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Installing GC Columns

Conditioning a column before it is installed into the GC/MSD
interface is essential

A small portion of the capillary column stationary phase is often carried
away by the carrier gas. This is called column bleed. Column bleed deposits
traces of the stationary phase in the MSD ion source. This decreases MSD
sensitivity and makes cleaning of the ion source necessary.

Column bleed is most common in new or poorly cross-linked columns. It is
much worse if there are traces of oxygen in the carrier gas when the column
is heated. To minimize column bleed, all capillary columns should be condi-
tioned

before

they are installed in the GC/MSD interface.

Conditioning ferrules is also beneficial

Heating ferrules to their maximum expected operating temperature a few
times before they are installed can reduce chemical bleed from the ferrules.

Tips and hints

• Note that the column installation procedure is different from that for

all

other Hewlett-Packard mass spectrometers and MSDs. Using the
procedure from another instrument will not work.

• For optimal sensitivity performance, install your caapillary column

without

using the installation tool.

• You can remove old ferrules from column nuts with an ordinary push pin.

• Always use carrier gas that is at least 99.999% pure.

• Because of thermal expansion, new ferrules may loosen after heating and

cooling a few times. Check for tightness after two or three heating cycles.

• Always wear clean gloves when handling columns, especially the end that

will be inserted into the GC/MSD interface.

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Summary of Contents for 5973

Page 1: ...H Hardware Manual HP 5973 Mass Selective Detector ...

Page 2: ...entions Cautions Cautions call attention to procedures which if not correctly performed or adhered to could result in damage to the instrument Warnings Warnings call attention to procedures which if not correctly performed or adhered to could result in personal injury Part Numbers In this manual Hewlett Packard part numbers are generally listed in parentheses after the name of the part or in table...

Page 3: ...HP 5973 Mass Selective Detector Hardware Manual ...

Page 4: ...he MSD is through the data system The data system features Hewlett Packard MSD ChemStation software It includes programs to calibrate tune the MSD acquire data and analyze data Tuning programs adjust voltages in the ion source calibrate mass assign ments and control the scanning of the analyzer Data acquisition programs allow you to monitor the total ion chromato gram TIC automatically storing the...

Page 5: ...iode gauge tube With an HP 59864B Gauge Controller the tube can be used to measure pressure high vacuum in the vacuum manifold Installation and operation of the gauge controller is described in this manual The gauge controller is required for chemical ionization CI operation HP 6890 Series Gas Chromatograph HP 5973 Mass Selective Detector ...

Page 6: ...e procedures Chapter 5 describes operation of the components of the vacuum system Chapter 6 describes the GC MSD interface Chapter 7 describes operation of the ion source mass filter and detector Chapter 8 describes the electronics that control the MSD Chapter 9 contains illustrated parts identification and part numbers To report errors in this manual please send e mail to chem sid hp com For upda...

Page 7: ...monitors for MSD temperature and vacuum status 38 To set the MSD analyzer temperatures 40 To set the interface temperature from the ChemStation 42 To monitor high vacuum pressure 44 To measure column flow linear velocity 46 To calculate column flow 47 To tune the MSD 48 To set the interface temperature from an HP 6890 GC 49 To remove the MSD covers 50 Upper MSD cover 50 Lower MSD cover 50 To vent ...

Page 8: ... drift shorter 73 Retention times for all peaks drift longer 73 Poor sensitivity 74 Poor Repeatability 74 Mass spectral symptoms 75 Isotopes are missing or isotope ratios are incorrect 75 High background 75 High abundances at m z 18 28 32 and 44 or at m z 14 and 16 75 Mass assignments are incorrect 76 Peaks have precursors 76 Peak widths are inconsistent 76 Relative abundance of m z 502 is less th...

Page 9: ... HED supply 85 Difficulty with the high vacuum pump 85 Diffusion pump 85 Turbomolecular pump 86 Foreline pressure has exceeded 300 mTorr 86 Internal MS communication fault 86 Lens supply fault 86 Log amplifier ADC error 86 No peaks found 86 Temperature control disabled 87 Temperature control fault 87 The high vacuum pump is not ready 87 The system is in standby 87 The system is in vent state 88 Th...

Page 10: ...ge 128 To remove the calibration valve 130 To reinstall a calibration valve 132 To replace the fan for the high vacuum pump 134 To remove the triode gauge tube 136 To reinstall a triode gauge tube 138 To lubricate the side plate O ring 140 To lubricate the vent valve O ring 142 Maintaining the analyzer 144 To remove the ion source 146 To disassemble the ion source 148 To clean the ion source 150 T...

Page 11: ... pump MSD vacuum system 186 Turbo pump MSD vacuum system 187 Diffusion pump vacuum manifold 188 Turbo pump vacuum manifold 189 Side plate 190 Vacuum seals 192 Face seals 192 KF NW seals 192 Compression seals 192 High voltage feedthrough seal 193 Foreline pump 194 Foreline gauge 196 Diffusion pump and fan 198 Turbomolecular pump and fan 202 Calibration valve and vent valve 204 Calibration valve 204...

Page 12: ...r 221 Drawout plate and cylinder 222 Ion focus 222 Entrance lens 222 Entrance lens offset 222 Entrance lens gain 222 Mass filter 223 AMU gain 223 AMU offset 224 219 width 224 DC polarity 225 Mass axis gain 225 Mass axis offset 225 Quadrupole maintenance 226 Detector 227 Detector focus lens 227 High energy dynode 227 Electron multiplier horn 227 Analyzer heaters and radiators 230 ...

Page 13: ...Remote start connector 245 I O HP IB connector 245 HP IB address switch 245 High vacuum signal HIVAC SIGNAL connector 246 High vacuum power HIVAC POWER connector 246 Power cord receptacle 246 Foreline pump power cord receptacle 246 Primary fuses 246 Interfacing to external devices 248 Remote control processor 248 Remote start signals 248 System ready 249 Start run input 249 Status display and powe...

Page 14: ...14 Contents Chapter 9 Parts Electronics 256 Vacuum system 260 Analyzer 268 GC MSD interface 274 Consumables and maintenance supplies 276 ...

Page 15: ...prepare a capillary column for installation 20 To install a capillary column in a split splitless inlet 22 To condition a capillary column 24 To install a capillary column without the installation tool 26 To install a capillary column using the installation tool 28 ...

Page 16: ... 0 20 mm id or 0 25 mm id can be installed directly into the GC MSD interface Do not exceed recommended column flow Wide bore columns 0 32 mm id and megabore columns 0 53 mm id at least 100 meters long can be installed directly into the GC MSD interface of the turbo pump MSD Flow restrictions apply Wide bore and megabore columns cannot be used with the diffusion pump MSD This information is summar...

Page 17: ...0 37 3 2 0 15 22 0 2 0 15 30 3 4 0 0 250 60 32 3 2 0 30 18 5 2 0 15 8 8 2 0 15 18 5 4 03 0 323 60 25 9 4 03 wide bore 30 14 0 4 03 15 5 6 4 03 0 533 100 4 41 4 03 megabore 75 1 854 4 0 1 Nominal dimensions 2 Calculated values at 70 C with vacuum compensation turned on 3 Acceptable for turbo pump MSD only 4 Not acceptable flow too highor headpressure toolow for accurate control ...

Page 18: ...Conditioning ferrules is also beneficial Heating ferrules to their maximum expected operating temperature a few times before they are installed can reduce chemical bleed from the ferrules Tips and hints Note that the column installation procedure is different from that for all other Hewlett Packard mass spectrometers and MSDs Using the procedure from another instrument will not work For optimal se...

Page 19: ...KH 06 DQG WKH 06 KDV EHHQ SXPSHG GRZQ I WKH YDFXXP SXPSV DUH RII K GURJHQ ZLOO DFFXPXODWH LQ WKH 06 DQG DQ H SORVLRQ PD RFFXU 5HDG WKH GURJHQ DUULHU DV 6DIHW XLGH EHIRUH RSHUDWLQJ WKH 06 ZLWK K GURJHQ FDUULHU JDV 5 1 1 OZD V ZHDU VDIHW JODVVHV ZKHQ KDQGOLQJ FDSLOODU FROXPQV 8VH FDUH WR DYRLG SXQFWXULQJ RXU VNLQ ZLWK WKH HQG RI WKH FROXPQ ...

Page 20: ... 8650 0029 Inlet column nut 5181 8830 Magnifying glass Septum may be old used inlet septum 1 Slide a septum column nut and conditioned ferrule onto the free end of the column The tapered end of the ferrule should point away from the column nut 2 Use the column cutter to score the column 2 cm from the end 3 Break off the end of the column Hold the column against the column cutter with your thumb Br...

Page 21: ...1 Installing GC Columns To prepare a capillary column for installation 21 Column cutter Ferrule Inlet column nut Septum Capillary column ...

Page 22: ...re the column for installation page 20 2 Position the column so it extends 4 to 6 mm past the end of the ferrule 3 Slide the septum to place the nut and ferrule in the correct position 4 Insert the column in the inlet 5 Slide the nut up column the to the inlet base and finger tighten the nut 6 Adjust the column position so the septum is even with the bottom of the column nut 7 Tighten the column n...

Page 23: ...1 Installing GC Columns To install a capillary column in a split splitless inlet 23 Reducing nut Ferrule not visible Inlet column nut Septum Capillary column Insulation cup 4 to 6 mm ...

Page 24: ... the carrier gas to flow for several hours 5 Return the GC oven temperature to a low standby temperature See Also For more information about installing a capillary column refer to the Hewlett Packard application note Optimizing splitless injections on your GC for high performance MS analysis publication number 5091 4587E 5 1 1 R QRW FRQGLWLRQ RXU FDSLOODU FROXPQ ZLWK K GURJHQ GURJHQ DFFXPXODWLRQ L...

Page 25: ...1 Installing GC Columns To condition a capillary column 25 ...

Page 26: ... optimal sensitivity performance 1 Condition the column page 24 2 Vent the MSD page 52 and open the vacuum manifold page 54 Be sure you can see the end of the GC MSD interface 3 Slide an interface nut and ferrule onto the free end of the GC column 4 Slide the column into the GC MSD interface until you can pull it out through the vacuum manifold 5 Break 1 cm off the end of the column page 20 Do not...

Page 27: ...ut the installation tool 27 9 Tighten the nut 1 4 to 1 2 turn Check tightness after one or two heat cycles Vacuum manifold GC MSD interface MSD end GC side panel Oven wall Interface column nut GC MSD interface GC end Interface cover Column MSD GC oven 1 to 2 mm ...

Page 28: ...ormance see To install a capillary column without the installation tool 26 1 Slide a septum interface column nut and conditioned ferrule onto the free end of the column The tapered end of the ferrule should point toward the nut 2 Insert the column into the column installation tool Slide the column through until the end extends past the end of the tool 3 Cut 1 cm off the end of the column page 20 4...

Page 29: ...olumn into the GC MSD interface 10 Tighten the nut 1 4 to 1 2 turn Check tightness after one or two heat cycles Column installation tool Interface column nut Column 1 to 2 mm Interface ferrule Septum 8 7 2 1 The column installation tool must be kept clean to prevent contaminating the column and the ion source Keep it in its storage tube and clean it by flushing with methanol after each use ...

Page 30: ...30 ...

Page 31: ...rature from the ChemStation 42 To monitor high vacuum pressure 44 To measure column flow linear velocity 46 To calculate column flow 47 To tune the MSD 48 To set the interface temperature from an HP 6890 GC 49 To remove the MSD covers 50 To vent the MSD 52 To open the vacuum manifold 54 To close the vacuum manifold 56 To pump down the MSD 58 To connect the optional gauge controller 60 To move or s...

Page 32: ...The vent valve must be closed the knob turned all the way clockwise All other vacuum seals and fittings must be in place and fastened correctly The the front side plate screw must be secure but not over tight The MSD is connected to a grounded power source The GC MSD interface extends into the GC oven A conditioned capillary column is installed in the GC inlet and in the GC MSD interface The GC is...

Page 33: ...plays turbo pump motor speed Each MSD is equipped with a triode gauge tube If your MSD is also equipped with an HP 59864B Gauge Controller the triode gauge can measure the pressure in the vacuum manifold The high vacuum pressure measured by the triode gauge cannot be monitored through the data system It is dis played on the gauge controller 5 1 1 7KH H KDXVW IURP WKH IRUHOLQH SXPS FRQWDLQV VROYHQW...

Page 34: ...onic pneumatic control EPC set to Const Flow constant flow the same column flow is be maintained regard less of oven temperature The MSD can be used to measure actual column flow You inject a small amount of air or other unretained chemical and time how long it takes to reach the MSD With this time you can calculate the column flow The data system aids in venting A program in the data system guide...

Page 35: ...DV D FDUULHU JDV WKH FDUULHU JDV IORZ PXVW EH RII EHIRUH WXUQLQJ RII WKH 06 SRZHU I WKH IRUHOLQH SXPS LV RII K GURJHQ ZLOO DFFXPXODWH LQ WKH 06 DQG DQ H SORVLRQ PD RFFXU 5HDG WKH GURJHQ DUULHU DV 6DIHW XLGH EHIRUH RSHUDWLQJ WKH 06 ZLWK K GURJHQ FDUULHU JDV 8 7 2 1 1HYHU vent the MSD by allowing air in through either end of the foreline hose Use the vent valve or remove the column nut and column 8 ...

Page 36: ...e Load MS Tune File dialog box 3 Analyzer temperatures and vacuum status are displayed in the Zones field Unless you have just begun the pumpdown process the foreline pressure should be less than 300 mTorr or the turbo pump should be running at least 80 speed MSD heaters remain off as long as the diffusion pump is cold or the turbo pump is operating at less than 80 Normally the foreline pressure w...

Page 37: ...2 Operating the MSD To view MSD analyzer temperature and vacuum status 37 ...

Page 38: ...o not match your MSD ChemStation software refer to the manuals and online help supplied with the software for more information 1 Select MS Monitors from the Instrument menu 2 In the Edit MS Monitors box under Type select Zone 3 Under Parameter select MS Source and click Add 4 Under Parameter select MS Quad and click Add 5 Under Parameter select Foreline or TurboSpd and click Add 6 Click OK The new...

Page 39: ...2 Operating the MSD To set monitors for MSD temperature and vacuum status 39 ...

Page 40: ...menu 2 Select the tune file you plan to use with your method from the Load MS Tune File dialog box 3 Select Temperatures from the MoreParams menu 4 Type the desired Source and Quad mass filter temperatures in the setpoint fields and click OK Recommended settings for operation are Source 230 C Quad 150 C The GC MSD interface ion source and quadrupole heated zones interact The analyzer heaters may n...

Page 41: ...2 Operating the MSD To set the MSD analyzer temperatures 41 ...

Page 42: ...hat MSD is selected under Type and Thermal Aux 2 is selected under Aux Channel 4 Turn the heater on and type the setpoint in the Next C column Do not set temperature ramps 5 The typical setpoint is 280 C The limits are 0 C and 350 C A setpoint below ambient temperature turns off the interface heater 6 Click Apply to download setpoints or click OK to download setpoints and close the window 7 To mak...

Page 43: ...2 Operating the MSD To set the interface temperature from the ChemStation 43 ...

Page 44: ...k The triode gauge tube can measure pressures between approximately 8 10 3 and 3 10 6 Torr The gauge controller is calibrated for nitrogen but all pressures listed in this manual are for helium The largest influence on operating pressure is the carrier gas column flow The following table lists typical pressures for various helium carrier gas flows These pressures are approximate and will vary from...

Page 45: ...e approximately 8 10 3 Torr the gauge controller will turn off the triode gauge tube The gauge tube does not turn back on automatically Table 2 Typical MSD pressure readings for various helium carrier gas flow rates Diffusion pump MSD Column flow ml min Triode gauge reading Torr Foreline gauge reading Torr 1 0 5 0 10 5 40 1 5 7 5 10 5 53 2 0 1 0 10 5 66 Turbo pump MSD Column flow ml min Triode gau...

Page 46: ...ar velocity Average linear velocity cm sec where L length of the column in meters t retention time in seconds Be sure to account for any pieces of column broken off A 1 meter section missing from a 25 meter column can yield a 4 error 6 Use this value to verify the MSD ChemStation flow calculations page 47 If the numbers disagree click the Change button to calibrate the column dimen sions 7 To calc...

Page 47: ...nstrument Control view click the Columns icon 2 Check that the correct column dimensions are entered 3 Type the desired value in the pressure field 4 If the Average Velocity displayed is different from that obtained on page 46 click the Change button to calibrate the column dimensions ...

Page 48: ...nment and abundance without changing ion ratios Always tune the MSD with the same column flow and the same analyzer temperatures that will be used for data acquisition 3 Wait for the tune to complete and to generate the report Save your tune reports To view history of tune results select View Tunes under the Qualify menu 4 To manually tune your MSD or to perform special autotunes select Manual Tun...

Page 49: ...al setpoint is 280 C The limits are 0 C and 350 C A setpoint below ambient temperature turns off the interface heater 4 Press the Enter key to download the new setpoint If you want the new setpoint to become part of the current method click Save under the Method menu Otherwise the first time a method is loaded all the set points in the method will overwrite those set from the GC keyboard 8 7 2 1 N...

Page 50: ... upper MSD cover and lift up enough to disengage the front latch 2 Reach back and grasp the back edge of the upper MSD cover 3 Pull forward to disengage the spring latch It may take a firm pull to disengage the latch To reinstall the upper MSD cover reverse these steps Lower MSD cover 1 Remove the upper MSD cover 2 Remove the 3 screws that hold the lower MSD cover in place 3 Move the cover left sl...

Page 51: ...2 Operating the MSD To remove the MSD covers 51 Upper cover Lower cover ...

Page 52: ...d the GC oven The pro gram turns off the analyzer heaters and the high vacuum pump The software will prompt you when it is safe to switch off the power 4 When prompted turn off the MSD power switch 5 Unplug the MSD power cord 6 Remove the upper MSD cover page 50 7 Turn the vent valve knob counterclockwise only 1 4 to 3 4 turns to admit air into the vacuum manifold Do not turn the knob too far Be s...

Page 53: ...t the MSD 53 Vent valve knob 5 1 1 W DQDO HU SDUWV DUH VWLOO KRW HQRXJK WR EXUQ EDUH VNLQ R QRW KDQGOH KRW SDUWV 8 7 2 1 Always wear clean gloves while handling any parts that go inside the vacuum manifold YES NO Vent valve knob ...

Page 54: ...ened during shipping The front side plate thumbscrew should only be fas tened for CI operation or if hydrogen or other flammable or toxic substances are used for carrier gas 8 7 2 1 Electrostatic discharges to analyzer components are conducted to the side board where they can damage sensitive components Wear a grounded anti static wrist strap and take other anti static precautions see page 100 bef...

Page 55: ...not tighten Source power cable Side board control cable Front thumbscrew Side plate 8 7 2 1 If you feel resistance stop Do not try to force the side plate open Applying force will ruin the side plate Verify that MSD is vented Verify that both the front and rear side plate screws are completely loose ...

Page 56: ...control cable and source power cable to the side board 5 Make sure the vent valve is closed 6 Pump down the MSD page 58 7 Gently hand tighten the front side plate thumbscrew This is only necessary for CI MSDs or if hydrogen or other flammable or toxic sub stance is used for carrier gas 8 Once the MSD has pumped down reinstall the upper MSD cover Wait until after pumpdown to reinstall the upper MSD...

Page 57: ...2 Operating the MSD To close the vacuum manifold 57 Rear thumbscrew do not tighten Source power cable Side board control cable Front thumbscrew Side plate ...

Page 58: ... valve or the sideplate 4 Click OK Within 10 to 15 minutes the diffusion pump should be hot or the turbo pump speed up to 80 If the MSD does not pump down correctly see the online help for information on troubleshooting air leaks and other vacuum problems 5 1 1 0DNH VXUH RXU 06 PHHWV DOO WKH FRQGLWLRQV OLVWHG LQ WKH LQWURGXFWLRQ WR WKLV FKDSWHU SDJH EHIRUH VWDUWLQJ XS DQG SXPSLQJ GRZQ WKH 06 DLOXU...

Page 59: ...etpoints are stored in the current autotune u file 6 After the message Okay to run appears wait two hours for the MSD to reach thermal equilibrium Data acquired before the MSD has reached thermal equilibrium may not be reproducible 7 Reinstall the MSD top cover The top cover was removed during the vent procedure 8 7 2 1 Do not turn on any heated zones until carrier gas flow is on Heating a column ...

Page 60: ...cal outlet If you wish to share one controller among MSDs obtain one cable for each instru ment Leave a cable connected to the triode gauge tube on each MSD This will avoid having to vent the MSD before connecting the controller 5 1 1 1HYHU FRQQHFW RU GLVFRQQHFW WKH FDEOH IURP WKH WULRGH JDXJH WXEH ZKLOH WKH 06 LV XQGHU YDFXXP 5LVN RI LPSORVLRQ DQG LQMXU GXH WR EURNHQ JODVV H LVWV 8 7 2 1 DoQRW us...

Page 61: ...2 Operating the MSD To connect the optional gauge controller 61 Triode gauge tube Triode gauge cable Triode gauge cable Gauge controller Power cord ...

Page 62: ... away from the GC page 112 Unplug the GC MSD interface heater cable from the GC 6 Remove the upper MSD cover page 50 7 Tighten the side plate thumbscrews to finger tight 8 Plug the MSD power cord in 9 Switch the MSD on to establish a rough vacuum Verify that the foreline pressure is below 300 mTorr or the turbo pump speed greater than 50 10 Switch the MSD off 11 Reinstall the upper MSD cover 12 Di...

Page 63: ...moved with the MSD Make sure the MSD remains upright and is never tipped on its side or inverted Rear side plate thumbscrew Front side plate thumbscrew 8 7 2 1 The MSD must remain upright at all times If you need to ship your MSD to another location contact your Hewlett Packard service representative for advice about packingand shipping ...

Page 64: ...bo pump but the cooling fans and foreline pump stay on 4 After 45 minutes turn off the MSD power switch 5 Unplug the MSD power cord 6 Reconnect the HIVAC POWER cable 7 Remove the upper MSD cover page 50 8 Turn the vent valve knob counterclockwise to admit air into the vacuum manifold Do not remove the knob Be sure to retighten the knob before pumping down See Also To open the vacuum manifold page ...

Page 65: ...ow to identify the symptoms and causes of problems in your MSD General symptoms 68 Chromatographic symptoms 70 Mass spectral symptoms 75 Pressure symptoms 79 Temperature symptoms 82 Error messages 84 Air leaks 89 Contamination 90 ...

Page 66: ...easiest to check and correct This section is only a quick reference No corrective actions are listed for the possible causes for each symptom For more extensive troubleshooting information see the Troubleshooting HP 5973 MSD section in the online help of the MSD ChemStation software The online troubleshooting pro vides more explanation and in many cases corrective actions 5 1 1 7KLV FKDSWHU GRHV Q...

Page 67: ...3 Troubleshooting the MSD 67 If the material in this chapter and in the online help proves insufficient to help you diagnose a problem contact your Hewlett Packard service repre sentative ...

Page 68: ...r supply is not working correctly MSD does not turn on This refers to a condition in which nothing happens when the MSD is switched on The foreline pump does not start The cooling fan for the high vacuum pump does not turn on The status LEDs on the front of the MSD do not light Disconnected MSD power cord No voltage or incorrect voltage at the electrical outlet Failed primary fuses MSD electronics...

Page 69: ...control card When this occurs the status LEDs will all light for a few seconds and then begin to operate normally leaving the power LED on and the others off If the sta tus LEDs do not stop blinking or if the status LEDs are all blinking at a time other than startup one of the following may be the cause Temporary power failure interrupted communications Bad connection between the MSD and the data ...

Page 70: ...d If repeatability is poor also apply to mass spectral data No peaks If an analysis shows no chromatographic peaks only a flat baseline or minor noise run one of the automated tune programs If the MSD passes tune the problem is most likely related to the GC If the MSD does not pass tune the problem is most likely in the MSD Passes tune Incorrect sample concentration No analytes present Syringe mis...

Page 71: ...ion Bad detector wiring connection Failed electron multiplier horn Peaks are tailing Active sites in the sample path Injection is too large Incorrect injection port temperature Insufficient column flow GC MSD interface temperature is too low Ion source temperature is too low Peaks are fronting Column film thickness mismatched with analyte concentration column overload Initial oven temperature is t...

Page 72: ... Column bleed Other contamination Baseline is high Column bleed Other contamination Electron multiplier voltage is too high Baseline is falling A falling baseline indicates contamination is being swept away Wait until the base line reaches an acceptable level Common causes include Residual water air and water from a recent venting Column bleed Septum bleed Splitless injection time too long inlet i...

Page 73: ...the GC that would prevent the GC from operating Retention times for all peaks drift shorter Column has been shortened Initial oven temperature was increased Column is getting old Retention times for all peaks drift longer Column flow has been reduced Initial oven temperature was decreased Active sites in the sample path Leaks in the injection port This could cause a fault condition in the GC that ...

Page 74: ...cessive pressure in the MSD Dirty ion source Air leak Poor filament operation Detector HED electron multiplier is not working correctly Incorrect mass filter polarity This could cause a fault condition in the GC that would prevent the GC from operating Poor Repeatability Dirty syringe needle Dirty injection port Leaking injection port Injection is too large Loose column connections Variations in p...

Page 75: ...Chromatographic symptoms If sensitivity is poor and If repeatability is poor also apply to mass spectra Isotopes are missing or isotope ratios are incorrect Peaks are too wide or too narrow Scan speed is too high scan mode Dwell time is too short SIM mode Electron multiplier voltage is too high Repeller voltage is too high High background Dirty ion source High background Pressure in the vacuum man...

Page 76: ...the size of the precursors for the tune masses Small precur sors are not unusual There are no specifications for acceptable or unacceptable precursor size If the precursors are unacceptably large for your application one of the following may be responsible Repeller voltage is too high Peaks are too wide Incorrect dc polarity on the quadrupole mass filter Dirty quadrupole mass filter Peak widths ar...

Page 77: ...es Sensitivity at high masses can be excellent even if the relative abundance of m z 502 is near 3 If your MSD produces low absolute abundances at high masses refer to the symptom High mass sensitivity is poor Tune programs other than autotune have different relative abundance targets The DFTPP and BFB target tune programs tune the HP 5973 MSD to achieve about a 0 8 ratio of m z 502 69 Tune progra...

Page 78: ...relative abundance percentage of m z 502 to m z 69 Sensitivity at high masses can be excellent even if the relative abundance of m z 502 is low Wrong tune program Wrong tune file Repeller voltage is too low Not enough time for the MSD to warm up and pump down Vacuum manifold pressure is too high Column carrier gas flow is too high Poor filament operation Dirty ion source Air leak Incorrect dc pola...

Page 79: ...he vacuum manifold pressures can only be measured if your system is equipped with the optional gauge controller Foreline pressure is too high If the pressure you observe is above 100 mTorr or if the pressure you observe for a given column flow has increased over time check the following Column carrier gas flow is too high Air leak usually the sideplate is not pushed in or vent valve is open Foreli...

Page 80: ...ck for the following Column carrier gas flow is too low Column plugged or crushed by overtightened nut Empty or insufficient carrier gas supply Bent or pinched carrier gas tubing These could create a fault condition in the GC that would prevent the GC from operating Gauge controller displays 9 9 9 and then goes blank This indicates the pressure in the vacuum manifold is above 8 10 3 Torr Solvent p...

Page 81: ...ing the MSD Pressure symptoms 81 Power indicator on the gauge controller does not light Unplugged gauge controller power cord Incorrect or inadequate line voltage at the electrical outlet Failed gauge controller fuse ...

Page 82: ...ntrolled by the MSD The GC MSD interface is powered and controlled by the GC Ion source will not heat up High vacuum pump is off or has not reached normal operating conditions Incorrect temperature setpoint Ion source has not had enough time to reach temperature setpoint Ion source heater cartridge is not connected Ion source temperature sensor is not connected Ion source heater failed burned out ...

Page 83: ...perature sensor failed Source power cable is not connected to the sideboard MSD electronics are not working correctly These will cause an error message GC MSD interface will not heat up Incorrect setpoint Setpoint entered in wrong heated zone GC MSD interface has not had enough time to reach temperature setpoint GC is off GC experienced a fault and needs to be reset GC MSD interface heater sensor ...

Page 84: ...ss Enter The corresponding error message s will appear Some error messages are latched These messages remain active in your data system even if the condition that caused the message has corrected itself If the cause is removed these messages can be removed by checking instrument status through the data system Difficulty in mass filter electronics Pressure in the vacuum manifold is too high RFPA is...

Page 85: ...ctor and the MSD electronics Detector is not working correctly MSD electronics are not working correctly Difficulty with the high vacuum pump In an MSD equipped with a diffusion pump this indicates the diffusion pump became too hot In an MSD equipped with a turbomolecular pump this indicates the pump failed to reach 50 of full speed in a preset time or experienced a fault You must switch the MSD o...

Page 86: ...ressure gauge Excessive carrier gas flow typically 5 ml min Excessive solvent volume injected Large vacuum leak Collapsed or kinked foreline hose Foreline pump is not working correctly Foreline gauge is not working correctly Internal MS communication fault MSD electronics are not working correctly Lens supply fault Electrical short in the analyzer MSD electronics are not working correctly Log ampl...

Page 87: ...iled Heater voltage is too low Temperature zone has timed out heater failed bad heater wiring or loose temperature sensor Problem with the temperature control electronics The high vacuum pump is not ready Diffusion pump is on but has not had enough time 10 15 minutes to reach its normal operating temperature Turbomolecular pump is on but has not had enough time 5 10 minutes to reach 80 of its norm...

Page 88: ... cartridge has failed MSD electronics are not working correctly There is no emission current Filament is not connected properly Filament has failed MSD electronics are not working correctly There is not enough signal to begin tune Poor mass axis calibration Amu gain or offset is too high Calibration vial is empty or almost empty Excessive pressure in the vacuum manifold Air leak Electron multiplie...

Page 89: ... m z 502 this varies with the tune program used Leaks can occur in either the GC or the MSD The most likely point for an air leak is a seal you recently opened In the GC most leaks occur in Injection port septum Injection port column nut Broken or cracked capillary column Leaks can occur in many more places in the MSD GC MSD interface column nut GC MSD interface O ring where the interface attaches...

Page 90: ...g in the GC typically comes from one of these sources Column or septum bleed Dirty injection port Injection port liner Contaminated syringe Poor quality carrier gas Dirty carrier gas tubing Fingerprints improper handling of clean parts Contamination originating in the MSD typically comes from one of the following sources Air leak Cleaning solvents and materials Diffusion pump fluid Foreline pump o...

Page 91: ...solvent 78 Benzene Cleaning solvent 91 92 Toluene or xylene Cleaning solvent 105 106 Xylene Cleaning solvent 151 153 Trichloroethane Cleaning solvent 69 Foreline pump oil or PFTBA Foreline pump oil vapor or calibration valve leak 73 147 207 221 281 295 355 429 Dimethylpolysiloxane Septum bleed or methyl silicone column bleed 77 94 115 141 168 170 262 354 446 Diffusion pump fluid and related ions D...

Page 92: ...92 ...

Page 93: ...procedures for the MSD Many of these procedures are demonstrated on the HP MSD Reference Collection CD ROM Before starting 94 Maintaining the vacuum system 101 Maintaining the analyzer 144 Maintaining the GC MSD interface 172 Maintaining the electronics 177 ...

Page 94: ...operations performed This makes it easier to identify variations from nor mal operation and to take corrective action Table 4 Maintenance schedule Task Every week Every 6 months Every year As needed Tune the MSD Check the foreline pump oil level Check the calibration vial Replace the foreline pump oil1 Check the diffusion pump fluid Clean the ion source Check the carrier gas trap s on the GC Repla...

Page 95: ...or that procedure Tables 5 and 6 summarize these Table 5 Tools Description HP part number Ball driver 1 5 mm 8710 1570 2 0 mm 8710 1804 2 5 mm 8710 1681 Funnel Hex nut driver 5 5 mm 8710 1220 Pliers long nose 1 5 inch nose 8710 1094 Screwdriver flat blade large 8730 0002 TORX T 10 8710 1623 TORX T 15 8710 1622 TORX T 20 8710 1615 Tweezers non magnetic 8710 0907 Wrench open end 1 4 inch 5 16 inch 8...

Page 96: ...0103 Filament assembly 05972 80053 Foreline exhaust oil trap 3150 0761 Foreline pump oil 1 liter 6040 0834 Gloves chemical resistant resistant to oils and solvents clean lint free large 8650 0030 clean lint free small 8650 0029 Grease Apiezon L high vacuum 6040 0289 Heater sensor assemblies GC MSD interface 05972 60106 ion source G1099 60177 mass filter G1099 60172 Octafluoronaphthalene 1 pg ul 85...

Page 97: ...ic circuit boards Toroidal transformer Turbomolecular pump controller Wires and cables between these boards Wires and cables between these boards and the connectors on the back panel of the MSD Some connectors on the back panel for example the foreline power receptacle Normally all of these parts are shielded by safety covers As long as the safety covers are in place it should be difficult to acci...

Page 98: ... hot enough to be dangerous Many parts in the MSD operate at or reach temperatures high enough to cause serious burns These parts include but are not limited to GC MSD interface Analyzer parts Vacuum pumps The GC injection ports and GC oven also operate at very high temperatures Use the same caution around these parts See the documentation supplied with your GC for more information 5 1 1 1HYHU WRX...

Page 99: ...stead install a hose to take the exhaust from the foreline pump outdoors or into a fume hood vented to the outdoors Be sure to comply with your local air quality regulations The fluids in the diffusion pump and foreline pump also collect traces of the samples being analyzed All used pump fluid should be considered hazard ous and handled accordingly Dispose of used fluid correctly as specified by y...

Page 100: ...ents with wires contacts or cables connected to printed circuit boards always use a grounded anti static wrist strap and take other anti static precautions The wrist strap should be connected to a known good Earth ground If that is not possible it should be connected to a conductive metal part of the assembly being worked on but not to electronic compo nents exposed wires or traces or pins on conn...

Page 101: ...led can result in decreased instru ment performance It can also result in damage to your instrument Other procedures should be performed as needed Tasks such as replacing a foreline vacuum gauge or triode gauge tube should be performed only when needed See Chapter 3 Troubleshooting the MSD on page 65 and see the online help in the MSD ChemStation software for symptoms that indicate this type of ma...

Page 102: ... be almost clear If the oil level is near or below the lower line follow the steps 2 6 to add foreline pump oil If your MSD is nearing its scheduled time for replacement of the foreline pump oil replace the oil instead of adding oil If the oil is dark or cloudy replace it See page 104 for instructions about replacing the foreline pump oil 2 Vent the MSD page 52 3 Remove the fill cap 4 Add pump flu...

Page 103: ...4 Maintaining the MSD To check and add foreline pump oil 103 Lower line Oil level window Fill cap Upper line ...

Page 104: ...he vacuum manifold The foreline pump may be located on the floor on the lab bench next to or behind the MSD or under the vacuum manifold at the back of the MSD 3 Place a book or other object under the pump motor to tilt it up slightly 4 Remove the fill cap 5 Place a container under the drain plug 6 Remove the drain plug Allow the pump oil to drain out The oil drains faster if it is still warm 7 Re...

Page 105: ...4 Maintaining the MSD To drain the foreline pump 105 Fill cap Drain plug Pump motor ...

Page 106: ...pump motor 4 Add foreline pump oil until the oil level in the window is near but not above the upper line The foreline pump requires approximately 0 28 liters of oil 5 Wait a few minutes for the oil to settle If the oil level drops add oil to bring the oil level to near the upper line 6 Reinstall the fill cap 7 If necessary slide the foreline pump back under the vacuum manifold The foreline pump m...

Page 107: ...4 Maintaining the MSD To refill the foreline pump 107 Fill cap Upper line Oil level window Drain plug ...

Page 108: ...e trap adapter 5 1 1 R QRW EUHDWKH WKH SXPS H KDXVW LW PD FRQWDLQ SXPS RLO YDSRU R QRW UHSODFH WKH WUDS ZKLOH VDPSOHV DUH EHLQJ DQDO HG 5 1 1 7KH WUDS VWRSV RQO IRUHOLQH SXPS RLO W GRHV QRW WUDS RU ILOWHU RXW WR LF FKHPLFDOV I RX DUH XVLQJ WR LF VROYHQWV RU DQDO LQJ WR LF FKHPLFDOV UHPRYH WKH RLO WUDS R QRW XVH WKH WUDS ZLWK D 06 QVWDOO D KRVH WR WDNH WKH IRUHOLQH SXPS H KDXVW RXWVLGH RU WR D IXPH...

Page 109: ...4 Maintaining the MSD To replace the oil trap 109 Oil trap Clamp O ring assembly Oil trap adapter Foreline pump ...

Page 110: ...ing temperature Use the COLD marks if the pump is off and has had time to cool If the fluid level is below the bottom of the appropriate range replace the diffusion pump fluid Do not just add fluid The pump fluid should be clear or almost clear Dark or cloudy pump fluid indi cates an air leak or excessive heat If the pump fluid appears dark or cloudy replace it Then check for an air leak The diffu...

Page 111: ...4 Maintaining the MSD To check the diffusion pump fluid 111 Fan Fluid level window sight glass ...

Page 112: ...cuum manifold The foreline pump may be located on the floor on the lab bench next to or behind the MSD or under the vacuum manifold at the back of the MSD 5 Move the MSD away from the GC until you have access to the GC MSD interface cable 6 Disconnect the GC MSD interface cable Disconnecting the cable with the GC on can cause a fault condition 7 Continue to move the MSD until you have access to th...

Page 113: ...4 Maintaining the MSD To separate the MSD from the GC 113 ...

Page 114: ...arness These are on the side of the diffusion pump not shown in the illustration 5 Disconnect high vacuum power HIVAC POWER cable from the back panel of the MSD This is the thick black cable that emerges near the bottom of the pump 6 Support the diffusion pump with one hand 7 Remove the KF50 clamp 8 Lower the diffusion pump 9 Remove the O ring assembly from the top of the diffusion pump The O ring...

Page 115: ...p 115 10 Remove the diffusion pump through the side of the MSD You may have to tilt the pump slightly to remove it Do not tilt the pump past 45 if the pump is warm KF50 clamp O ring assembly Diffusion pump Diffusion pump outlet Foreline gauge assembly ...

Page 116: ...the pump fluid pours very slowly Charred or blackened pump fluid If the diffusion pump has been heated with insufficient pump fluid or with a large air leak in the MSD the remaining pump fluid may be severely blackened Black ened pump fluid may also be baked onto the internal parts stack of the pump If so you may have to remove the diffusion pump stack and clean its parts and the interior of the p...

Page 117: ...tions on the bottle for pre heating the diffusion pump fluid 6 Pour new diffusion pump fluid into diffusion pump until the fluid level is within the FULL COLD range It will require approximately 1 5 to 2 containers 18 5 ml each of diffusion pump fluid Watch the sight glass while pouring Do not overfill 7 Reinstall the diffusion pump page 118 ...

Page 118: ...usion pump into the MSD You may have to tilt the pump slightly to get it into the MSD tilt it past 45 3 Install the O ring assembly on the diffusion pump 4 Lift the diffusion pump into its normal position 5 Install the KF50 clamp 6 Reconnect the diffusion pump temperature sensor wires to the wiring harness 7 Reconnect the high vacuum power cable to the HIVAC POWER connector on the back panel of th...

Page 119: ...4 Maintaining the MSD To reinstall the diffusion pump 119 KF50 clamp O ring assembly Diffusion pump Diffusion pump outlet Foreline gauge assembly ...

Page 120: ...e GC Be careful not to damage the GC MSD interface as it passes into the GC Make sure the end of the GC MSD interface extends into the GC oven 4 If necessary slide the foreline pump back under the vacuum manifold The foreline pump may be located on the floor on the lab bench next to or behind the MSD or under the vacuum manifold at the back of the MSD 5 Reinstall the capillary column page 28 6 Pum...

Page 121: ...4 Maintaining the MSD To reconnect the MSD to the GC 121 ...

Page 122: ...FF from the Execute menu In the Manual Tune view select MS OFF from the Execute menu Type MSOFF on the command line and press Enter Verify that only the power LED is lit on the front of the MSD 3 If your MSD is equipped with a gauge controller switch off the triode gauge and the gauge controller 4 Remove the upper MSD cover page 50 5 Loosen the calibration vial collar by turning it counterclockwis...

Page 123: ...4 Maintaining the MSD To remove the calibration vial 123 Calibration valve Collar Calibration vial ...

Page 124: ...as possible 4 Withdraw the vial 1 mm This prevents damage when you tighten the collar 5 Turn the collar clockwise to tighten it Clockwise as viewed from the bottom vial side of the collar The collar should be snug but not overly tight Do not use a tool to tighten the collar It does not require that much force 6 Reinstall the upper MSD cover 7 Select Purge Cal Valve from the Vacuum menu in the Diag...

Page 125: ...4 Maintaining the MSD To refill and reinstall the calibration vial 125 Calibration valve Collar Calibration vial 6 mm ...

Page 126: ... the foreline gauge cable from the foreline gauge 4 Disconnect the foreline gauge assembly from the diffusion pump outlet 5 Loosen the hose clamp 6 Pull the foreline gauge assembly out of the foreline hose 5 1 1 7KH IRUHOLQH SXPS DQG GLIIXVLRQ SXPS PD VWLOO EH KRW 8 7 2 1 Be sure the MSD is vented to atmosphere before breaking the seal at the foreline gauge Never vent the MSD at the pump end use t...

Page 127: ...4 Maintaining the MSD To remove the foreline gauge 127 Foreline gauge Foreline gauge cable Foreline gauge assembly Foreline hose and hose clamp Diffusion pump outlet ...

Page 128: ...hose 2 Tighten the hose clamp 3 Reconnect the foreline gauge cable to the foreline gauge 4 Reconnect the foreline gauge assembly to the diffusion pump outlet 5 Reconnect the MSD to the GC page 120 6 If necessary slide the foreline pump back under the vacuum manifold The foreline pump may be located on the floor on the lab bench next to or behind the MSD or under the vacuum manifold at the back of ...

Page 129: ...4 Maintaining the MSD To reinstall a foreline gauge 129 Foreline gauge Foreline gauge cable Foreline gauge assembly Foreline hose and hose clamp Diffusion pump outlet ...

Page 130: ...622 1 Vent the MSD page 52 2 Disconnect the calibration valve cable from the connector next to the fan 3 Loosen the collar and remove the calibration vial Turn the collar counterclockwise as viewed from the bottom vial side of the thumbscrew Just loosen the collar do not remove it 4 Remove the calibration valve from the front end plate ...

Page 131: ...4 Maintaining the MSD To remove the calibration valve 131 Calibration valve Collar Calibration vial Front end plate Calibration valve O ring ...

Page 132: ... calibration valve Tighten the screws that hold it in place Make sure you use the calibration valve that matches the high vacuum pump in your MSD The different calibration valves have different restrictors Using the wrong valve will interfere with tuning 4 Reconnect the calibration valve cable to the connector next to the fan 5 Remove the vial from the new calibration valve page 122 The valve is s...

Page 133: ...4 Maintaining the MSD To reinstall a calibration valve 133 Calibration valve Collar Calibration vial Front end plate Calibration valve O ring ...

Page 134: ...nect the fan wiring and safety grill from the old fan The fan wiring ends in a small connector on the back of the fan 6 Connect the fan wiring and safety grill to the new fan 7 Install the new fan and reinstall the 4 screws 8 Connect the fan wiring to the fan connector on the MSD frame 9 Reinstall the MSD covers 10 Pump down the MSD page 58 5 1 1 R QRW WRXFK WKH KLJK YDFXXP SXPS 7KH KLJK YDFXXP SX...

Page 135: ...4 Maintaining the MSD To replace the fan for the high vacuum pump 135 Fan wiring disconnect from back side of fan also Fan Safety grill ...

Page 136: ...sen the triode gauge collar by turning it counterclockwise Do not remove the collar 4 Pull the triode gauge tube out of the collar 5 Remove the baffle from the open end of the triode gauge tube Wear clean gloves when handling the baffle If you set the baffle down make sure it is on a clean surface 5 1 1 1HYHU FRQQHFW RU GLVFRQQHFW WKH FDEOH IURP WKH WULRGH JDXJH WXEH ZKLOH WKH 06 LV XQGHU YDFXXP 7...

Page 137: ...4 Maintaining the MSD To remove the triode gauge tube 137 Triode gauge cable Triode gauge collar Triode gauge tube Baffle ...

Page 138: ...be If you set the baffle down make sure it is on a clean surface 3 Slide the triode gauge tube into the collar Leave 3 mm of the metal sleeve exposed Be sure the pins are oriented as in the illustration 4 Gently hand tighten the collar by turning it clockwise 5 Reconnect the cable from the gauge controller to the triode gauge tube Route the cable so it does not put stress on the triode gauge tube ...

Page 139: ...4 Maintaining the MSD To reinstall a triode gauge tube 139 Triode gauge cable Triode gauge collar Triode gauge tube Baffle ...

Page 140: ...manifold page 54 3 Use a clean lint free cloth or glove to spread a thin coat of high vacuum grease on the exposed surface of the O ring 4 Use a clean lint free cloth or glove to wipe away excess grease If the O ring looks shiny there is too much grease on it 5 Close the vacuum manifold page 56 6 Pump down the MSD page 56 8 7 2 1 Vacuum seals other than the side plate O ring and vent valve O ring ...

Page 141: ...4 Maintaining the MSD To lubricate the side plate O ring 141 Side plate O ring ...

Page 142: ...is procedure 1 Vent the MSD page 52 2 Completely remove the vent valve knob 3 Inspect the O ring If the O ring appears damaged replace it 4 Use a clean lint free cloth or glove to spread a thin coat of high vacuum grease on the exposed surface of the O ring 5 Use a clean lint free cloth or glove to wipe away excess grease If the O ring looks shiny there is too much grease on it 8 7 2 1 Vacuum seal...

Page 143: ... vent valve knob 7 Pump down the MSD page 58 Vent valve O ring Vent valve knob Front end plate 8 7 2 1 Be very careful when reinstalling the vent valve knob It is very easy to cross thread the knob and damage the threads in the front end plate Be sure the O ring stays in place ...

Page 144: ...des more extensive information Care must be taken during analyzer maintenance to keep components clean Analyzer maintenance involves opening the vacuum manifold and removing parts from the analyzer During analyzer maintenance procedures care must be take to avoid contaminating the analyzer or interior of the vacuum manifold Clean gloves should be worn during all analyzer maintenance procedures Aft...

Page 145: ...ce In general the mass filter should never be disturbed In the event of extreme contam ination it can be cleaned but such cleaning should only be done by a trained Hewlett Packard service representative More information is available If you need more information about the locations or functions of analyzer components refer to Chapter 7 Analyzer on page 215 Most of the procedures in this chapter are...

Page 146: ...and take other anti static precautions before touching analyzer components 3 Disconnect the 7 colored wires from the ion source 4 Disconnect the wires for the ion source heater and temperature sensor from the feedthrough board 5 Remove the thumbscrews that hold the ion source in place 6 Pull the ion source out of the source radiator 8 7 2 1 Pull on the connectors not on the wires 5 1 1 7KH DQDO HU...

Page 147: ...4 Maintaining the MSD To remove the ion source 147 Thumbscrew Thumbscrew Ion source Feedthrough board Source radiator Source heater and temperature sensor wires ...

Page 148: ...5 5 mm 8710 1220 Wrench open end 10 mm 8710 2353 1 Remove the ion source page 146 2 Remove the filaments 3 Separate the repeller assembly from the source body The repeller assembly includes the source heater assembly repeller and related parts 4 Remove the repeller 5 Unscrew the interface socket A 10 mm open end wrench fits on the flats on the interface socket 6 Remove the setscrew for the lenses ...

Page 149: ...9 Entrance lens Lens insulator one of a pair Drawout plate Drawout cylinder Ion focus lens Filament Repeller nut do not overtighten Washer Repeller insulator Source heater assembly Interface socket Source body Set screw Repeller Repeller insulator Filament ...

Page 150: ...de methylene chloride reagent grade Ultrasonic bath 1 Disassemble the ion source page 148 2 Collect the following parts to be cleaned Repeller Interface socket Source body Drawout plate Drawout cylinder Ion focus lens Entrance lens These are the parts that contact the sample or ion beam The other parts normally should not require cleaning 8 7 2 1 If insulators are dirty clean them with a cotton sw...

Page 151: ...4 Maintaining the MSD To clean the ion source 151 Drawout plate Drawout cylinder Ion focus lens Entrance lens Source body Repeller Interface socket ...

Page 152: ...h reagent grade methanol Make sure all abrasive residue is rinsed way before ultrasonic cleaning If the methanol becomes cloudy or contains visible particles rinse again 5 Separate the parts that were abrasively cleaned from the parts that were not abrasively cleaned 6 Ultrasonically clean the parts for 15 minutes in each of the following solvents Ultrasonically clean each group of parts separatel...

Page 153: ...n oven at 100 150 C for 30 minutes Take care to avoid recontaminating cleaned and dried parts Put on new clean gloves before handling the parts Do not set the cleaned parts on a dirty surface Set them only on clean lint free cloths 5 1 1 HW WKHVH SDUWV FRRO EHIRUH RX KDQGOH WKHP ...

Page 154: ...e source body 4 Install the setscrew that holds the lenses in place 5 Reinstall the repeller repeller insulators washer and repeller nut into the source heater assembly The resulting assembly is called the repeller assembly 6 Reconnect the repeller assembly to the source body The repeller assembly includes the source heater assembly repeller and related parts 7 Reinstall the filaments 8 Reinstall ...

Page 155: ...source 155 Entrance lens Lens insulator one of a pair Drawout plate Drawout cylinder Ion focus lens Filament Repeller nut Washer Repeller insulator Source heater assembly Interface socket Source body Set screw Repeller Repeller insulator Filament ...

Page 156: ...nd hand tighten the source thumbscrews Do not overtighten the thumbscrews 3 Reconnect the 7 colored wires to the appropriate pins on the ion source 4 Reconnect the source heater and temperature sensor wires to the pins on the feedthrough board 5 Close the vacuum manifold page 56 6 Pump down the MSD page 58 Wire color Connects to Blue Entrance lens Orange Ion focus White Filament 1 top filament Red...

Page 157: ...Maintaining the MSD To reinstall the ion source 157 Thumbscrew Thumbscrew Ion source Feedthrough board Source radiator Source heater and sensor wires Ion focus pin orange wire Entrance lens pin blue wire ...

Page 158: ...int free large 8650 0030 small 8650 0029 Hex ball driver 1 5 mm 8710 1570 1 Vent the MSD page 52 2 Open the vacuum manifold page 54 3 Remove the ion source page 146 4 Remove the filament s to be replaced 5 1 1 7KH DQDO HU RSHUDWHV DW KLJK WHPSHUDWXUHV R QRW WRXFK DQ SDUW XQWLO RX DUH VXUH LW LV FRRO ...

Page 159: ...4 Maintaining the MSD To remove a filament 159 Filament 2 Filament 1 ...

Page 160: ...ource page 156 3 Close the vacuum manifold page 56 4 Pump down the MSD page 58 5 Autotune the MSD page 48 6 In the Edit Parameters dialog box Instrument Edit MS Tune Parameters select the other filament 7 Autotune the MSD again 8 Select and use the filament that give the best results If you decide to use the first filament run Autotune again to make sure the tune parameters are compatible with the...

Page 161: ...4 Maintaining the MSD To reinstall a filament 161 Filament 2 Filament 1 ...

Page 162: ...mm 8710 1220 1 Vent the MSD page 52 2 Open the vacuum manifold page 54 3 Remove the ion source from the source radiator page 146 4 Remove the filaments 5 Remove the repeller assembly The repeller assembly includes the source heater assembly repeller and related parts 6 Remove the repeller nut washer repeller insulators and repeller You do not need to remove the heater and temperature sensor from t...

Page 163: ...4 Maintaining the MSD To remove the heater and sensor from the ion source 163 Source heater assembly Filament Repeller nut Washer Repeller insulator Source body Filament Repeller insulator Repeller ...

Page 164: ...2 Reinstall the repeller repeller insulators washer and repeller nut The resulting assembly is called the repeller assembly 3 Connect the repeller assembly to the source body 4 Reinstall the filaments 5 Reinstall the ion source in the source radiator page 156 Do not forget to reconnect the wires from the feedthrough board to the ion source Do not forget to reconnect the heater and temperature sens...

Page 165: ...4 Maintaining the MSD To reinstall the heater and sensor in the ion source 165 Source heater assembly Filament Repeller nut Washer Repeller insulator Source body Filament Repeller insulator Repeller ...

Page 166: ... 8650 0029 Hex ball driver 1 5 mm 8710 1570 Hex ball driver 2 0 mm 8710 1804 1 Vent the MSD page 52 2 Open the vacuum manifold page 54 3 Disconnect the mass filter heater and temperature sensor wires from the feedthrough board 4 Remove the mass filter heater assembly from the mass filter radiator 8 7 2 1 Do not touch the mass filter contact leads This could cause ESD damage to the side board ...

Page 167: ...ing the MSD To remove the heater and sensor from the mass filter 167 Mass filter contact lead do not touch Mass filter radiator Mass filter heater assembly Feedthrough board Mass filter contact lead do not touch ...

Page 168: ...8710 1804 Mass filter heater assembly G1099 60172 1 Unpack the new mass filter heater assembly The heater temperature sensor and heater block are already assembled 2 Install the heater assembly on top of the mass filter radiator 3 Connect the heater and temperature sensor wires to the feedthrough board 4 Close the vacuum manifold page 56 5 Pump down the MSD page 58 8 7 2 1 Do not touch the mass fi...

Page 169: ...ing the MSD To reinstall the heater and sensor in the mass filter 169 Mass filter contact lead do not touch Mass filter radiator Mass filter heater assembly Feedthrough board Mass filter contact lead do not touch ...

Page 170: ...he retaining clip Pinch the two arms of the clip together and swing the clip down 4 Remove the electron multiplier horn 5 Install the new electron multiplier horn 6 Close the retaining clip The signal pin on the horn should rest on the outside of the loop in the contact strip Do not put the signal pin on the inside of the loop in the contact strip Incor rect installation will result in poor sensit...

Page 171: ...4 Maintaining the MSD To replace the electron multiplier horn 171 Contact strip Retaining clip Electron multiplier horn Signal pin Signal pin ...

Page 172: ... is necessary to replace the heater and sensor This section contains proce dures for removing the heater and sensor and installing new ones More information is available If you need more information about the locations or functions of GC MSD interface components refer to Chapter 6 GC MSD Interface on page 211 Most of the procedures in this chapter are illustrated with video clips in the HP 5973 MS...

Page 173: ...rature sensor from the heater sleeve Heat and oxidation often result in a heater or less frequently a temperature sen sor being welded inside the heater sleeve The holes for the heater and sensor pass all the way through the heater sleeve A rod can be inserted to drive the stuck part out However to function correctly the heater and sensor must have perfect contact with their holes If a heater or s...

Page 174: ... 4 Maintaining the MSD To remove the GC MSD interface heater and sensor Heater sleeve Temperature sensor Heater Interface welded assembly Insulation Cover Set screw Heater sleeve screw Heater sleeve screw ...

Page 175: ...en the screws evenly 4 Slide the insulation onto the GC MSD interface 5 Reinstall the GC MSD interface cover Make sure the wires from the heater and sensor pass through the cutout in the interface cover 6 Reconnect the MSD to the GC page 120 Make sure you reconnect the GC MSD interface cable to the GC Make sure you reinstall the capillary column 7 Pump down the MSD page 58 8 Turn on the GC Re esta...

Page 176: ...176 Heater sleeve Temperature sensor Heater Interface welded assembly Insulation Cover Set screw Heater sleeve screw Heater sleeve screw ...

Page 177: ...ics during maintenance All of the printed circuit boards in the MSD contain components that can be damaged by electrostatic discharge ESD Do not handle or touch these boards unless absolutely necessary In addition wires contacts and cables can conduct ESD to the printed circuit boards to which they are connected This is especially true of the mass filter quadrupole contact wires which can carry ES...

Page 178: ...tra precautions such as a grounded anti static mat if you must work on components or assemblies that have been removed from the MSD This includes the analyzer More information is available If you need more information about the functions of electronic components refer to Chapter 8 Electronics on page 233 Most of the procedures in this chapter are illustrated with video clips in the HP 5973 MSD Ref...

Page 179: ...4 In the Diagnostics Vacuum Control view select Set RFPA from the Diagnostics menu 5 Enter an amu value of 100 6 Slowly turn the RF coil adjustment screws to minimize the voltage displayed Turn the adjustment screws alternately Turn each screw only a little bit at a time Keep the screws at equal extension The minimum voltage is typically between 70 and 100 mV 7 When the voltage is minimized click ...

Page 180: ...eps 4 through 7 for 650 amu The minimum voltage is typically between 500 and 650 mV 9 Exit the Set RFPA program 10 Select MS OFF from the Diagnostics menu 11 Reinstall the upper MSD cover 12 Tune the MSD page 48 RF coil adjustment screw RF coil adjustment screw ...

Page 181: ... Vent the vacuum manifold by opening the vent valve knob 3 Turn one of the fuse holders counterclockwise until it pops out The fuse holders are spring loaded 4 Remove the old fuse from the fuse holder 5 Install a new fuse in the fuse holder 6 Reinstall the fuse holder 5 1 1 1HYHU UHSODFH WKH SULPDU IXVHV ZKLOH WKH 06 LV FRQQHFWHG WR D SRZHU VRXUFH 8 7 2 1 If a fuse failure turns off the MSD wait a...

Page 182: ...182 7 Repeat steps 3 6 for the other fuse Always replace both fuses 8 Reconnect the MSD power cord to the electrical outlet 9 Pump down the MSD page 58 Primary fuses in holders ...

Page 183: ...em 186 Turbo pump MSD vacuum system 187 Diffusion pump vacuum manifold 188 Turbo pump vacuum manifold 189 Side plate 190 Vacuum seals 192 Foreline pump 194 Foreline gauge 196 Diffusion pump and fan 198 Turbomolecular pump and fan 202 Calibration valve and vent valve 204 Triode gauge tube 206 Gauge controller 208 ...

Page 184: ...cuum system are common to both but some parts are specific to the one high vacuum pump or the other Many components make up the vacuum system Many parts make up the vacuum system Vacuum manifold Side plate and front and rear end plates Vacuum seals Foreline rough pump High vacuum pump Calibration valve and vent valve Vacuum control electronics Vacuum gauges and gauge control electronics Each of th...

Page 185: ...uum cooling fan Foreline pump Foreline hose High vacuum pump Triode gauge tube Vacuum manifold Side plate Calibration valve Side plate hinge Rear side plate thumbscrew High vacuum pump clamps Front side plate thumbscrew Vent valve ...

Page 186: ...r from migrating into the vacuum manifold Foreline pressure is monitored by the foreline gauge The ac board controls the diffusion pump heater The diffusion pump MSD can accept up to 2 ml min carrier gas flow Diffusion pump baffle adapter Diffusion pump Foreline gauge Too hot switch Manifold cooling fins Calibration valve Diffusion pump vacuum manifold Too cold switch High vacuum cooling fan diffu...

Page 187: ...een to keep debris out of the pump but no baffle is necessary Pump speed is controlled by the turbo controller there is no foreline gauge The turbo pump MSD can accept up to 4 ml min carrier gas flow The calibration valve has a restrictor with a larger internal diameter Turbo pump controller Calibration valve Turbo pump vacuum manifold High vacuum cooling fan turbo pump position Turbo pump ...

Page 188: ...ide attachment points for the triode gauge tube calibration valve vent valve GC MSD interface and high vacuum pump The diffusion pump attaches with a KF50 seal to a baffle adapter that is clamped to the bottom of the manifold A vapor baffle helps prevent migration of pump fluid vapor into the manifold Cooling fins on the bottom of the manifold keep the baf fle cool so the vapor will condense on it...

Page 189: ...ng fins The turbo pump and the mounting bracket for the turbo controller are clamped directly to the manifold In every other respect the two manifolds are identical Triode gauge port behind shield GC MSD interface port Rear end plate Side plate O ring groove Front end plate Calibration valve port Vent valve port Triode gauge port shield ...

Page 190: ...edthroughs to analyzer components The electronic side board is mounted on the atmospheric side of the side plate Thumbscrews are located at each end of the side plate 8 7 2 1 Fasten both side plate thumbscrews for shipping or storage RQO For normal operation the both thumbscrews should be loose For operation with hydrogen carrier gas or with flammable or explosive CI reagent gases the front thumbs...

Page 191: ...tput feedthrough EM voltage feedthrough High voltage HED feedthrough Detector focus feedthrough Side plate hinge Rear side plate thumbscrew Side board Screws for radiator mounting brackets Front side plate thumbscrew Vacuum manifold Side plate O ring Mass filter quadrupole feedthrough Ion source and heater feedthroughs ...

Page 192: ...ifold and should not need to be removed The GC MSD interface fastens to the manifold with three screws The calibration valve assembly is fastened onto the front end plate by two screws The vent valve knob threads into the front end plate Small O rings in grooves in the front end plate provide vacuum seals The diffusion pump baffle adapter has a groove for its O ring The baffle adapter is clamped t...

Page 193: ...n O ring that is compressed against the side plate by a threaded collar Side plate KF seal with internal centering ring Vacuum manifold Side plate and other face seals KF flange clamp not shown KF flange clamp not shown Ferrule O ring Triode tube Collar KF seal with external centering ring Vacuum manifold ...

Page 194: ...c chemicals or using toxic solvents do not use the trap Instead install a hose to take the foreline pump exhaust outside or to a fume hood A window sight glass in the front of the foreline pump shows the level of the foreline pump oil There are two marks next to the window The level of the pump oil should never be above the upper mark or below the lower mark If the level of pump oil is near the lo...

Page 195: ...5 Vacuum System Foreline pump 195 Foreline hose from high vacuum pump outlet Oil fill cap Ballast control leave closed Exhaust outlet Drain plug Oil level window ...

Page 196: ...he diffusion pump is automatically switched on If the fore line pressure rises above 400 mTorr 0 4 Torr the ac board switches off the diffu sion pump heater and the analyzer electronics The foreline pressure can be monitored from your data system The turbo pump MSD does not require a foreline gauge Instead the motor speed is monitored See Also To view MSD temperature and vacuum status page 36 Gaug...

Page 197: ...5 Vacuum System Foreline gauge 197 Foreline gauge assembly Foreline gauge cable part of high vacuum control cable Diffusion pump outlet KF10 16 seal Foreline hose and hose clamp KF10 16 clamp ...

Page 198: ... molecules down toward the outlet near the bottom of the pump Another nozzle in the stack points directly at the outlet and forces the gas molecules out The vapor condenses on the sides of the pump and the liquid drains down to the bottom The liquid is boiled again and is reused continuously The foreline pump is connected by the foreline hose to the outlet of the diffusion pump It removes the gas ...

Page 199: ... the front cover of the MSD The fan draws air through the cover and blows it over the pump Without this cooling the pump fluid vapor would not condense correctly but would diffuse into the vacuum manifold Diffusion pump operational readiness is monitored by two thermal switches Table 7 Diffusion pump thermal switches 7KHUPDO 6ZLWFK Too Cold Too Hot 1RUPDO VWDWH Normally open Normally closed KDQJHV...

Page 200: ...tions or if the fluid turns dark brown or black replace the fluid Diffusion pump fluid that is exposed to air at operating temperature will break down and turn dark brown or black This reaction is called cracking Cracked pump fluid gives two symptoms higher manifold pressure and high background with a large peak at m z 446 See Also Maintaining the MSD page 93 Troubleshooting HP 5973 MSD in the onl...

Page 201: ... Vacuum System Diffusion pump and fan 201 Inlet Cooling fins Too cold sensor Too hot sensor Diffusion pump outlet Cold fluid level marker High vacuum power cable Hot fluid level marker Fluid level window ...

Page 202: ...s current to the pump and monitors pump motor speed and temperature A cooling fan is located between the turbo pump and the front panel of the MSD The fan draws air from outside the MSD and blows it over the pump The turbo pump turns on automatically as soon as the MSD power is switched on The system will allow the analyzer to be turned on when the turbo pump is greater than 80 speed but the pump ...

Page 203: ...5 Vacuum System Turbomolecular pump and fan 203 Turbo pump inlet Turbo pump outlet Foreline hose Hose clamp Connector for cable to turbo controller Pump vent port blanked off KF25 clamp ...

Page 204: ...ing compound into the vacuum manifold The turbo pump and the diffusion pump MSDs have different calibration valves designed to allow the correct diffusion of calibrant for each vacuum system Perfluorotributylamine PFTBA is the most commonly used tuning compound It is required for automatic tuning of the MSD Other compounds can be used for manual tuning Vent valve The vent valve knob screws into a ...

Page 205: ...5 Vacuum System Calibration valve and vent valve 205 Calibration valve Vent valve knob Calibration vial Air passage O ring Vent valve knob Valve closed Valve open Valve open too far ...

Page 206: ...r of ions formed is a function of the number of gas molecules present that is the gas pressure There fore pressure can be calculated based on the current applied to the filament cathode and the current measured in the collector Since one end of the triode gauge tube is open to the vacuum manifold the pres sure in the triode gauge is essentially the same as the pressure in the vacuum man ifold To p...

Page 207: ...mission current regulated by gauge controller Grid voltage supplied by gauge controller Filament voltage and emission current regulated by gauge controller Collector ion current measured by gauge controller Grid Filament cathode Collector Open to vacuum manifold ...

Page 208: ...essure present in the vacuum manifold The vacuum manifold pressure in Torr is displayed on the front panel of the con troller The gauge controller is calibrated for nitrogen N2 The carrier gas is usually helium which has does not ionize as readily as nitrogen Therefore the indi cated pressure for helium is approximately 6 times lower than the absolute pres sure For example a reading of 2 0 10 5 To...

Page 209: ...5 Vacuum System Gauge controller 209 Pressure display Gauge on off switch Power indicator Power cord Power switch Cable to triode gauge tube Fuse Ground point ...

Page 210: ...210 ...

Page 211: ...6 GC MSD Interface This chapter describes the function of the GC MSD interface GC MSD interface 212 ...

Page 212: ...apillary column extend past the end of the guide tube and into the ionization chamber The GC MSD interface is heated by an electric cartridge heater The heater is powered and controlled by Thermal Aux 2 heated zone of the HP 6890 Series GC The GC MSD interface temperature can be set from the MSD ChemStation or from the keypad of the gas chromatograph A sensor ther mocouple in the GC MSD interface ...

Page 213: ...erface 213 Heater sleeve Heater sleeve screws Welded interface assembly Insulation Interface cover Heater sensor assembly Vacuum manifold Ionization chamber O ring Screw Interface socket Guide tube Capillary column ...

Page 214: ...214 ...

Page 215: ...7 Analyzer This chapter describes the parts of the analyzer Ion source 218 Mass filter 223 Detector 227 Analyzer heaters and radiators 230 ...

Page 216: ...ugh the filter and strike the detector The detector generates a signal current proportional to the number of ions striking it The analyzer is attached to the vacuum side of the side plate The side plate is hinged to allow easy access to the analyzer Both the ion source and the mass filter are independently heated Each is mounted inside a radiator for correct heat distribution Each of the parts of ...

Page 217: ...or Detector end mounting bracket Source end mounting bracket Feedthrough board Side plate Side board Detector HED electron multiplier Mass filter heater assembly Mass filter inside radiator Mass filter contact cable Mass filter contact cable ...

Page 218: ... ions into the lens stack where they pass through several electrostatic lenses These lenses concentrate the ions into a tight beam which is directed into the mass filter Ion source body The ion source body is a cylinder Its cylindrical geometry ensures proper align ment of the lens stack It holds the other parts of the ion source With the repeller and the drawout plate it forms the ionization cham...

Page 219: ... on the electrons usually 70 eV The filament is shut off automatically if there is a general instrument shutdown There are three parameters that affect the filaments filament selection Filament filament emission Emission current and electron energy EleEnergy Filament selection The filament selection parameter Filament allows you to select which filament in the ion source is active Sometimes one fi...

Page 220: ...ween 0 and 315 µA but should be set to the software default for normal operation Electron energy The electron energy EleEnergy is the amount of energy on the ionizing electrons The electron energy is determined by the bias voltage 70 V dc bias on the fila ment causes emitted electrons to possess 70 eV electron volts This value is adjustable between 5 to 241 V dc but for normal operation set this p...

Page 221: ...mission current will reduce filament life Lower electron energy will reduce filament life Magnet The field created by the magnet directs the electrons emitted by the filament into and across the ionization chamber The magnet assembly is a permanent magnet with a charge of 350 gauss in the center of the field Repeller The repeller forms one wall of the ionization chamber A positive charge on the re...

Page 222: ...esponse Entrance lens The entrance lens is located at the entrance to the quadrupole mass filter This lens minimizes the fringing fields of the quadrupole which discriminate against high mass ions There is a permanent 4 4 volt voltage added to the entrance lens The total voltage applied to the entrance lens is the sum of the entrance lens offset and entrance lens gain and the 4 4 volt permanent of...

Page 223: ...frequency RF signal is applied to the two pairs of segments The magnitude of the RF voltage determines the mass to charge ratio of the ions that pass through the mass filter and reach the detector The ratio of dc to RF voltage determines the resolution widths of the mass peaks There are several parameters that control the dc and RF voltages All these parameters are set by Autotune but also can be ...

Page 224: ... all masses 219 width m z 219 is a prominent ion near the middle of the mass range of PFTBA The width parameter Wid219 makes small corrections to the m z 219 peak width Amu gain and amu offset must be readjusted after the 219 width is changed If you are tuning with a compound other than PFTBA there may not be an ion at m z 219 In that case set the 219 width to the last value found for it by Autotu...

Page 225: ...d by removing the upper MSD cover Mass axis gain Mass gain MassGain controls the mass assignment that is assignment of a partic ular peak to the correct m z value A higher gain yields higher mass assignment Mass gain affects peaks at high masses more than peaks at low masses Mass axis offset Mass offset MassOffs also controls the mass assignment A higher offset yields higher mass assignment Mass o...

Page 226: ...ed Cleaning must be performed by Hewlett Packard service personnel 8 7 2 1 1HYHU put the quadrupole in an ultrasonic cleaner 8 7 2 1 1HYHU change the physical orientation of the quadrupole mass filter 8 7 2 1 The fused quartz quadrupole is fragile and will break if dropped or handled roughly 8 7 2 1 The material in the cusps of the quadrupole is very hygroscopic If exposed to water the quadrupole ...

Page 227: ... mass filter to minimize signals due to photons hot neutrals and electrons coming from the ion source When the ion beam hits the HED electrons are emitted These electrons are attracted to the more positive electron multiplier horn Electron multiplier horn The electron multiplier horn carries a voltage of up to 3000 volts at its opening and 0 volts at the other end The electrons emitted by the HED ...

Page 228: ...th no other probable cause it may need to be replaced Check your tune charts for gradual degradation which indicates wearing out Select View Tunes from the Qualify menu in the Instrument Control view to see the tune charts Sudden changes usually indicate a different type of problem See Also Troubleshooting HP5973 MSD in the online help for more information about symptoms that may indicate electron...

Page 229: ...r 229 Mounting bracket EMV electron multiplier voltage wire High voltage HED wire HED feedthrough Detector focus wire Rear side plate thumbscrew HED high energy dynode Signal wire Electron multiplier horn Mounting screw ...

Page 230: ...ng the temperatures to use consider the following Higher temperatures help keep the analyzer clean longer Higher ion source temperatures result in more fragmentation and therefore lower high mass sensitivity After pumpdown it takes at least 2 hours for the analyzer to reach thermal equilib rium Data acquired sooner may not be reproducible Recommended settings for EI operation Ion source 230 C Quad...

Page 231: ...Analyzer heaters and radiators 231 Ion source radiator Detector end mounting bracket Source end mounting bracket Feedthrough board Mass filter heater assembly Mass filter radiator Side plate Source heater assembly ...

Page 232: ...232 7 Analyzer Analyzer heaters and radiators ...

Page 233: ...Electronics module 237 Main board 238 Signal amplifier board 239 HP IB MS control card 240 AC board 241 Power supplies 243 Toroid transformer 244 Back panel and connectors 245 Interfacing to external devices 248 Status display and power switch 250 Turbo pump controller 252 ...

Page 234: ... power switch Side board Turbo pump controller Each is discussed in this chapter Except for the Back panel and connec tors Status display and power switch and Interfacing to other devices sections most of this material is not essential for day to day operation of the MSD It may be of interest to persons responsible for servicing the MSD 5 1 1 DQJHURXV YROWDJHV DUH SUHVHQW XQGHU WKH VDIHW FRYHUV R ...

Page 235: ...wer cable HP IB MS control card Main board Signal amplifier board Toroid transformer AC board High voltage HED power supply Low voltage power supply Side board rear Signal cable Source power cable Side board control cable Detector focus cable ...

Page 236: ...nal to the mass selected Generates the dc component of the voltage applied to the quadrupole mass filter The magnitude of this voltage is proportional to the RF voltage Passes voltages generated on the main board and the detector focus voltage from the HED power supply to elements in the ion source and the detector Generates and adjusts filament emission current and electron energy as controlled b...

Page 237: ... The whole electronics module can be replaced if necessary by your Hewlett Packard service representative The electronics module contains Main board Signal amplifier board HP IB MS control card AC board power distribution vacuum control board Low voltage ac dc power supply High voltage HED power supply Toroid transformer assembly ...

Page 238: ...ages Performs analog to digital conversion for the coil DIP signal ion source and mass filter temperature signals and foreline pressure or turbo pump speed signal Monitors the signals from the vacuum system and fans and monitors the filament status HV fault and RF fault signals from the side board Activates the shutdown line when the analyzer electronics must be disabled Generates the control sign...

Page 239: ...li fier circuit produces an output voltage of 0 to 10 volts dc proportional to the loga rithm of the input current of 3 picoamps to 50 microamps An analog to digital converter converts the amplifier output voltage to digital information The HP IB MS control card unlogs the data into abundance counts proportional to the detector signal current ...

Page 240: ...ard has two main functions Providing a communication interface between the MSD and the data system Providing real time control of the MSD freeing the data system for other tasks Functional areas of the HP IB MS control card include Instrument controller Data processor Main processor Serial communication processor HP IB controller Remote start processor Random access memory RAM ...

Page 241: ... pump speed and other vacuum status information to the main board Turns off the foreline pump in case of a problem with pumpdown Provides power and logic interface to turbo controller Turns the calibration valve on or off as directed to by the main board Turns the diffusion pump on or off as directed to by the main board Provides the voltage for the calibration valve The power regulator ensures th...

Page 242: ...ove 300 mTorr after 4 minutes Turbo pump MSD turbo pump speed below 80 after 8 minutes This is usually because of a large air leak either the sideplate has not sealed cor rectly or the vent valve is still open This feature helps prevent the foreline pump from sucking air through the system which can damage the analyzer and pump To restart the MSD find and correct the air leak then switch the power...

Page 243: ...rest of the electronics The power supply generates the following dc voltages 24 V nominal 15 V nominal 15 V nominal 5 V nominal High voltage HED power supply The high voltage power supply provides the 10 000 volts dc for the high energy dynode HED in the detector The HED power supply also provides the 350 volts dc for the detector focus lens Due to the high impedance of this circuit it is not prac...

Page 244: ...ard It provides 24 V ac for the mass filter and source heater circuits The input wires take 120 V ac or 200 260 V ac from the ac board Depending on the line voltage one of two con nectors on the ac board is used determined by the position of a jumper on the AC board The output wires connect to the main board ...

Page 245: ...ceptacle HP IB address switches The following material describes the functions of these connectors and controls Remote start connector The remote start connector is the external connector for the remote start circuitry on the HP IB MS control card It receives remote start signals from the GC I O HP IB connector The HP IB cable from the data system is connected to the I O HP IB connector This cable...

Page 246: ...rbo controller The high vacuum power jumper connects the ac board to the high vacuum power connector Power cord receptacle The ac power cord brings in all electrical power for the MSD The power cord can be detached from the MSD The ac power receptacle is on the ac board extending through the back panel Foreline pump power cord receptacle The foreline pump power cord receptacle provides ac power fo...

Page 247: ...Electronics Back panel and connectors 247 High vacuum control cable High vacuum power cable HP IB address switch Primary fuses Foreline pump power cord Power cord receptacle HP IB cable Remote start cable ...

Page 248: ...sor are extended to the remote start Remote connector on the back panel of the MSD The remote start cable connects the GC and the MSD Remote start signals It is often necessary to communicate with external devices for example a purge and trap during a run Typically these communications are Requests to send a system ready signal Receive a start run signal from an external device Program the timing ...

Page 249: ... ready On system ready a logic high of 5 V dc is present between that pin and any ground This same high can be detected between the ready and ground pins on the remote start connector on the MSD Start run input The best way to generate a start run signal is to use the remote start connector on the GC Since remote start cables are made for most common devices this is often the simplest way A genera...

Page 250: ...D The analyzer ion source mass filter and detector is turned off except when the MSD is acquiring data or tuning This helps extend the life spans of the filaments and electron multiplier horn The analyzer status LED lights when the MSD receives the MS ON signal from the data system The analyzer LED should always be on during data acquisition or tuning Cal valve status LED The cal calibration valve...

Page 251: ...8 Electronics Status display and power switch 251 Power status LED Analyzer status LED Calibration valve status LED Power switch ...

Page 252: ...mp controller provides power to the turbomolecular pump and regu lates pump speed If the pump fails to reach 80 speed within 10 minutes after beginning pumpdown or if the speed drops below 50 during operation the con troller shuts off the turbo pump and triggers a fault state ...

Page 253: ...9 Parts This chapter lists parts that can be ordered for your MSD Electronics 256 Vacuum system 260 Analyzer 268 GC MSD interface 274 Consumables and maintenance supplies 276 ...

Page 254: ...l Hewlett Packard office Supply them with the following information Model and serial number of your MSD HP part number s of the part s needed Quantity of each part needed Some parts are available as rebuilt assemblies Rebuilt assemblies pass all the same tests and meet all the same specifica tions as new parts Rebuilt assemblies can be identified by their part numbers The first two digits of the l...

Page 255: ...art you need If a part you need is not listed in this chapter check the Hewlett Packard Analytical Supplies Catalog If you still can not find it contact your Hewlett Packard service representatives or your local Hewlett Packard of fice ...

Page 256: ...425 HED control cable1 G1099 60430 HED power cable1 G1099 60431 High vacuum power extender cable AC board to back panel 1 G1099 60436 Low voltage power supply input cable AC board to LV PS 1 G1099 60426 Low voltage power supply output cable LV PS to main board 1 G1099 60427 Mass filter contact cable kit inside vacuum manifold G1099 60130 Side board control ribbon cable main board to side board 1 G...

Page 257: ... 8120 2104 Power cord UK Hong Kong Singapore 8120 1351 Power cord US 8120 1378 Triode gauge cable triode gauge tube to gauge controller 8120 6573 Table 10 Fuses and power switch Description HP part number Fuse 4A 250V fast acting low breaking ac board and main board 1 2110 0875 Fuse 8A 250V time lag high breaking capacity primary fuses 2110 0969 Power button1 5041 1203 Power switch extender rod1 G...

Page 258: ...12 30 pin SIMM 2 required 1818 4271 72 pin SIMM 1 required 1818 5709 low voltage ac dc power supply 0950 3067 main board G1099 69010 signal amplifier board G1099 69001 toroid transformer 2 G1099 60229 Side board G1099 69015 Turbo pump controller G1099 89002 1 None of the parts in this table are user replaceable parts Refer service to your Hewlett Packard service representative 2 The toroid transfo...

Page 259: ...oard G1099 69010 Signal amplifier board G1099 69001 Toroid transformer G1099 60229 AC board G1099 69003 High voltage HED power supply G1099 80017 Low voltage ac dc power supply 0950 3067 Signal cable G1099 60416 Source power cable G1099 60428 Side board control cable G1099 60410 Fan for electronics module 3160 1038 ...

Page 260: ...adapter O ring 0905 1443 End plate O ring for front and rear end plates 0905 1441 GC MSD interface O ring 0905 1405 HED feedthrough G1099 80012 HED feedthrough O ring 0905 0490 KF10 16 seal foreline pump inlet oil trap and diffusion pump outlet 0905 1463 KF25 O ring assembly turbo pump outlet 0100 1551 KF50 seal diffusion pump inlet 0100 1884 Side plate O ring 0905 1442 Triode gauge tube O ring 09...

Page 261: ...9 Parts Vacuum system 261 Face seal Compression seal KF seal with external centering ring KF seal with internal centering ring ...

Page 262: ... G1099 89024 Foreline pump inlet seal KF10 16 0905 1463 Hose clamp 1400 1234 KF10 16 clamp foreline inlet and oil trap 0100 1397 KF16 hose adapter G1099 20531 KF25 clamp turbo pump end of foreline hose not shown 0100 0549 KF25 hose adapter turbo pump end of foreline hose not shown G1099 20532 Oil trap not shown 3150 0761 Oil trap adapter not shown 0100 1883 Oil trap seal KF10 16 0905 1463 ...

Page 263: ...9 Parts Vacuum system 263 Foreline hose 05971 60119 Hose clamp 1400 1234 KF10 16 seal 0905 1463 KF 10 16 clamp 0100 1397 Foreline pump 120 V ac G1099 89023 KF16 hose adapter G1099 20531 ...

Page 264: ... G1099 20021 Diffusion pump baffle adapter O ring 0905 1443 Diffusion pump control cable G1099 60437 End plate front G1099 20552 rear G1099 20553 Fan for high vacuum pump 3160 1037 Foreline gauge assembly G1099 60545 Foreline gauge seal 0905 1463 KF10 16 clamp diffusion pump outlet 0100 1397 KF10 16 seal diffusion pump outlet 0905 1463 KF50 clamp 0100 1395 KF50 seal foreline pump to baffle adapter...

Page 265: ... valve knob G1099 20554 Vacuum manifold diffusion pump version G1099 20549 Side plate G1099 60021 Triode gauge tube 0960 0897 Diffusion pump baffle adapter G1099 20021 KF50 clamp 0100 1395 Diffusion pump 120V G1099 80500 Foreline gauge assembly G1099 60545 Fan diffusion pump position 3160 1037 ...

Page 266: ...5 clamp for turbo pump outlet 0100 0549 KF25 O ring assembly for turbo pump outlet 0100 1551 Manifold end plates front G1099 20552 rear G1099 20553 Shield for triode gauge tube port G1099 00003 Side plate includes thumbscrews G1099 60021 Triode gauge tube 0960 0897 Turbomolecular pump1 G1946 89001 Turbo pump controller G1099 89002 Turbo pump seal1 0100 1879 Vacuum manifold G1099 20550 Vent valve k...

Page 267: ...Turbo pump controller G1099 89002 Fan turbo pump position 3160 1037 Calibration valve assembly turbo pump version G1099 60203 Vent valve knob G1099 20554 Vacuum manifold turbo pump version G0199 20550 Side plate G1099 60021 Triode gauge tube 0960 0897 ...

Page 268: ...1099 80012 O ring viton for HED feedthrough 0905 0490 ion source complete G1099 69106 magnet assembly 05971 60160 mass filter cable kit G1099 60130 mass filter contacts 4 required G1099 60142 mass filter ceramic support detector end G1099 20124 mass filter ceramic support source end G1099 20123 mass filter heater assembly G1099 60172 mass filter radiator G1099 20121 mounting bracket detector end G...

Page 269: ...nd detector to quadrupole radiator 0515 1052 Screws for mass filter contact assembly and heater block 0515 0319 Screws for radiator mounting brackets and for side board 0515 0430 Source radiator screws 0515 1052 Ion source inside radiator G1099 60021 Repeller G1099 20132 Source heater assembly G1099 60177 Magnet assembly 05971 60160 Mass filter heater assembly G1099 60172 Mass filter cable kit G10...

Page 270: ...008 drawout plate 05971 20134 entrance lens 05971 20126 filament 05972 60053 interface socket G1099 20136 ion focus lens 05971 20143 lens insulator pair 05971 20130 repeller assembly complete G1099 60170 screws for filaments and holding repeller assembly on source 0515 1046 setscrew for lens stack 0515 1446 source body G1099 20130 ...

Page 271: ...1099 60170 GC MSD interface socket G1099 20136 Lens insulator set 05971 20130 Entrance lens 05971 20126 Drawout cylinder G1072 20008 Ion focus lens 05971 20143 Drawout plate 05971 20134 Setscrew 0515 1446 Screws 0515 1046 Source body G1099 20130 Screws 0515 1046 ...

Page 272: ... parts Description HP part number Repeller assembly G1099 60170 insulator 2 required G1099 20133 nut 5 5 mm 0535 0071 repeller G1099 20132 setscrew 0515 1446 source heater assembly includes heater sensor and heater block G1099 60177 washer 3050 0891 ...

Page 273: ...9 Parts Analyzer 273 Repeller G1099 20132 Source heater assembly G1099 60177 Insulator G1099 20133 Washer 3050 0891 Nut 5 5 mm 0535 0071 Setscrew 0515 1446 Insulator G1099 20133 ...

Page 274: ...00 interface column nut not shown 05988 20066 heater sleeve G1099 20210 heater sensor assembly G1099 60107 insulation G1099 20301 setscrew for heater sensor assembly not shown 0515 0236 screws M4 x 0 7 panhead for heater sleeve 0515 0383 welded interface assembly G1099 60301 GC MSD interface O ring 0905 1405 Interface cover G1099 00005 Screws for mounting interface and cover to vacuum manifold 051...

Page 275: ...9 20210 Screws for heater sleeve 0515 0383 Welded interface assembly G1099 60301 Ion source body O ring 0905 1405 Interface socket Insulation G1099 20301 Interface cover G1099 00005 Heater sensor assembly G1099 60107 Vacuum manifold Screw 0515 0380 ...

Page 276: ...n HP part number Abrasive paper 30 µm 5061 5896 Alumina powder 8660 0791 Cloths clean package of 300 05980 60051 Cloths cleaning package of 300 9310 4828 Cotton swabs package of 100 5080 5400 Diffusion pump fluid 2 required 6040 0809 Foreline pump oil Inland 45 1 liter 6040 0834 Gloves clean large 8650 0030 small 8650 0029 Grease Apiezon L high vacuum 6040 0289 Paint touch up Glacier Gray 6010 149...

Page 277: ...1 Hex nut driver 5 5 mm 8710 1220 Pliers long nose 1 5 inch nose 8710 1094 Screwdrivers flat blade large 8730 0002 TORX T 10 8710 1623 TORX T 15 8710 1622 TORX T 20 8710 1615 Shipping kits HP 5973 MSD G1099 60565 HP 6890 Series GC G1530 60860 Tweezers non magnetic 8710 0907 Wrenches open end 1 4 inch x 5 16 inch 8710 0510 10 mm 8710 2353 Wrist strap anti static small 9300 0969 medium 9300 1257 lar...

Page 278: ...62 3508 0 5 mm id 85 Vespel 15 graphite for 0 32 mm id columns 5062 3506 0 8 mm id 85 Vespel 15 graphite for 0 53 mm id columns 5062 3538 Injection port 0 27 mm id 90 Vespel 10 graphite for 0 10 mm id columns 5062 3518 0 37 mm id 90 Vespel 10 graphite for 0 20 mm id columns 5062 3516 0 40 mm id 90 Vespel 10 graphite for 0 25 mm id columns 5181 3323 0 47 mm id 90 Vespel 10 graphite for 0 32 mm id c...

Page 279: ...G1099 60053 Foreline pump oil 1 liter 6040 0834 Foreline exhaust oil trap 3150 0761 Heater sensor assemblies GC MSD interface 05972 60106 ion source G1099 60177 mass filter G1099 60172 Octafluoronapthalene OFN 1 pg ul 8500 5441 Perfluorotributylamine PFTBA certified 1 gram 8500 0656 Perfluorotributylamine PFTBA sample kit 05971 60571 Vacuum gauges foreline gauge assembly G1099 60545 triode gauge t...

Page 280: ...280 ...

Page 281: ...0 Analyzer status LED 250 Analyzer temperatures 34 recommended 230 setting 40 Autotune 48 column flow and temperatures for 48 relative abundances of m z 502 produced by different autotunes 77 report generated by 48 viewing tune history 48 Auxiliary heated zones 34 Average linear velocity calculating 46 B Back panel and connectors 245 Background high 75 90 Ballast control on foreline pump 194 Basel...

Page 282: ...r velocity 46 effect on vacuum manifold pressure 45 for optimum sensitivity 35 maximum for diffusion pump MSD 16 maximum for turbo pump MSD 16 measuring with the MSD 34 46 Column installation tool 28 Column nut leaking 89 part numbers 20 28 Columns conditioning 18 24 installing 15 30 installing in a split splitless inlet 22 installing in the GC MSD interface 26 28 table of size pressure and flow 1...

Page 283: ...0 checking 110 replacing 116 Disassembling the ion source 148 Drawout plate and cylinder 222 Drying cleaned ion source parts 144 E Electron multiplier EM 227 See also Detector Electronics 233 252 ac board 241 ac dc board See low voltage power supply danger to from electrostatic discharge 100 177 high voltage HED power supply 243 HP IB MS control card 240 locations of major components 235 low volta...

Page 284: ...o messages 84 ESD See Electrostatic discharge Exhaust oil trap for foreline pump 108 194 venting the foreline pump 32 F Face seals 192 Fan for high vacuum pump 199 202 cleaning 118 incorrect operation of 69 85 replacing 134 Ferrules conditioning 18 part numbers 278 Filaments 219 care 221 electron energy 219 emission current 220 parameters affecting 219 reinstalling 160 removing 158 selection 219 F...

Page 285: ...MSD interface GC keypad setting GC MSD interface temperature from 49 GC MSD interface 211 214 failure to heat up 83 heated zone controlling 212 heater 34 212 maintaining 172 part numbers 274 reinstalling a heater and sensor 175 removing the heater and sensor 173 See also GC MSD interface temperature sensor thermocouple 212 GC MSD interface temperature 34 range 212 setting from the ChemStation 42 s...

Page 286: ...ed pressure 208 Installing GC columns 15 30 Interface socket reinstalling 154 removing 148 Interface See GC MSD interface Interfacing to external devices 248 start run input 249 system ready signal 249 Ion focus 222 Ion source 218 body 218 cleaning 150 153 disassembling 148 drawout plate and cylinder 222 drying cleaned parts 153 entrance lens 222 filament care 221 filament reinstalling 160 filamen...

Page 287: ...ectronics 177 fan replacing 134 filament reinstalling 160 filament removing 158 foreline gauge reinstalling 128 foreline gauge removing 126 foreline pump oil checking and adding 102 foreline pump oil draining 104 foreline pump refilling 106 GC MSD interface 172 GC MSD interface heater and sensor reinstall ing 175 GC MSD interface heater and sensor remov ing 173 ion source heater and sensor reinsta...

Page 288: ...ths 76 incorrect mass assignments 76 isotopes missing or ratios are incorrect 75 precursors 76 Mass to charge ratio 223 Monitoring foreline pressure 36 turbo pump speed 36 vacuum manifold pressure 44 Monitors 38 Moving the MSD 62 MS error numbers 84 MSD dangerous voltages in 97 dangerously hot parts in the 98 does not turn on 68 electronics 233 hazards from chemical residue 99 interfacing to exter...

Page 289: ...6 missing 70 86 precursors 76 split tops 72 tailing 71 PFTBA perfluorotributylamine 204 Polarity dc of the mass filter 225 Power cord ac 246 foreline pump 246 receptacle 246 Power status LED 250 Power supplies high voltage HED 243 low voltage ac dc 243 Power switch 250 Pre operation checklist 32 Pressure foreline pressure too high 79 foreline pressure too low 80 indicated vs absolute 44 monitoring...

Page 290: ...ses 78 Septum bleed as a source of contamination 90 Septum leaking 89 Service agreements inside back cover Shutdown See Venting Side plate lubricating the O ring 140 O ring 192 thumbscrews 190 Signal amplifier board 239 Signal not enough to begin tune 88 Smartcard See HP IB MS control card Solvent peak effect if analyzer is on 84 85 effect on triode gauge 80 Startup failure of the MSD to 68 See al...

Page 291: ...ing or ratios are incorrect 75 LEDs are all blinking 69 lens supply fault 86 log amplifier ADC error 86 mass assignments are incorrect 76 mass filter quad heater will not heat up 83 mass spectral symptoms 75 78 MSD does not turn on 68 MSD is on but status LEDs are all blinking 69 no peaks 70 86 peak widths are inconsistent 76 peaks are fronting 71 peaks are tailing 71 peaks have flat tops 72 peaks...

Page 292: ...o 60 ignition of hydrogen by 44 206 208 implosion hazard 44 monitoring high vacuum pressure 44 reinstalling 138 removing 136 shield 206 turning on 44 Troubleshooting 65 92 See also Symptoms of malfunctions Tune report 48 Tuning 48 cannot begin 88 compound 204 See also Autotune See also the online help in the software Turbo pump controller 252 Turbomolecular turbo pump 202 monitoring the speed of 3...

Page 293: ... vent 204 Vent cycle See Venting Vent cycle See Venting Vent program See Venting Vent program See Venting Vent valve 204 lubricating the O ring 142 Venting ChemStation control of 32 damage to MSD from incorrect 34 if ChemStation is not working 64 normal 52 Vial calibration 204 See also Calibration vial Voltages dangerous 97 W Warnings inside front cover Warranty claims inside back cover Warranty i...

Page 294: ...294 Index ...

Page 295: ...are hardware interfacing or consumables 3 Unauthorized modifications or misuse 4 Operation outside of the environmental and electrical specifications for the product 5 Improper site preparation and maintenance 6 Customer induced contamination or leaks This warranty may be modified in accordance with the laws of your country Please consult your local HP office for the period of the warranty for shi...

Page 296: ...294 Chapter ...

Page 297: ...H Manual Part Number G1099 90027 Copyright 1998 Hewlett Packard Printed in USA 11 98 ...

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