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Agilent Technologies 7000 Triple Quadrupole GC/MS Скачать руководство пользователя страница 62

62

Troubleshooting and Maintenance Manual

3

CI Troubleshooting

Signal-Related Symptoms

This section describes symptoms related to the signal. The symptom may be
too much signal, too little signal, a noisy signal, or an incorrect signal.
Signal-related symptoms are generally observed during tuning but may also be
observed during data acquisition.

Error messages in autotune due to insufficient signal may vary.

The following symptoms are covered in more detail in this section:

•

No peaks. See

.

•

No or low reagent gas signal. See

•

No or low PFDTD signal. See

.

•

Excessive noise. See

•

Low signal-to-noise ratio. See

•

Large peak at

m/z

19. See

.

•

Peak at

m/z

.

No peaks

When troubleshooting “no peaks” it is important to specify what mode of
operation is being used and what expected peaks are not being seen. Always
start with methane PCI and verify presence of reagent ions.

No reagent gas peaks in PCI

If MS has been working well and nothing seems to have been changed

•

Wrong tune file loaded, or tune file corrupted

•

Wrong ion polarity (there are no reagent ions visible in NCI)

•

No reagent gas flow; look for background ions and check pressure

•

Wrong reagent gas selected for the tune file (looking for wrong ions)

•

Large air leak

•

Dirty ion source

•

Poor vacuum (pump problem). See

.

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Содержание 7000 Triple Quadrupole GC/MS

Страница 1: ...Agilent Technologies Agilent 7000 Triple Quadrupole GC MS System Troubleshooting and Maintenance Manual...

Страница 2: ...ies of merchantability and fitness for a par ticular purpose Agilent shall not be liable for errors or for incidental or consequential damages in connec tion with the furnishing use or per formance of...

Страница 3: ...ydrogen Safety 15 Safety and Regulatory Certifications 20 Intended Use 23 Cleaning Recycling the Product 23 Liquid Spills 23 Moving or Storing the MS 23 2 General Troubleshooting Troubleshooting Tips...

Страница 4: ...ng the Mainframe 80 Maintaining the Vacuum System 93 Maintaining the Analyzers and Collision Cell 107 Maintaining the GC MS Interface 115 Maintaining the Electronics 119 5 CI Maintenance To Minimize F...

Страница 5: ...Vent Valve 141 7 Analyzers and Collision Cell Overview 146 EI Ion Source 148 CI Ion Source 150 Filaments 152 Other Source Elements 154 Quadrupole Mass Filters 156 Post and Pre Filters 159 Collision C...

Страница 6: ...ol Card Smartcard 4 176 Power Supplies 177 Back Panel Connectors 178 Interfacing to External Devices 180 9 Replacement Parts To Order Parts 184 Electronics 185 Local Control Panel 189 Vacuum System 19...

Страница 7: ...maintenance of the Agilent Technologies 7000 Triple Quadrupole Mass Spectrometer MS system It is often referred to in this document as the 7000 Triple Quad GC MS This manual assumes familiarity with t...

Страница 8: ...brant CC Collision cell CI Chemical ionization CID Collision induced dissociation DC Direct current DFTPP Decafluorotriphenylphosphine calibrant DIP Direct insertion probe EI Electron impact EM Electr...

Страница 9: ...fluoronaphthalene sample PCI Positive chemical ionization PFDTD Perfluoro 5 8 dimethyl 3 6 9 trioxydodecane calibrant PFTBA Perfluorotributylamine calibrant QQQ Triple quadrupole Quad Quadrupole mass...

Страница 10: ...onic upgrades for the EI source and HED available Local control panel LCP for locally monitoring the MS Physical description The 7000 Series Triple Quad GC MS is a rectangular box approximately 47 cm...

Страница 11: ...oxygen water hydrocarbons and sulfur compounds The MS CI system has been optimized to achieve the relatively high source pressure required for CI while still maintaining high vacuum in the collision c...

Страница 12: ...Introduction Triple Quad GC MS Hardware Description Figure 1 is an overview of a typical 7000 Triple Quad GC MS system Figure 1 7000 Triple Quad MS ALS 7000 Series Triple Quad MS Local control panel M...

Страница 13: ...ment The internal wires and cables connected to these boards The wires for any heater oven detector inlet or valve box Electrostatic discharge is a threat to MS electronics The printed circuit boards...

Страница 14: ...e standard foreline pump can be a fire hazard Oily rags paper towels and similar absorbents in the oil pan could ignite and damage the pump and other parts of the MS WARNING Be careful when working be...

Страница 15: ...operation Dangers include but are not limited to Combustion of leaking hydrogen Combustion due to rapid expansion of hydrogen from a high pressure cylinder WARNING The use of hydrogen as a GC carrier...

Страница 16: ...that column fittings should always be either connected to a column or have a cap or plug installed Table 2 Hydrogen accumulation mechanisms Mechanism Results Mass spectrometer turned off A mass spect...

Страница 17: ...be fairly rapid Power failure If the power fails both the GC and mass spectrometer shut down The flow of carrier gas however is not necessarily shut down As described previously in some GCs a power fa...

Страница 18: ...autions Turn off the hydrogen at its source every time you shut down the GC or MS Do not use hydrogen as a collision cell gas WARNING You MUST make sure the top thumbscrew on the front analyzer side p...

Страница 19: ...the system has restarted by itself 1 Immediately turn off the hydrogen at its source 2 Turn off the GC 3 Turn off the MS and allow it to cool for 1 hour 4 Eliminate all potential sources of ignition...

Страница 20: ...et appareil ISM est conforme a la norme NMB 001 du Canada The 7000 Series Triple Quad GC MS is designed and manufactured under a quality system registered to ISO 9001 Information The Agilent Technolog...

Страница 21: ...e to comply with these precautions violates safety standards of design and the intended use of the instrument Agilent Technologies assumes no liability for the customer s failure to comply with these...

Страница 22: ...adio or antenna 2 Move the device away from the radio or television 3 Plug the device into a different electrical outlet so that the device and the radio or television are on separate electrical circu...

Страница 23: ...in violation of applicable laws rules or regulations Cleaning Recycling the Product To clean the unit disconnect the power and wipe down with a damp lint free cloth For recycling contact your local Ag...

Страница 24: ...24 Troubleshooting and Maintenance Manual 1 Introduction...

Страница 25: ...age 51 for help with CI specific problems For each symptom one or more possible causes are listed In general the causes listed first are the most likely causes or the easiest to check and correct This...

Страница 26: ...ect gas If the GC column was just replaced suspect air leaks or a contaminated or bleeding column Rule 2 If complex isn t working go back to simple A complex task is not only more difficult to perform...

Страница 27: ...ens when the MS is switched on The foreline pump does not start The cooling fan for the high vacuum pump does not turn on The local control panel LCP does not turn on Disconnected MS power cord No vol...

Страница 28: ...s not sealed correctly 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 See Pumpdown failure shut...

Страница 29: ...tral data No peaks If an analysis shows no chromatographic peaks only a flat baseline or minor noise run the automated tune program If the MS passes tune the problem is most likely related to the GC I...

Страница 30: ...h Injection is too large Incorrect GC inlet temperature Insufficient column flow GC MS interface temperature is too low Ion source temperature is too low Peaks are fronting Column film thickness misma...

Страница 31: ...d Other contamination Electron multiplier voltage is too high Baseline is falling A falling baseline indicates contamination is being swept away Wait until the baseline reaches an acceptable level Com...

Страница 32: ...sed 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 GC inlet This coul...

Страница 33: ...mass filter polarity Collision cell voltage This could cause a fault condition in the GC that would prevent the GC from operating Poor repeatability Dirty syringe needle Dirty GC inlet Leaking GC inl...

Страница 34: ...r sensitivity and Poor repeatability also apply to mass spectra No peaks Ion source cables not connected Bad connections to or from the detector HED power supply output cable has failed Collision cell...

Страница 35: ...t is operating Incorrect tune file inappropriate parameters No voltage to extractor lens if using extractor EI source Peaks have precursors The tune report lists the size of the precursors for the tun...

Страница 36: ...absolute abundances at high masses Sensitivity at high masses can be excellent even if the relative abundance of m z 502 is near 1 If your MS produces low absolute abundances at high masses refer to t...

Страница 37: ...sses 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 MS to warm up and pump down Analyzer chamb...

Страница 38: ...oo high If the pressure you observe for a given column flow has increased over time check the following Column carrier gas flow is too high Collision cell gas flow is too high Air leak usually the sid...

Страница 39: ...hed carrier gas tubing Foreline gauge is not working correctly This could create a fault condition in the GC that would prevent the GC from operating Analyzer chamber pressure is too low If the pressu...

Страница 40: ...heater cartridge is not connected Ion source temperature sensor is not connected Ion source heater failed burned out or shorted to ground Ion source temperature sensor failed Source power cable is no...

Страница 41: ...tered in wrong heated zone GC MS interface has not had enough time to reach temperature setpoint GC is off GC experienced a fault and needs to be reset GC MS interface heater sensor cable is not conne...

Страница 42: ...filter quad contacts are shorted or otherwise not working correctly Mass filters are not working correctly MS electronics are not working correctly Difficulty with the electron multiplier supply Larg...

Страница 43: ...the MS off and back on to remove this error message Be sure the turbo pump has slowed down before switching off the MS The message will reappear if the underlying problem has not been corrected Large...

Страница 44: ...d Calibration vial s empty or almost empty Excessive pressure in the analyzer chambers Air leak Signal cable is not connected Electrical leads to the detector are not connected correctly HED power sup...

Страница 45: ...s not ready Turbo pump is on but has not had enough time 10 minutes to reach 80 of its normal operating speed Turbo pump is not working correctly Foreline pump has not reached its target of 300 mTorr...

Страница 46: ...ctly There is not enough signal to begin tune Corrupted tune file Poor mass axis calibration Width gain or offset is too high Calibration vial s empty or almost empty Excessive pressure in the analyze...

Страница 47: ...z 14 and 16 Poor sensitivity Low relative abundance of m z 502 this varies with the tune program used Leaks can occur in either the GC or the MS The most likely point for an air leak is a seal you rec...

Страница 48: ...in the MS Contamination originating in the GC typically comes from one of these sources Column or septum bleed Dirty GC inlet GC inlet liner Contaminated syringe Poor quality carrier gas Dirty carrier...

Страница 49: ...pound 31 Methanol Cleaning solvent 43 58 Acetone Cleaning solvent 78 Benzene Cleaning solvent 91 92 Toluene or xylene Cleaning solvent 105 106 Xylene Cleaning solvent 151 153 Trichloroethane Cleaning...

Страница 50: ...50 Troubleshooting and Maintenance Manual 2 General Troubleshooting...

Страница 51: ...Troubleshooting Tips and Tricks 53 Air Leaks 54 Pressure Related Symptoms 58 Signal Related Symptoms 62 Tuning Related Symptoms 70 This chapter outlines the troubleshooting of Agilent 7000 Series Trip...

Страница 52: ...ith EI if the MS tunes well and no air leak is present sample sensitivity problems should be addressed by GC inlet maintenance first Wrong reagent gas Reagent gas not hooked up or hooked up to wrong r...

Страница 53: ...gas suspect the tune file you have loaded in memory Is it the appropriate file for your mode of operation Rule 2 If complex isn t working go back to simple A complex task is not only more difficult to...

Страница 54: ...s calibrated for nitrogen so measurements are not accurate in absolute terms Familiarize yourself with the measurements on your system under operating conditions Watch for changes that may indicate a...

Страница 55: ...he base peak should be at m z 272 If the abundance of m z 238 is much greater than that of m z 272 you have an air leak How do I find the air leak 1 See Figure 3 and Table 4 2 Look for the last seal t...

Страница 56: ...as flow paths Leaks into the analyzer chamber are not likely to be seen in CI because of the higher pressure inside the ionization chamber 6 Half split the system Close valves starting at the gas sele...

Страница 57: ...ictor Calibration vial Shutoff valve GC MS interface GC column CI ion source Table 4 Flow module valve state diagram Result Gas A flow Gas B flow Purge with Gas A Purge with Gas B Pump out flow module...

Страница 58: ...served readings They were taken with the following set of conditions Source temperature 300 C Quad temperature 150 C Interface temperature 280 C to 320 C Helium carrier gas flow 1 mL min Table 5 Typic...

Страница 59: ...Check for and correct any leaks See Air Leaks on page 54 The foreline pump is not working properly For the standard foreline pump replace the pump oil If that does not help or for the dry foreline pum...

Страница 60: ...low as appropriate Verify that reagent ion ratios are correct Air leak Run Methane Pretune See the Operation Manual Visible peak at m z 32 indicates air in the system Check for and correct any leaks S...

Страница 61: ...obutane or ammonia The valve on the reagent gas bottle is closed Check and if necessary open the valve on the reagent gas bottle The reagent gas supply is empty Check and if necessary replace the reag...

Страница 62: ...l See page 66 Excessive noise See page 67 Low signal to noise ratio See page 67 Large peak at m z 19 See page 68 Peak at m z 32 See page 69 No peaks When troubleshooting no peaks it is important to sp...

Страница 63: ...not sealed big air leak No calibrant in vial Defective calibration valve s Air leak in carrier or reagent gas path No reagent gas peaks in NCI Reagent gases do not ionize in NCI look for background io...

Страница 64: ...Reagent gas supply tubing is blocked kinked pinched or disconnected Inspect and if necessary repair or replace the reagent gas supply tubing Wrong filament wires are connected to filament Make sure t...

Страница 65: ...ion source probably needs to be cleaned See Chapter 4 General Maintenance on page 75 for more information Ion source wires are not connected or incorrectly connected Inspect the repeller Make sure th...

Страница 66: ...ake sure the regulator on the methane supply is set to 10 psig 70 kPa The CI ion source is dirty Clean the ion source See Chapter 5 CI Maintenance on page 123 for more information The calibration valv...

Страница 67: ...eck the pressure on the high vacuum gauge controller Air leak Run Methane Pretune in PCI Large peak at m z 32 indicates air in the system Check for and correct any leaks See Air Leaks on page 54 Satur...

Страница 68: ...ystem was not baked out sufficiently after it was last vented Bake out the system as described in Chapter 4 General Maintenance on page 75 Moisture left over in the reagent gas supply tubing and flow...

Страница 69: ...lines and flow module for at least 60 minutes See the Operation Manual Air leak Check for leaks and correct any that you find See Air Leaks on page 54 After all leaks have been corrected clean the io...

Страница 70: ...n describes symptoms related to tuning Most symptoms involve difficulties with tuning or with the results of tuning The following symptoms are covered in this section CI ion ratio is difficult to adju...

Страница 71: ...sent purge the reagent gas supply lines and bake out the MS Continued presence of a large peak at m z 32 may indicate an air leak After correcting the problems you may need to clean the ion source Air...

Страница 72: ...inflection point If the curve is linear with a positive slope and no inflection point and the EMV is high the filament has stretched to the point where it does not line up with the hole in the ion sou...

Страница 73: ...7 ion ratio for methane is incorrect The correct ratio should be between 1 5 and 5 0 If the ion ratio is incorrect adjust it See the Operation Manual The CI ion source is dirty Clean the ion source Se...

Страница 74: ...tune parameters The CI ion source is dirty Clean the ion source See Chapter 5 CI Maintenance on page 123 for more information Air leak Run Methane Pretune in PCI A visible peak at m z 32 indicates ai...

Страница 75: ...and Maintenance Manual Agilent Technologies 4 General Maintenance Before Starting 76 Maintaining the Mainframe 80 Maintaining the Vacuum System 93 Maintaining the Analyzers and Collision Cell 107 Main...

Страница 76: ...ariations from normal operation and to take corrective action Table 6 Maintenance schedule Task Every week Every 6 months Every year As needed Tune the MS X Check the foreline pump oil level X Check t...

Страница 77: ...nd cables between these boards and the connectors on the back panel of the MS Some connectors on the back panel for example the foreline power receptacle Normally all of these parts are shielded by sa...

Страница 78: ...o not use this oil trap For all foreline pumps install a hose to take the exhaust from the foreline pump outdoors or into a fume hood vented to the outdoors For the foreline pump this requires removin...

Страница 79: ...printed circuit boards or when you work on components with wires contacts or cables connected to printed circuit boards always use a grounded antistatic wrist strap and take other antistatic precauti...

Страница 80: ...he front right analyzer window cover 1 Pull out from the top of the window and forward from the bottom The cover is held in place by magnets 2 Lift the window forward and off the MS To remove the fron...

Страница 81: ...el 3 Remove the screws that hold the left side cover in place 4 Push the cover slightly to the rear to disengage the two right side tabs and then lift it off the MS To remove the left rear cover 1 Ope...

Страница 82: ...82 Troubleshooting and Maintenance Manual 4 General Maintenance Figure 4 MS covers Left side panel Front bottom cover Left side cover Top cover Front right analyzer window cover Left rear cover...

Страница 83: ...fore turning off the MS power If the foreline pump is off hydrogen will accumulate in the MS and an explosion may occur Read Hydrogen Safety before operating the MS with hydrogen carrier gas WARNING W...

Страница 84: ...To remove the MS covers on page 80 8 Finger tighten the side plate thumbscrews for both analyzers Figure 5 9 Switch the MS on to establish a rough vacuum 10 When you hear the hissing sound of the pum...

Страница 85: ...t be moved with the MS Make sure the MS remains upright and is never tipped on its side or inverted Figure 5 Side plate thumbscrews Side plate thumbscrews CAUTION The MS must remain upright at all tim...

Страница 86: ...from the GC until you have access to the GC MS interface cable Figure 6 WARNING Make sure the GC MS interface and the analyzer zones are cool below 100 C before you vent the MS A temperature of 100 C...

Страница 87: ...connect the GC MS interface cable Disconnecting the cable with the GC on can cause a fault condition 8 Continue to move the MS until you have access to the part requiring maintenance Reconnection 1 Po...

Страница 88: ...ation Manual 7 Turn on the GC Enter appropriate temperature setpoints for the GC MS interface and GC oven WARNING Make sure your MS meets all the conditions listed in the Pump Down section of the Agil...

Страница 89: ...ise to loosen it Figure 7 Do not remove the collar 5 Pull the calibration vial out You may feel some resistance due to the O ring around the vial tube section 6 Syringe or pipette PFTBA into the vial...

Страница 90: ...he MS Tune icon to display the GC QQQ Tune dialog box Select the Manual Tune tab then select the Ion Source tab to display the ion source parameters 12 Turn off the Emission by clicking in the check b...

Страница 91: ...a carrier gas do not start carrier gas flow until the MS has been pumped down If the vacuum pumps are off hydrogen will accumulate in the MS and an explosion may occur Read Hydrogen Safety before ope...

Страница 92: ...the calibration and vent valve assembly and tighten the screws that hold it in place 4 Reconnect the calibration valve cable to the connector 5 Remove the vial from the new calibration valve See To r...

Страница 93: ...these tasks as scheduled can result in decreased instrument performance It can also result in damage to your instrument Other procedures Tasks such as replacing an ion vacuum gauge should be performe...

Страница 94: ...fety before operating the MS with hydrogen carrier gas WARNING The turbo pump can cause burns if touched when operating Make sure the pump has time to cool before touching CAUTION Never vent the MS by...

Страница 95: ...r Installation analyzer chamber gauge Installation is the reverse of the removal procedure Removal foreline pump gauge 1 Vent the MS See the Agilent 7000 Series Triple Quad GC MS Operation Manual 2 Se...

Страница 96: ...96 Troubleshooting and Maintenance Manual 4 General Maintenance Figure 8 Ion vacuum gauge cables Cable to analyzer chamber pressure gauge Cable to forepump pressure gauge Wingnut...

Страница 97: ...s The foreline pump oil should be almost clear If the oil level is near or below the lower line follow steps 2 through 6 to add foreline pump oil If your MS is nearing its scheduled time for replaceme...

Страница 98: ...ump fluid until the oil level in the window is near but not above the upper line 5 Reinstall the fill cap 6 Pump down the MS See the Agilent 7000 Series Triple Quad GC MS Operation Manual Figure 9 Sta...

Страница 99: ...sible location The foreline pump may be located on the floor on the lab bench next to or behind the MS or under the analyzer chamber at the back of the MS 3 Place a book or other object under the back...

Страница 100: ...to bring the oil level near the upper line 6 Reinstall the fill cap 7 If necessary slide the foreline pump back under the analyzer chamber The foreline pump may be located on the floor on the lab ben...

Страница 101: ...6 Remove the four fan screws and the safety grill Remove the fan Keep the screws 7 Connect the fan wiring to the new fan 8 Install the new fan with the flow arrow on the side pointing toward the pump...

Страница 102: ...102 Troubleshooting and Maintenance Manual 4 General Maintenance Figure 10 Replacing the turbo pump fan Fan Screen Wires to extender cable...

Страница 103: ...er 3 Use a clean lint free cloth or glove to spread a thin coat of high vacuum grease only on the exposed surface of the O ring Figure 11 WARNING The analyzer GC MS interface and other components in t...

Страница 104: ...hamber 6 Repeat this procedure for the other analyzer chamber 7 Pump down the MS See the Agilent 7000 Series Triple Quad GC MS Operation Manual CAUTION Do not use anything except the recommended vacuu...

Страница 105: ...See the Agilent 7000 Series Triple Quad GC MS Operation Manual 2 Completely remove the vent valve knob Figure 12 3 Inspect the O ring If the O ring appears damaged replace it 4 Use a clean lint free...

Страница 106: ...the MS See the Agilent 7000 Series Triple Quad GC MS Operation Manual Figure 12 Vent valve O ring Vent valve knob Vent valve O ring CAUTION Be very careful when reinstalling the vent valve knob It is...

Страница 107: ...ntenance Precautions Cleanliness Keep components clean during analyzer maintenance Analyzer maintenance involves opening the analyzer chamber and removing parts from the analyzer During analyzer maint...

Страница 108: ...e done by a trained Agilent Technologies service representative The HED insulator must never be touched More information is available See the Agilent 7000 Series Triple Quad GC MS Operating Manual for...

Страница 109: ...yzer chamber See the Agilent 7000 Series Triple Quad GC MS Operation Manual 3 Remove the ion source See To remove the EI ion source in the Agilent 7000 Series Triple Quad GC MS Operation Manual 4 Remo...

Страница 110: ...See Figure 13 6 Disassemble the repeller assembly by removing the repeller nut washers ceramic insulators and repeller See Figure 13 7 Unscrew the interface socket from the source body A 10 mm open en...

Страница 111: ...o the ion source 7 Reconnect the heater and temperature sensor wires to the feedthrough board 8 Close the analyzer chamber 9 Pump down the MS See the Agilent 7000 Series Triple Quad GC MS Operation Ma...

Страница 112: ...dthrough board 4 Remove the mass filter heater assembly from the mass filter radiator by removing the two screws See Figure 14 for the front mass filter The rear mass filter heater sensor removal is s...

Страница 113: ...gure 14 for replacing the front mass filter heater sensor The rear mass filter heater sensor is similar 3 Connect the heater and temperature sensor wires to the feedthrough board 4 Close the analyzer...

Страница 114: ...114 Troubleshooting and Maintenance Manual 4 General Maintenance Figure 14 Mass filter heater and sensor Mass filter radiator Heater sensor assembly Front analyzer shown rear analyzer is similar...

Страница 115: ...Rarely the heater cartridge in the GC MS interface fails In those cases it is necessary to replace the heater and sensor This section contains procedures for removing the heater and sensor and instal...

Страница 116: ...gently pry open the slot in the heater sleeve to loosen the heater sleeve from the interface 8 Loosen the setscrew and remove the heater and temperature sensor from the heater sleeve Heat and oxidatio...

Страница 117: ...if it is damaged Screwdriver Torx T 15 8710 1622 Hex driver 1 5 mm 8710 1570 CAUTION Installing a new heater and sensor in a damaged heater sleeve will result in poor performance of the heated zone an...

Страница 118: ...res from the heater and sensor pass through the cutout in the interface cover 6 Reconnect the MS to the GC See step 1 on page 87 7 Reconnect the GC MS interface cable to the GC Reinstall the capillary...

Страница 119: ...ition 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 ESD to sen...

Страница 120: ...ies that have been removed from the MS This includes the analyzer More information is available If you need more information about the functions of electronic components refer to Chapter 8 Electronics...

Страница 121: ...ill already be off but for safety you should switch off the MS and unplug the power cord It is not necessary to allow air into the analyzer chamber 2 The fuse holders are on the back panel Turn one of...

Страница 122: ...122 Troubleshooting and Maintenance Manual 4 General Maintenance...

Страница 123: ...mize Foreline Pump Damage from Ammonia 124 To Replace the Methane Isobutane Gas Purifier 125 To Clean the Reagent Gas Supply Lines 126 To Refill the CI Calibrant Vial 127 This chapter describes mainte...

Страница 124: ...e to run samples while the pump is ballasting 3 Close the ballast valve by aligning the 0s Leaving the ballast valve open all the time will result in loss of pump oil and damage to the pump CAUTION On...

Страница 125: ...ced metal of the oxygen and moisture traps Procedure 1 To install the methane isobutane gas purifier follow the instructions on the label for installation and replacement intervals 2 Disconnect the fi...

Страница 126: ...ng the instructions on the label 3 Connect one end of the tubing to a supply of clean dry nitrogen and turn on gas flow 4 Use the heat gun to warm the tubing starting at the supply end and working you...

Страница 127: ...MS next to the GC See page 86 10 Reinstall the capillary column 11 Pump down the MS 12 In Instrument Control panel select the MS Tune icon to display the GC QQQ Tune dialog box Select the Manual Tune...

Страница 128: ...er removing the calibrant vial you must purge the calibration valve Failure to do so will result in severe contamination of the ion source and damage to the filament and electron multiplier Figure 18...

Страница 129: ...m Overview 130 Vacuum System Components 131 Common Vacuum System Problems 132 Foreline Pump 133 Turbo Pump 135 Analyzer Chambers 135 Side Plates 136 Vacuum Seals 137 Foreline Gauge 139 Turbo Pump and...

Страница 130: ...reach the detector Operation at high pressures also would damage analyzer components The 7000 Series Triple Quad GC MS uses two vacuum pumps to obtain the vacuum levels needed The foreline pump creat...

Страница 131: ...Collision cell cover Side plates analyzer doors and front and rear end plates Vacuum seals Calibration valve and vent valve Vacuum control electronics Vacuum gauges and gauge control electronics Each...

Страница 132: ...system will shut down both the high vacuum and the foreline pump if the system fails to pump down correctly It takes approximately 10 minutes for the foreline pump to achieve 300 mTorr which then star...

Страница 133: ...turned on The foreline pump has a built in check valve to help prevent backstreaming in the event of a power failure The foreline pump is usually on the floor below the MS An oil trap not shown is ava...

Страница 134: ...p stops only foreline pump oil It does not trap or filter out toxic chemicals If you are using toxic solvents or analyzing toxic chemicals remove the oil trap do not use the trap if you are using a CI...

Страница 135: ...rom an aluminum alloy Large openings in the side front rear and top of the manifold are closed by plates and sealed by O rings Ports in the manifold and the plates provide attachment points for the io...

Страница 136: ...trical feedthroughs are built into the side plates Wires connect the feedthroughs to analyzer components Thumbscrews are located at each end of the side plates We recommend that the thumbscrews be loo...

Страница 137: ...d on for pumpdown to ensure a good seal The front and rear end plates are screwed onto the manifold and should not need to be removed The GC MS interface fastens to the manifold with three screws The...

Страница 138: ...al The high voltage HED feedthrough seal is an O ring that is compressed against the side plate by a threaded collar Figure 22 Vacuum seals Side plate O ring seal KF seal with internal centering ring...

Страница 139: ...it of the turbo pump The primary function of the foreline gauge is pump control When the foreline pump has reduced the pressure in the analyzer chamber to below 300 mTorr 0 3 Torr the turbo pump is au...

Страница 140: ...tlet A controller regulates 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 MS The fan draws air from outsi...

Страница 141: ...I operation PFTBA is required for automatic tuning of the MS CI Calibration Valve The CI tuning compound is perfluoro 5 8 dimethyl 3 6 9 trioxidodecane PFDTD The CI calibration valve is part of the re...

Страница 142: ...and Maintenance Manual 6 Vacuum System Figure 23 Triple quad vent valve and EI calibration valve Figure 24 CI calibration valve EI calibration valve Vent valve EI calibration vial CI calibration valve...

Страница 143: ...Vacuum System 6 Troubleshooting and Maintenance Manual 143 Figure 25 Vent valve Vent valve knob O ring Air passage Valve closed Valve open Valve open too far...

Страница 144: ...144 Troubleshooting and Maintenance Manual 6 Vacuum System...

Страница 145: ...nance Manual Agilent Technologies 7 Analyzers and Collision Cell Overview 146 EI Ion Source 148 CI Ion Source 150 Filaments 152 Other Source Elements 154 Quadrupole Mass Filters 156 Post and Pre Filte...

Страница 146: ...rce the sample molecules are ionized and fragmented The resulting ions are repelled from the ion source into the front quadrupole mass filter The selected ions pass through the filter and post filter...

Страница 147: ...collision cell to the rear analyzer It also aligns the rear of the collision cell with the rear analyzer The rear analyzer The rear analyzer consists of the rear quadrupole the detector and a heater s...

Страница 148: ...itive voltage on the repeller pushes the positive ions into the lens stack where they pass through several electrostatic lenses These lenses concentrate the ions into a tight beam which is directed in...

Страница 149: ...Maintenance Manual 149 The CI ion source is similar in design but critical dimensions are different Do not interchange parts Figure 27 Ion source structure Entrance lens Filament Drawout cylinder Dra...

Страница 150: ...connections for the other wires The holes in the ion source electron entrance and ion exit are very small 0 5 mm making it possible to pressurize the ionization chamber Both the source body and the pl...

Страница 151: ...Manual 151 Figure 29 CI ion source exploded view Setscrew CI repeller CI repeller insulator CI filament CI ion source heater assembly CI dummy filament CI interface tip seal CI lens insulator CI ion...

Страница 152: ...eneral instrument shutdown Three parameters affect the filaments filament selection Filament filament emission Emission current and electron energy EIEnrgy Filament selection The filament selection pa...

Страница 153: ...acuum before turning on the analyzer especially after any maintenance was performed When setting up data acquisition parameters set the solvent delay so that the analyzer will not turn on while the so...

Страница 154: ...e optimum setting Setting repeller voltage too low results in poor sensitivity and poor high mass response Setting repeller voltage too high results in precursors poor mass filtering and poor low mass...

Страница 155: ...vity at higher masses Incorrect ion focus adjustment results in poor high mass response Entrance lens The entrance lens Figure 27 is at the entrance to the quadrupole mass filter This lens minimizes t...

Страница 156: ...ary for mass selection Opposing rods are connected adjacent rods are electrically isolated One pair has positive voltages applied the other negative A combined direct current DC and radio frequency RF...

Страница 157: ...cts the ratio of DC voltage to RF frequency on the mass filter Higher offset yields narrower peaks Width offset generally affects peak widths equally at all masses Mass gain Mass gain controls the mas...

Страница 158: ...rom the radiator If absolutely necessary that is if the only alternative is replacement the quadrupole can be cleaned Cleaning must be performed by Agilent Technologies service personnel CAUTION Never...

Страница 159: ...front analyzer and the beginning of the rear analyzer They have three purposes Support and align the collision cell between the two analyzers Direct the selected ion stream into the collision cell Dir...

Страница 160: ...s from the front analyzer may interact with the reaction gas to form product ions When the front and rear analyzer doors close alignment pins on the collision cell engage the post and pre filters They...

Страница 161: ...center of the quadrupole 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...

Страница 162: ...ed increases over time If the EM voltage must always be set at or near 3000 VDC to complete Autotune with no other probable cause it may need to be replaced A warning message will alert you if more th...

Страница 163: ...Hunter Workstation software In selecting the temperatures to use consider the following Higher temperatures help keep the analyzer clean longer Higher ion source temperatures result in more fragmentat...

Страница 164: ...Maintenance Manual 7 Analyzers and Collision Cell Figure 34 Heaters and radiators Mass filter radiator Mass filter heater assembly Ion source radiator Ion source heater assembly Front analyzer shown R...

Страница 165: ...Supplies 177 Back Panel Connectors 178 Interfacing to External Devices 180 The following assemblies make up the MS electronics Except for the Back panel and connectors and Interfacing to external devi...

Страница 166: ...witch is located on the lower left of the front of the MS It is separate from the electronics module and is connected via a cable It is used to turn the MS and foreline pump on and off CAUTION Do not...

Страница 167: ...these functions Passes voltages generated on the main board and the filament drive board to elements in the ion source Generates and adjusts filament emission current and electron energy as controlled...

Страница 168: ...ge applied to the quadrupole mass filters according to a signal from the main board The amplitude of this voltage is proportional to the mass selected Generate the DC component of the voltage applied...

Страница 169: ...ubleshooting and Maintenance Manual 169 Collision Cell Board This board has two functions Generates the controlling voltages for the hexapole Creates the RF signal for the collision cell Figure 38 Col...

Страница 170: ...eshooting and Maintenance Manual 8 Electronics Detector Board The detector board performs these functions Passes high voltage to the detector Receives and passes on the detector signal Figure 39 Detec...

Страница 171: ...odule can be replaced if necessary by your Agilent Technologies service representative The electronics module contains Main Board 1 Main Board 2 Signal amplifier board LAN MS control card Smartcard 4...

Страница 172: ...172 Troubleshooting and Maintenance Manual 8 Electronics Figure 40 Electronics module side 1 HED supply Toroid transformer AC board Low voltage power supply...

Страница 173: ...perform these functions Receive and decode digital instructions from the LAN MS control card Send digital information to the LAN MS control card Generate voltages for the ion source lenses and the col...

Страница 174: ...nal amplifier board The log amplifier board amplifies the output of the detector It produces an output voltage of 0 to 10 volts DC proportional to the logarithm of the input current of 3 picoamps to 5...

Страница 175: ...in 10 minutes after beginning pumpdown or if the speed drops below 50 during operation the controller shuts off the turbo pump and the AC board shuts off the foreline pump Pumpdown failure shutdown Th...

Страница 176: ...ntrol Card Smartcard 4 The LAN MS control card is located to the left of Main Boards 1 and 2 on the electronics panel The LAN MS control card has two main functions Provide a communication interface b...

Страница 177: ...the 10 000 volts DC for the high energy dynode HED in the detector for the EI MS The HED power supply also provides 600 VDC for the detector focus lens Due to the high impedance of this circuit measur...

Страница 178: ...Panel Connectors The back panel contains several connectors Figure 42 and the four primary fuses Figure 42 Back panel connections Fuses Turbo pump power Foreline pump power Turbo controller fan Main...

Страница 179: ...eceptacle This provides power and control for the turbo pump controller and the turbo pump cooling fan Main power cord receptacle The AC power cord brings in all electrical power for the MS The power...

Страница 180: ...and the MS 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...

Страница 181: ...cted between the ready and ground pins on the remote start connector on the MS Start run input The best way to generate a start run signal is to use the remote start connector on the GC Since remote s...

Страница 182: ...182 Troubleshooting and Maintenance Manual 8 Electronics...

Страница 183: ...ystem 190 Analyzer 195 EI GC MS Interface 205 Consumables and Maintenance Supplies 206 Additional CI Parts 210 This chapter lists parts that can be ordered for use in maintaining your 7000 Series Trip...

Страница 184: ...ications as new parts Rebuilt assemblies can be identified by their part numbers The first two digits of the second part of the part number are 69 or 89 such as xxxxx 69xxx or xxxxx 89xxx Rebuilt asse...

Страница 185: ...Y Remote Start Stop Cable G1530 61200 H Remote Start Stop Cable 35900 60800 LAN Cable shielded 8121 0008 Power cord Australia New Zealand 8120 1369 Power cord Australia 15 A 8120 6900 Power cord Chin...

Страница 186: ...rough G2571 60806 Cable RFPA DC power G7000 60807 Cable Fan extension G1960 60846 Cable Power supply DC G7000 60820 Cable Power supply AC G7000 60821 Cable LCP G7000 60808 Cable Quad driver 1 data G70...

Страница 187: ...1 GB memory 0960 2490 SDRAM 256 MB 1818 8947 PLX board G2571 61001 4 GByte USB drive G7000 80200 Main board G7000 61001 SC4 bus G7000 61008 Log amp G3170 65101 Extender board PCI 32 bit 0403 1169 Tabl...

Страница 188: ...power switch Table 11 Fuses and power switches Description Part number Fuse 8A slow blow electronics fans and power supplies 2110 0969 Fuse 12 5A slow blow foreline and turbo pump 2110 1398 Power swit...

Страница 189: ...nel This section lists replaceable parts for the LCP and related covers See Figure 44 Figure 44 Local control panel replacement parts Table 12 LCP and related parts Item Description Part number 1 LCP...

Страница 190: ...for front and rear end plates 0905 1441 GC MS interface O ring 0905 1405 HED feedthrough G1099 80012 HED feedthrough O ring 0905 0490 KF10 16 seal foreline pump inlet and turbo pump outlet 0905 1463...

Страница 191: ...e pump 120V G3170 89025 Rebuilt standard foreline pump 220V G3170 89026 Rebuilt standard foreline pump 200V Japanese G3170 89024 Exch Avail RV5 pump 200V Inland G7000 80021 Exch Avail RV5 pump 115V In...

Страница 192: ...pter exhaust fitting G3170 80006 O ring for oil mist filter and hose barb adapter 0905 1193 Pump oil Inland 45 6040 0621 Safety Cage kit Duo foreline pump G3170 60028 5 Standoff Pump Cage Qty 2 G3170...

Страница 193: ...Replacement Parts 9 Troubleshooting and Maintenance Manual 193 Figure 45 Foreline pump top and safety cage parts 1 6 5 7...

Страница 194: ...turbo pump outlet 0100 1551 Split flow turbo pump G7000 80010 Split flow turbo pump rebuilt G7000 89010 ISO100 seals 0100 1879 Flat washers 4 to mount pump 3050 0881 Lock washers 4 to mount pump 2190...

Страница 195: ...port G3170 00003 Ion vacuum gauge baffle G3170 00015 M3X12 TX T10 PN SQ Cone SS qty 2 0515 0664 2 EI Calibration valve assembly G3170 60204 3 Calibration vial G3170 80002 4 End plate front glass G3170...

Страница 196: ...filter contacts 4 G1099 60142 G1099 60142 Mass filter canted coil support detector end G3170 20025 Mass filter canted coil spring G1460 2724 Mass filter ceramic support source end G1099 20123 3 Mass f...

Страница 197: ...ilter contact assembly heater block G3170 20122 Screws radiator Mounting brackets quadrupole board 0515 0430 Source radiator screws 0515 1052 Screws for Quad Stop 0515 0221 Table 19 Inert EI ion sourc...

Страница 198: ...tor one piece G3170 20530 Inert EI 350 Anodized Repeller assembly G3170 60171 7 Screws for filament G1999 20021 6 Source heater assembly G3170 60177 2 Setscrew for lens stack G1999 20021 1 Source body...

Страница 199: ...Replacement Parts 9 Troubleshooting and Maintenance Manual 199 Figure 47 EI 7000 ion source 1 2 3 8 9 10 11 12 4 5 7 3 7 6...

Страница 200: ...mm G7000 20446 12 Extractor lens insulator G7000 20445 Extractor lens wire G7000 60827 9 Entrance lens G3170 20126 3 EI filament G2590 80070 EI high temp filament G2590 60053 4 Interface socket G7000...

Страница 201: ...Replacement Parts 9 Troubleshooting and Maintenance Manual 201 Figure 48 EI extractor ion source 1 2 3 8 9 10 11 12 4 5 7 3 7 6...

Страница 202: ...126 3 CI filament G1099 80053 13 CI Dummy filament G1999 60454 4 CI interface tip seal G1999 60412 10 CI Ion focus lens G1999 20443 8 CI lens insulator one piece G3170 20540 5 CI repeller G1999 20432...

Страница 203: ...Replacement Parts 9 Troubleshooting and Maintenance Manual 203 Figure 49 CI ion source 1 2 3 8 9 10 11 12 4 5 7 13 7 6 14...

Страница 204: ...assembly Description Part number EI 350 Anodized Repeller assembly G3170 60172 Inert EI 350 Anodized Repeller assembly G3170 60171 Insulator 2 required G1099 20133 Nut 5 5 mm 0535 0071 Repeller G2589...

Страница 205: ...ce column nut 05980 20066 Heater sleeve G1099 20210 Heater Sensor assembly G1099 60107 Insulation G1099 20301 Setscrew for heater sensor assembly 0515 0236 Screws M4x0 7 panhead for heater sleeve 0515...

Страница 206: ...d maintaining your MS Table 24 EI maintenance supplies Description Part number Abrasive paper 30 m 5061 5896 Alumina powder 1 kg 8660 0791 Cloths clean qty 300 05980 60051 Cloths cleaning qty 300 9310...

Страница 207: ...nose 1 5 inch nose 8710 1094 Screwdrivers Flat blade large 8730 0002 Screwdrivers Torx T 10 8710 1623 Screwdrivers Torx T 15 8710 1622 Screwdrivers Torx T 20 8710 1615 MS shipping kit G3170 60501 RV5...

Страница 208: ...id 85 15 for 0 20 and 0 25 mm id columns 5062 3508 0 5 mm id 85 15 for 0 32 mm id columns 5062 3506 0 8 mm id 85 15 for 0 53 mm id columns 5062 3538 For the GC inlet 0 27 mm id 90 10 for 0 10 mm id c...

Страница 209: ...phthalene OFN 100 fg L 5188 5348 PFTBA 10 gram 8500 0656 Benzopheone 100 pg L 8500 5440 PFTBA sample kit 05971 60571 Foreline pump tray G1099 00015 Eval A hydrocarbons 05971 60045 Micro Ion gauge elec...

Страница 210: ...0 2 Calibration sample vial G3170 80002 Sample vial O ring 1 4 inch Viton 5180 4182 Solenoid valve and cable G1999 60452 CI cable from SC to CI Flow Module G3170 60808 Cable CI to CI Bulkhead G7000 60...

Страница 211: ...er clamp G1999 20410 Heater Sensor assembly G1099 60107 Transfer line cup cover G3170 00405 Interface insulation G1999 20401 Screws for heater clamp 0515 0383 Screws to attach interface to manifold 05...

Страница 212: ...212 Troubleshooting and Maintenance Manual 9 Replacement Parts Figure 50 CI flow control module 5 3 4 2 1...

Страница 213: ......

Страница 214: ...Agilent Technologies Agilent Technologies Inc Printed in USA September 2009...

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