inc P O Box 55603 Houston Texas 77255 or phone 713 688 9345 At Seller s option repairs or replacements will be made on site
10. NNECTION CONNECTION Figure 5 7890 FID logic board 6 Press the lt Config gt key then press lt Back det gt or lt Front Det gt corre sponding to the location where the PDD will be installed For this example we will select Back Det The display will read Configured or Unconftigured Ignore ready False B DET Signal FID 7 Press lt Mode Type gt The display will read CONFIGURE BACK DETECTOR Remove Module lt cursor is here 8 Press lt Enter gt to clear the existing configuration The display will read CAUTION Instrument power must be turned off and back on for set point to take effect 9 Do notturn off the GC instead press lt Enter gt The display will read CONFIGURE BACK DETECTOR Unconfigured lt cursor is here B Det Signal FID EPC4 Not Found A Det2 Not Found 10 Press lt Mode Type gt The display will read CONFIGURE BACK DETECTOR CPDET FID No Htr No EPC lt cursoris here CPDET FID Htr No EPC Installation 10 11 Scroll to select the second line and press lt Enter gt The display will read CAUTION Instrument power must be turned off and back on for set point to take effect 12 Do notturn off the GC instead press lt Enter gt The display should read CONFIGURE BACK DETECTOR Configured Channel Partner Ignore Ready False B det Signal FID 13 Turn off the GC and power it back up Verify the configuration by pressing lt Back Det gt The
11. VIGI Valco Instruments Co Inc Pulsed Discharge Detector Models D 3 I HP and D 3 I 7890 Instruction Manual Rev 1 15 North America South America and Australia Oceania contact Europe Asia and Africa contact Valco Instruments Co Inc VICI AG International 800 367 8424 sales Schenkon Switzerland 713 688 9345 tech Int 41 41 925 6200 phone 713 688 8106 fax Int 41 41 925 6201 fax valco vici com info vici ch This page intentionally left blank for printing purposes Table of Contents Introduction Description and Operating Principles 0 cccccceseeeceseeeeeeeeeeteneeeeeeeeeteneeeeeee 1 Safety Notes and Information c cccceceeeeeeeeeeeeeeeeeneeeeeeeeeeeeeeeeeeaeeeeeneeeenee 2 Symbols Installation Category Safety Components of the Detector System cccceeeeeeeeeeseeeeteneeeeeneeeeeeeeetetaeeeeee 3 System Requirements Components not Included with the Detector System ccccceceeeeeeeeeneees 4 SYSTEM Purity e eea ieee tives Sede a les Teena evden see 4 Gas Specifications ccccccccceececeeeeeeeeeeeeeeeeeeeeaeeeeeeeeeeseaaeeeseeeeeseneeeeseaeeessaas 5 Installation General Precautions cccceeccceeeeneeeeeeeeeeeeeeeeeteaeeeeeaeeeeeaeeetecaeeeseaeeeeteaeeeea 6 Checking the Firmware Version Agilent 6890 GC sancasvtvd iin ede aan wie Sai ee es 6 Agilent 7890 GC cceeeececeeceeeeeneeeeeeeeeeeeeaeeeeeaeeeeeeeeeseaeeeseaeeeseaeeeseeaeeeee 6 Mounting the Detector
12. age cable to the pulser module The electrometer and heater cables will be connected after the FID logic board is installed Installation 7 Figure 2 A D3 detector in the Back position on a 7890A CRO CAPTIVE SCREWS 4 DISCHARGE GAS INLET L 30 mL min 60 psi HEATER SENSOR X 5 TO D3 PULSER MODULE PD M2 oO ELECROMETER RIBBON CABLE COLUMN INLET CAPILLARY COLUMN ADAPTER Packed column adapter shown on page10 TO FID LOGIC BOARD Figure 3 Mounting and connecting the detector Installation 8 CAUTION A D 3 I HP will not work on a 7890 GC anda D 3 I 7890 will not work on a 6890 If you are not sure which model you have call the VICI detector department with the detector serial number Installing and Configuring the FID Logic Board Agilent 6890 GC units without EPC The D3 uses the electrometer portion of the Agilent FID logic board which must be configured to ignore the ignitor circuit 1 Plug the FID logic board into the GC main board at the location corresponding to the detector mounting position front or rear which you intend for the D3 Refer to the GC manual as required Tighten the detector card screw Figure 4 Connect the heater sensor cable to the main board and the electrometer cable to the interface board Push lt Config gt and scroll down to select In
13. ased packing or lubricating material is to be particularly avoided Pressure Regulators We recommend commercial ultra pure grade regulators with stainless steel diaphragms Regulators with diaphragms made of neoprene or other elastomers should never be used Introduction 5 Gas Specifications Detector Mode PDHID Ar PDPID Kr PDPID Xe PDPID Discharge gas 2 Ar in He 1 5 Kr in He 0 8 Xe in He Any gas including He which has an ionization potential greater than 12 eV x Any gas including He which has an ionization potential greater than 11 eV Purity Specifications e Helium discharge and carrier gas must have a minimum purity of 99 999 with lt 20 ppm Ne impurity For trace analysis of fixed gases we strongly recomment 99 9999 purity He with lt 0 5 ppm Ne e Ar PDPID mode 2 0 2 Ar in 99 999 He balance Kr PDPID mode 1 5 0 1 Kr in 99 999 He balance e Xe PDPID mode 0 8 0 2 Xe in 99 999 He balance 6 Installation General Precautions e Do not use plastic polymer or copper tubes for gas handling and interconnectons Use only stainless steel tubing with Valco gold plated ferrules e Do not turn the discharge power on until the helium discharge gas is flowing through the detector e Do not shut off or disconnect the discharge gas when the detector is hot even if the GC is turned off e Do not turn on the GC during detector installation Checking the Firmware Versi
14. display should read Back detector CP Temperature xX X Output XXXX Installation 11 Gas Connections Remember these three points discussed earlier 1 all surfaces that contact the gas stream must be glass or stainless steel 2 do not use copper tubing or brass fittings and 3 all tubes must be thoroughly cleaned and baked before use The installation instructions below assume that the detector discharge gas will be supplied from a nearby cylinder of helium of the proper purity If your installation is different you may need to modify the instructions appropriately A number of Valco fittings have been supplied in the fittings kit to handle different situations Since the distance from the helium supply to the GC varies from installation to installation we do not supply tubing to go from that point to the GC Figure 6 illustrates gas connections for the PD D3 I detector system Since the distance from the helium supply to the GC varies from installation to installation we do not supply tubing for that purpose TEE ZT1 TGA R 30F60P RESTRICTOR 30 mL min minimum DISCHARGE GAS S 99 999 He DISCHARGE GAS INLET ELECTRONIC PNEUMATIC CONTROL VENT VICI MINIATURE HELIUM PURIFER COLUMN INLET covuwin _ iNsECTOR j GAS CHROMATOGRAPH Figure 6 Gas connections for a PD D3 I system Installing and Purging the Gas Regulator
15. ducer EZR21 if it has a 1 4 male cone type outlet port install the Valco 1 4 external to 1 16 internal reducer EZR41 For other regulator outlet fittings a wide variety of Valco adapters is available 2 Remove the cap from the inlet tube of the Valco helium purifier and insert the tube fitting into the 1 16 reducer port Keep the outlet tube capped Use a 1 4 wrench to turn the nut one quarter turn past the point where the ferrule first starts to grab the tubing Do not remove the fitting When made up properly it should be leak tight 3 Turn the output pressure regulating knob clockwise until the gauge registers 345 KPA 50 psi 4 Allow five minutes for equilibration then turn the regulating knob all the way counterclockwise 5 Observe the needle of the output pressure gauge for 15 minutes There will be a slight initial drop but if it doesn t move after that consider that all the connections are tight 6 If necessary use an electronic leak detector to locate any leaks Ifa leak detector is not available tighten all the fittings including the output pressure guage and repressurize the system for another test CAUTION Never use leak detecting fluids on any part of this system 7 Upcap the outlet tube of the purifier and purge the system for 15 to 30 minutes at 60 80 mL min to eliminate air from the purifier getter material Connecting the Discharge Gas to the Detector 1 Connect the discharge
16. eaks 1 Check column flow 2 Check the column insertion position 10 3 cm for capillary columns 8 7 cm for packed columns 3 If there are still no peaks check to make sure that the GC is actually making an injection 4 If there are still no peaks consult Valco Troubleshooting 19 High Noise Level If the noise lievel is high 1 2 See if it improves with the GC fan turned off Check the column insertion position 10 3 cm for capillary columns 8 7 cm for packed columns 3 If the noise level is still high do a hydrogen leak test described below 4 If there are no leaks found or leaks are found and repaired and the noise level is still high consult Valco Performing a Hydrogen Leak Test A hydrogen leak test allows you to pinpoint loose fittings and leaks inside the detector 1 Connect a length of plastic tubing to a regulated hydrogen bottle Establish a flow of 5 10 ml min Hold the hydrogen outlet tube at a fitting connection for ten seconds while monitoring the baseline Tighten the fitting and test it again repeating as necessary until every connection has passed the ten second test Hold the hydrogen outlet close to the detector Do not insert the tube into any detector holes If a leak in the detector is indicated contact Valco 20 Warranty This Limited Warranty gives the Buyer specific legal rights and a Buyer may also have other
17. ection and Setup 17 Ar PDPID Changing the discharge gas from helium to a mixture of 2 argon in helium changes the photon energy level from the 17 13 5 eV range to the 11 8 9 8 eV range The argon emission consists of resonance radiation at 11 8 eV and 11 6 eV and the diatomic Ar emission in the range of 9 2 10 3 eV Except for fixed gases and a few organic compounds like CH IP 12 5 eV CH CN IP 12 2 eV and some fluro chloro hydro carbons the majority of organic compounds have ionization potentials lower than 11 8 eV Thus the Ar PDPID is nearly universal like the flame ionization detector but without the risks associated with the presence of an open flame and hydrogen Kr PDPID The recommended proportion is 1 4 Kr in He as the discharge gas The krypton emission consists principally of resonance lines at 10 6 eV and 10 1 eV The Kr PDPID can detect compounds with IP lt 10 6 eV which includes unsaturated and cyclic hydrocarbons alcohols aldehydes organic acids esters etc Xe PDPID The recommended proportion is 0 8 Xe in He as the discharge gas The xenon emission consists principally of resonance lines at 9 6 eV and 8 4 eV and can detect compounds with IP lt 9 6 like aromatics ethers alcohols aldehydes etc In addition to the specific compounds named in the three paragraphs above certain important inorganic compounds like ammonia hydrogen peroxide arsenic trichloride hydrogen sulfide arsine
18. ent is still high Consult Valco Baseline current falls to Snare normal range lt 2000 pA Baseline current is still high Consult Valco Possible bad carrier gas or empty He bottle Install a new bottle gt 2000 pA Baseline current falls to E normal range lt 2000 pA Baseline current is still high Consult Valco Background current remains high Remove column and condition it then run a sample High background current Normal background current gt 2000 pA lt 2000 pA Background current Check column inlet for increases leaks Tighten fittings Background current drops to normal range Run a sample Refer to Troubleshooting High Background Current Reinstall column and check background current Background current remains in normal range No Peaks Check column position according to drawing on p 14 and run a sample Sensitivity is in acceptable range Sensitivity is in acceptable range Sensitivity is still too low r Sensitivity is in acceptable range Sensitivity is still too low Remove column and bake detector at 300 C for four hours Install column and run a sample r Sensitivity is in acceptable range Sensitivity is still too low k Consult Valco If the background current is stable but there are no p
19. gas source to restrictor TGA R 30F60P and connect the restrictor to the detector inlet 2 Connect a flow measuring device to the vent and adjust the helium pressure to obtain a flow of 30 mL min Installation 13 Initial Power Up CAUTION Always make sure that discharge gas is flowing before heating and powering up the detector 1 Before installing the column set the gas flow to 30 ml min measured at the detector vent Let it flow for 15 minutes so that all air is purged from the helium purifiers 2 Plug in the helium purifiers and turn on the GC 3 Set the detector temperature to 100 C and allow time for the detector and helium purifiers to reach the set temperature 4 Plug the 24 VDC output from the power supply Il 23569 1 into the pulser module PD M2 5 Plug the power supply cord to a 100 250 VAC source and look through the hole in the detector housing to see if the discharge is on CAUTION During normal operation the detector pro duces ultraviolet energy UVA UVB some of which may be emitted Do not watch the arc without eye protection 6 Check the standing background current and record it in the Detector Performance Log on the last page of this manual Optimum range is 600 2000 pA at 100 C Lower current indicates a clean leak free system 7 The recommended detector temperature is 20 C above the column temperature with a minimum of 100 C Set the detector to the operating
20. ioactive pulsed discharge ionization detector PDID with models available for plug and play installation on the Agilent 6890 or 7890 GC A schematic representation of the detector is shown in Figure 1 The D3 utilizes a stable low power pulsed DC discharge in helium as the ionization source Elutants from the column flowing counter to the flow of helium from the discharge zone are ionized by photons from the helium discharge above Resulting electrons are focused toward the collector electrode by the two bias electrodes The principal mode of ionization is photoionization by radiation arising from the transition of diatomic helium He A Li to the dissociative 2He 1S ground state This is the well known Hopfield emission The photon energy from the He continuum is in the range of 13 5 eV to 17 7 eV The D3 is essentially non destructive 0 01 0 1 ionization and highly sensitive The response to organic compounds is linear over five orders of magnitude with minimum detectable quantities MDQs in the low picogram range The response to fixed gases is positive the standing current increases with MDGs in the low ppb range Detector response is universal except for neon which has an ionization potential of 21 56 eV Since this potential is close to the energy of the He metastable 19 8 eV but greater than the photon energy from the He continuum neon exhibits a low ionization efficiency and low detector response When a do
21. l adapters required for connection to the gas regulator e SS tubing to go from gas supply to GC e Flow measuring device System Purity Discharge Carrier Gas Considerations The performance of the detector is adversely affected by the presence of any impurities in the gas streams carrier discharge or dopant We recommend that a quality grade of helium 5 0 99 999 pure or better be used at all times Major gas suppliers offer research grade helium 99 9999 pure which is particularly low in fixed gas impurities and should give good results in a clean system but even the highest quality carrier gas may contain some water vapor and fixed gas impurities hence a helium purifier is included as part of the detector system The discharge gas should always be run through the helium purifier Whenever a new batch of discharge gas is received we recommend performing a blank GC analysis of the gas in the PDHID mode to detect and identify the presence of any impurities Gas purity requirements are specified on the next page Tubing Standards of cleanliness that are suitable for many GC applications may be totally inadequate for the sensitive PDHID PDPID work All surfaces that contact the gas stream must be glass or stainless steel Do not use copper tubing or brass fittings All tubes must be thoroughly cleaned and baked before use Flow Controllers The use of valves or flow controllers in which the gas stream is exposed to any polymer b
22. omic emissions from the rare gas added Thus a single detector can be operated in any of the three photoionization detector PID modes Ar Kr or Xe PID Doped helium is used rather than other pure gases in order to retain the benefits of the helium namely its transparency for Ar Kr an Xe resonance radiation and its efficient cooling of the electrodes Any problems associated with the presence of a window between the photon source and the ionization chamber are eliminated In most applications involving current commercial PIDs analyte condensation and decomposition on the window attenuate the lamp energy necessitating frequent cleaning and recalibration Custom gas blends for the pulsed discharge detector are available from leading gas suppliers at special prices Alternatively they may be form ulated on the spot by using appropriate fixed restrictors to mix appropriate amounts of pure helium and pure dopant through a tee Since all gas streams must pass through a Valco purifier the second option requires an additional purifier for each dopant This may still be more cost effective than requesting a custom blend of the more expensive Kr or Xe since the typical flow rate required for the pure dopant rare gas is about 0 3 1 mL min a small lecture bottle can last for a long time In either case the total discharge gas flow rate should be the same as specified in Connecting the Discharge Gas to the Detector on page 12 Mode Sel
23. on How do they know if they have a problem related to firmware version Will they get some message about incompatibility Agilent 6890 GC 1 Push lt Options gt and scroll down to select Diagnostics Press lt Enter gt 2 Select Instrument status and press lt Enter gt 3 Scroll down to read Version A 0x0x Successful operation of the D3 I HP requires either 6890 firmware version A 02 12 or higher or the GC s FID pneumatic control EPC If the EPC is used all it does is provide the detector title which remains FID Agilent 7890 GC When the GC is first powered on the display will read Agilent 7890 GC A 0x 0x Power on successful If the instrument is already on and displaying other information push lt Status gt and then lt Clear gt to display the message shown above The second line is the firmware version Successful operation of the D3 requires 7890 firmware version A 01 05 or higher If you experience problems contact Agilent technical support and request a firmware version compatible with Channel Partner detectors If you are running ChemStation please check with Agilent to determine that your version is compatible with Channel Partner detectors A software upgrade may be required Mounting the Detector 1 Place the D3 on the top of the GC in either the front or back detector position Figure 2 and tighten the four captive Torx T 20 screws in the detector pallet Figure 3 2 Connect the high volt
24. onents of the detector system are listed in Table 1 below Check the contents of the packages to verify that everything is present Contact the factory if anything is missing or damaged NOTE damaged shipments must remain with the original packaging for freight company inspection 3 Description Quantity Product number Detector assembly includes detector heater and electrometer for Agilent 6890 1 PD D3 I for Agilent 7890 1 PD D3 I 7890 Pulser module 1 PD M2 Pulser power supply 1 1 23569 1 Agilent FID board for Agilent 6890 1 I G1531 60020 for Agilent 7890 1 I G3431 60020 Helium purifier il HP2 Miniature helium purifier 1 HPM Fittings kit 1 PD KIT D3 Includes 1 32 polyimide ferrule 5 ZF 5V 1 16 gold plated ferrule 5 ZF1GP 0 25 0 44 mm polyimide column ferrule 5 FS 4 0 4 0 5 mm polyimide column ferrule 5 FS 5 1 16 union 2 ZU1 1 16 tee 1 ZT1 1 8 external to 1 16 internal reducer 2 EZR21 1 8 to 1 16 reducing union 2 EZRU21 1 32 external nut 1 EN 5KN Packed column adapter il 1 23642 D3 Restrictor 30 cc min 60 psi He 1 TGA R 30F60P Instruction manual 1 MAN PDD3 Table 1 Components of the D3 system Introduction 4 System Requirements Components Not Included with the Detector System e Helium 99 999 purity and other support gases e Ultra high purity grade gas pressure regulator with stainless steel diaphragm e Any specia
25. pant is added to the discharge gas the D3 also functions as a selective photoionization detector Suitable dopants include Ar for organic compounds Kr for unsaturated compounds or Xe for polynuclear aromatics GROUND PIN DISCHARGE REGION HIGH VOLTAGE HELIUM INLET SAPPHIRE INSULATORS CAPILLARY COLUMN COLLECTOR ELECTRODE VENT COLUMN INLET Figure 1 Schematic of the D 3 detector Introduction 2 Safety Notes and Information Symbols ATTENTION Refer to the manual Installation Category This equipment has been designed for installation category overvoltage category II pollution degree 2 It has been approved for use only in heavy industrial environments and may not be used in the residential commercial or light industrial environment Safety This instrument left the factory in a safe condition This instruction manual contains important information and warnings which must be followed by the user to insure safe operation and to retain the instrument in a safe condition Use only with an approved mains supply cord having a rating of 2A 250V or greater Do not use this equipment in a manner not specified herein CAUTION During normal operation the detector produces ultraviolet energy UVA UVB some of which may be emitted Do not watch the arc without eye protection Introduction Components of the Detector System Comp
26. strument Press lt Enter gt Select F det FID for front position or R det FID for rear position and push lt gt lt gt lt Mode Type gt Select Electrometer and press lt Enter gt HEATER SENSOR CABLE CONNECTOR FID BOARD SCREW FID LOGIC BOARD ELECTROMETER CABLE CONNECTOR Figure 4 6890 FID board To switch back to standard FID mode repeat the procedure and slect FID on the last step Agilent 7890 GC 1 Refer to the GC manual for instructions on removing access panels Install the FID logic board as illustrated in Figure 5 at the location corresponding to the detector mounting position front or back Secure the thumb screw at the top right corner FID logic board as shown in Figure 5 Connect the heater sensor cable and the electrometer ribbon cable to the Connect the appropriate F DET front or B DET back cable to the logic board The AUX DET1 cable is not be used with the VICI D3 detector and press lt Enter gt lt Off No gt key Press lt Options gt and use the scroll keys to select Keyboard amp Display Scroll to select Hard Configuration Lock Set it to OFF by pressing the Installation 9 MODEL D3 IN BACK POSITION FRONT OF 7890 HEATER CABLE CONNECTIONS THUMBSCREW FID LOGIC BOARD FOR FRONT POSITION ELECTROMETER CABLE CONNECTIONS FID LOGIC BOARD FOR BACK POSITION B DET CABLE F DET CABLE CO
27. the capillary column adapter is installed in the column inlet 1 2 Make a mark on the column 10 3 cm from the end Remove the knurled nut and plug from the capillary column adapter in the column inlet at the bottom of the detector Figure 3 Slide the nut over the end of the column followed by the appropriate column ferrule FS 4 or FS 5 or ZF 5V for megabore Seat the ferrule in the detail of the column adapter and begin sliding the column through the capillary column adapter and into the column inlet Get the nut started on the threads and tighten it until you feel it contact the ferrule then back off half a turn Slide the column into the column inlet until the mark is flush with the surface of the knurled nut and secure the column in the adapter by tightening the knurled nut finger tight only If the capillary column adapter has been removed reinstall it 1 3 Unscrew the liner as far as it will go then screw the fitting body into the column inlet fingertight While using a 1 8 wrench to prevent rotation of the liner the part with the seat for the column ferrule use a 1 4 wrench to tighten the body of the adapter until the ferrule has sealed The liner will deform if it rotates Proceed to Step 1 above Packed Column Connection 14 fr COLUMN INLET CAPILLARY COLUMN Y ADAPTER IZERA1 5 10 3cm 4 COLUMN FERRULE NUT CAPILLARY COLUMN ON COLUMN INLET
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