Agilent Technologies 7250 Troubleshooting And Maintenance Manual
Agilent Technologies 7250 Troubleshooting And Maintenance Manual

Agilent Technologies 7250 Troubleshooting And Maintenance Manual

Accurate-mass quadrupole time-of-flight gc/ms system
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Agilent 7250 Accurate-Mass Quadrupole
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Summary of Contents for Agilent Technologies 7250

  • Page 1 Agilent 7250 Accurate-Mass Quadrupole Time-of-Flight GC/MS System Troubleshooting and Maintenance Manual...
  • Page 2 Do not proceed beyond a CAUTION notice until the indicated conditions are fully understood and met. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 3: Table Of Contents

    Safety and Regulatory Certifications Intended Use Cleaning/Recycling the Product Accidental Liquid Spillage Moving or Storing the MS General Troubleshooting Troubleshooting Tips and Tricks General Symptoms Chromatographic Symptoms Mass Spectra General Symptoms Pressure Symptoms 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 4 Large peak at m/z 238 in NCI OFN spectrum No or low reagent gas signal No or low PFDTD signal, but reagent ions are normal Excessive noise or low signal-to-noise ratio Peak at m/z 32 Tuning-Related Symptoms 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 5 CI Maintenance To Minimize Rotary Vane Foreline Pump Damage from Ammonia To Replace the Chemical Ionization Gas Purifier To Clean the Reagent Gas Supply Lines To Refill the CI Calibration Vial Vacuum System Overview 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 6 To change the exhaust silencer filter cartridge To install the IDP pump ballast To remove the IDP pump ballast Side Plate Vacuum Seals EI Calibration Valve CI Calibration Valve Replacement Parts To Order Parts 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 7 Electronics Vacuum System Analyzer GC/MS Interface Consumables and Maintenance Supplies Additional CI Parts 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 8 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 9: Introduction

    Intended Use 24 Cleaning/Recycling the Product 24 Moving or Storing the MS 24 This chapter provides general information about the Agilent 7250 Accurate-Mass Quadrupole Time-of-Flight (Q-TOF) GC/MS System, including a hardware description and general safety warnings. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 10: Abbreviations Used

    Mass spectrometer Quadrupole Octafluoronaphthalene (sample) PFTBA Perfluorotributylamine (calibrant) Q-TOF Quadrupole time-of-flight Quad Quadrupole mass filter Radio frequency RFPA Radio frequency power amplifier Time-of-flight Torr Unit of pressure, 1 mm Hg Turbo Turbomolecular vacuum pump 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 11: The 7250 Accurate-Mass Quadrupole Time-Of-Flight Gc/Ms System

    Independently GC-heated GC/MS interface Physical description The 7250 Q-TOF GC/MS is approximately 53.5 cm high, 69 cm wide, and 92 cm deep. The flight tube extends 136 cm up over the top of the instrument. The turbo pump mainframe weighs 159 kg. The weight of the attached foreline (rotary) pump is 25 kg for the DS202 rotary vane pump model, and 45 kg for the IDP model.
  • Page 12 Ionization modes The 7250 Accurate-Mass Q-TOF GC/MS can operate in EI mode using the standard LE-EI ion source or in CI mode using the optional CI MS system. In electron impact mode, the Q-TOF can operate in standard or low-energy modes.
  • Page 13: 7250 Accurate-Mass Q-Tof Gc/Ms Description

    Introduction 7250 Accurate-Mass Q-TOF GC/MS Description Figure 1 is an overview of a typical 7250 Accurate-Mass Q-TOF GC/MS system. Flight tube 8890 GC Q-TOF MS power Front right Source GC power Oven door Drawer switch grill window cover switch latch Figure 1.
  • Page 14: Side Panel Ac Power Connectors

    The foreline pump power cord receptacle located on the left side of the MS provides AC power for the foreline pump. If the power switch is off, no power is supplied to the foreline pump. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 15: Back Panel Connectors

    LAN communications connector. It carries all data communication between the PC and the MS. Directly connect a single dedicated LAN cable between the PC and the 7250 C AU T I O N Q-TOF. Do not use a LAN switch, router, or other device between the PC and the Q-TOF.
  • Page 16: Interfacing Start Events To External Devices

    On receipt of the ready signal, the desorption cycle begins. When a specific temperature is reached, the purge-and-trap closes a contact to indicate the run has started. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 17: Start Run Input

    If necessary, the remote start connector on the back of the MS can be used to send the start run signal. A contact closure between the start and ground pins will start the run if the system is ready. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 18: Important Safety Warnings

    The printed circuit boards in the MS can be damaged by electrostatic discharge. Do not touch any of the boards unless it is absolutely necessary. If you must handle them, wear a grounded wrist strap, and take other antistatic precautions. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 19 Turn the zone off after it has reached the setpoint. If you must perform maintenance on hot parts, use a wrench and wear gloves. Whenever possible, cool the part of the instrument that you will be maintaining before you begin working on it. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 20 Combustible materials (or flammable/nonflammable wicking material) placed WAR N IN G under, over, or around the foreline (roughing) pump constitutes a fire hazard. Keep the pan clean, but do not leave absorbent material such as paper towels in it. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 21: Safety And Regulatory Certifications

    This ISM device complies with Canadian ICES-001. Cet appareil ISM est conforme a la norme NMB—001 du Canada. The 7250 Q-TOF GC/MS is designed and manufactured under a quality system registered to ISO 9001. The 7250 A-TOF GC/MS is RoHS compliant.
  • Page 22 Failure 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 requirements.
  • Page 23 • Consult your equipment dealer, Agilent Technologies, or an experienced technician for assistance. Changes or modifications not expressly approved by Agilent Technologies could void the user’s authority to operate the equipment. Sound emission declaration Sound pressure Sound pressure Lp < 70 dB according to EN 27779:1991 and EN ISO 3744:1995.
  • Page 24: Intended Use

    The MS must remain upright at all times; this requires special caution when moving. The MS should not be left vented to atmosphere for long periods. For more information, see “To Move or Store the MS” on page 79. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 25: General Troubleshooting

    See the other chapters in this manual for more information. If the material in this chapter and in the online help proves insufficient to help you diagnose a problem, contact your Agilent Technologies service representative. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 26: Troubleshooting Tips And Tricks

    To determine whether an air leak is in the GC or the MS, vent the MS, remove the column, and install the blank interface ferrule. If the leak goes away, it was in the 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 27: General Symptoms

    A large air leak (usually the analyzer door open) has caused pumpdown failure. You must power cycle the MS to recover from this state. • Disconnected foreline pump power cord • Malfunctioning foreline pump • Check power switch on foreline pump 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 28 This feature helps prevent the foreline pump from sucking air through the system, which can damage the analyzer and the turbo pumps. You must power cycle the MS to recover from this state. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 29: Chromatographic Symptoms

    * This could cause a fault condition in the GC that would prevent the GC from operating. Does not pass tune • Calibration vial is empty • Excessive foreline or analyzer chamber pressure • Very dirty ion source • Calibration valve is not working correctly 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 30 Injection is too large • GC inlet pressure too high • Insufficient column flow Peaks have flat tops • Insufficient solvent delay • Incorrect scale on the display • Injection is too large 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 31 Residual air and water from a recent venting • Column bleed • Septum bleed • Splitless injection time too long (inlet is not properly swept, resulting in excess solvent on the column and slow solvent decay) 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 32 Incorrect temperatures (oven, GC/MS interface, ion source, or mass filter) • Incorrect sample concentration • Leaking GC inlet* • Dirty GC inlet • Incorrect split ratio • Purge-off time in splitless mode is too short 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 33 Variations in pressure, column flow, and temperature • Dirty ion source • Loose connections in the analyzer • Ground loops * This could cause a fault condition in the GC that would prevent the GC from operating. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 34: Mass Spectra General Symptoms

    MCP or PMT voltage is too low • Repeller voltage is too high • Wrong ions are chosen • High background • Dirty ion source • Collision cell voltage • Collision cell gas flow 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 35 General Troubleshooting High background • TOF vacuum or Quad vacuum • Air leak • Contamination 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 36: Pressure Symptoms

    Rotary foreline pump oil level is low or oil is contaminated • IDP foreline pump tip seal is worn down and needs replacing • Foreline hose is constricted • Foreline pump is not working correctly 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 37 Turbos are not up to speed • Too much water is in the system • Did not wait long enough for system to pump down • Poor carrier gas quality • System is not leak tight, check fittings 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 38: Temperature Symptoms

    • Mass filter heater cartridge is not connected* • Mass filter temperature sensor is not connected* • Mass filter heater failed (burned out or shorted to ground)* • Mass filter temperature sensor failed* 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 39 GC/MS interface heater failed (burned out)* • GC/MS interface sensor failed* • GC electronics are not working correctly* * This will cause a GC error message. GC error messages are described in the documentation supplied with your GC. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 40: Error Messages

    “The system is in vent state” on page 43 in this section for precautions to take. • The fan is disconnected • The fan has failed • MS electronics are not working correctly 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 41 Internal MS communication fault • MS electronics are not working correctly Lens supply fault • Electrical short in the analyzer • MS cannot maintain the voltage setpoint • MS electronics are not working correctly 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 42 Temperature zone has timed out (heater failed, bad heater wiring, or loose temperature sensor) • Problem with the temperature control electronics • Source heater is open • Source heater is shorted • Mass filter heater is open • Mass filter heater is shorted 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 43 Filament has failed; try the other filament • MS electronics are not working correctly There is not enough signal to begin tune • Corrupted tune file • Poor mass axis calibration • Width gain or offset is too high 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 44 Electrical leads to the detector are not connected correctly • Electrical leads to the ion source are not connected correctly • Filament shorted to the source body • Collision cell gas flow • Collision cell voltages 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 45: Air Leaks

    Side plate O-rings (all the way around) • Calibration valve • GC/MS interface O-ring (where the interface attaches to the analyzer chamber) • End plate O-ring • Turbo pump O-rings • Collision cell cover O-ring 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 46: Contamination

    Fingerprints (improper handling of clean parts) Table 3, “Common contaminants,” on page 47 lists some of the more common contaminants, the ions characteristic of those contaminants, and the likely sources of those contaminants. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 47 73, 147, 207, 221, 281, 295, 355, Dimethylpolysiloxane Septum bleed or methyl silicone column bleed Plasticizer (phthalates) Vacuum seals (O-rings) damaged by high temperatures, vinyl gloves Peaks spaced 14 m/z apart Hydrocarbons Fingerprints, foreline pump oil 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 48 General Troubleshooting 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 49: Ci Troubleshooting

    Pressure-Related Symptoms 55 Signal-Related Symptoms 58 Tuning-Related Symptoms 64 This chapter outlines the troubleshooting of the Agilent 7250 Accurate-Mass Q-TOF GC/MS System equipped with the chemical ionization (CI) source. Most of the troubleshooting information in the previous chapter also applies to CI Q-TOFs.
  • Page 50: Common Ci-Specific Problems

    Air leaks in reagent gas flow path • CI filament has stretched and sagged: • High emission current • High temperature • Filament was defective • Linear (no inflection point) electron energy (EIEnrgy) ramp 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 51: Troubleshooting Tips And Tricks

    • To isolate an air leak, select Shutoff valve. If abundance of m/z 32 decreases, the problem is not in the flow module. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 52: Air Leaks

    Watch for changes that may indicate a vacuum or gas flow problem. There should not be any peak visible at m/z 32 (O ). This almost always indicates an air leak. Figure 5. Looking for air leaks 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 53: Special Nci Notes

    6, “Schematic of CI flow control,” on page 54 and Table 4, “Flow module valve state diagram,” on page 54. • Cool and vent the MS, remove the GC column, and cap off the interface. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 54 Closed Open Closed Open Closed Closed MFCV On (at setpoint) On (at setpoint) On (at 100%) On (at 100%) On (at 100%) Off (at 0%) Shutoff valve Open Open Open Open Open Closed 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 55: Pressure-Related Symptoms

    1.23e+01 1.62e-06 1.67e-07 1.5+02 3.71e-05 3.39e-07 1.31e+01 1.96e-06 1.67e-07 1.57+02 3.73e-05 3.41e-07 1.39e+01 2.32e-06 1.70e-07 1.63+02 3.77e-05 3.41e-07 1.46e+01 2.64e-06 1.71e-07 1.69+02 3.81e-05 3.41e-07 1.52e+01 3.00e-06 1.71e-07 1.74+02 3.83e-05 3.43e-07 1.58e+01 3.34e-06 1.72e-07 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 56: Poor Vacuum Without Reagent Gas Flow

    Run an air and water check. See the software online help for additional information. Interface tip seal is not installed Check the source storage box. If the seal is not in the box, vent the MS and verify that the seal is correctly installed. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 57: Pressure Does Not Change When Reagent Flow Is Changed

    Ensure the methane line is connected to the Gas A inlet. GC/MS interface clogged or damaged Check for flow and repair or replace components as indicated. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 58: Signal-Related Symptoms

    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 page 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 59: No Pfdtd Peaks In Pci

    Go back to methane PCI No sample peaks in NCI • Look for background ions: 35 (Cl ), and 235 (ReO3 • Go back to methane PCI • Poor quality reagent gas (purity less than 99.99%) 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 60: Large Peak At M/Z 238 In Nci Ofn Spectrum

    Fix the air leak. Clean the ion source. Then bake out for two hours before tuning. See the Agilent 7250 Accurate-Mass Quadrupole Time-of-Flight GC/MS System Operating Manual. The wrong reagent gas is flowing.
  • Page 61: No Or Low Pfdtd Signal, But Reagent Ions Are Normal

    The pressure of the methane entering the flow controller is too high. Make sure the regulator on the methane supply is set to 20 to 25 psi (138 to 172 kPa). 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 62: Excessive Noise Or Low Signal-To-Noise Ratio

    CI Troubleshooting The CI ion source is dirty. Clean the ion source. See the Agilent 7250 Accurate-Mass Quadrupole Time-of-Flight GC/MS System Operating Manual. The calibration valve was not purged after the vial was refilled. Purge the calibration valve as described in “To Refill the CI Calibration Vial”...
  • Page 63: Peak At M/Z 32

    A visible peak at m/z 32 in methane pretune often indicates air in the system. New or dirty reagent gas supply tubing Purge the reagent gas supply lines and flow module for at least 60 minutes. See the Agilent 7250 Accurate-Mass Quadrupole Time-of-Flight GC/MS System Operating Manual for more information. Air leak Check for leaks and correct any that you find.
  • Page 64: Tuning-Related Symptoms

    Check the reagent gas path. Tighten fittings. The CI ion source is dirty. Clean the ion source. See the Agilent 7250 Accurate-Mass Quadrupole Time-of-Flight GC/MS System Operating Manual for more information. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 65: Cannot Complete Autotune

    The m/z 28/27 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 Agilent 7250 Accurate-Mass Q-TOF GC/MS System Operating Manual for more information. The CI ion source is dirty.
  • Page 66 CI Troubleshooting 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 67: General Maintenance

    To Move or Store the MS 79 To Access the Left Side Lifting Handle 82 This chapter describes maintenance procedures and requirements that are used with all Agilent 7250 Accurate Mass Q-TOF GC/MS Systems. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 68: Before Starting

    * Or as needed, every 3 months if ammonia is being used as CI reagent gas. † Vacuum seals other than the side plate O-ring and vent valve O-ring do not need to be lubricated. Lubricating other seals can interfere with their correct function. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 69: Tools, Spare Parts, And Supplies

    To reduce the risk of electric shock, follow the procedures carefully. Dangerous temperatures Many parts in the MS operate at, or reach, temperatures high enough to cause serious burns. These parts include, but are not limited to: • GC/MS interface 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 70: Chemical Residue

    The oil in the rotary vane foreline pump also collects traces of the samples being analyzed. All used pump oil should be considered hazardous and handled accordingly. Dispose of used oil as specified by your local regulations. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 71: Electrostatic Discharge

    Take extra precautions, such as a grounded antistatic mat, if you must work on components or assemblies that have been removed from the MS. This includes the analyzer. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 72 Antistatic precautions are not 100% effective. Handle electronic circuit boards as little as possible and then only by the edges. Never touch components, exposed traces, or pins on connectors and cables. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 73: To Refill The Ei Calibration Vial

    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. Calibration vial Collar Figure 7. Removing the EI calibration vial 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 74 12 Turn off the Emission by selecting the check box. 13 Purge the calibration valve by selecting the EI Cal Valve check box to open the calibration valve. Close the EI Cal Valve after 30 seconds. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 75: To Connect The Gc Nitrogen Gas Source To The Collision Cell

    Nitrogen connection Figure 8. Collision cell nitrogen gas connection 2 Place Swagelok nut and ferrule on the end of the nitrogen line tubing from the 3 Connect the nitrogen line to the instrument. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 76: To Separate The Gc From The Ms

    4 Carefully pull the GC away from the MS until you have access to the GC/MS interface cable. (See Figure 9, “Separating/connecting the MS and GC,” on 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 77 If you are moving or storing the MS, see “To Move or Store the MS” on page 79. GC/MS interface Interface cable Figure 9. Separating/connecting the MS and GC 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 78: To Position The Gc Next To The Ms

    4 If needed, connect the column to the transfer line. See the Agilent 7250 Accurate-Mass Q-TOF GC/MS System Operating Manual. 5 Wind the excess column slack in the GC oven around the column basket. 6 Turn on the GC, and start carrier gas flow. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 79: To Move Or Store The Ms

    2 Vent the MS. See the Agilent 7250 Accurate-Mass Q-TOF GC/MS System Operating Manual. 3 Shut off the carrier gas at the source. 4 Shut off the GC, and unplug the power cord. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 80 11 Finger-tighten the side plate thumbscrews for the analyzer. Do not overtighten the side plate thumbscrews. Overtightening will strip the C AU T I O N threads in the analyzer chamber. It will also warp the side plate and cause leaks. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 81 The MS must remain upright at all times. If you need to ship your MS to another C AU T I O N location, contact your Agilent Technologies service representative for advice about packing and shipping. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 82: To Access The Left Side Lifting Handle

    Separate the GC from the MS” on page 76.) Both the GC and MS should be shut down and disconnected from the building power supply. All gas lines must be disconnected from the MS. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 83 2 Swing the grill open, and remove it by disengaging the cover tabs on the right side. 3 To remove the left side cover, disengage the two captive screws at the front edge of the cover. (See Figure 14.) Captive screws Figure 14. Left side cover captive screws 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 84 General Maintenance 4 Slide the left side cover towards the front of the instrument. 5 Remove this cover to access the handle. (See Figure 15.) Lifting handles Figure 15. Left side lifting handles 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 85 To Clean the Reagent Gas Supply Lines 89 To Refill the CI Calibration Vial 90 This chapter describes maintenance procedures and requirements that are unique to an Agilent 7250 Accurate-Mass Q-TOF GC/MS System equipped with the chemical ionization hardware. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 86: Ci Maintenance

    The sound of the pump will get much louder. Ballast valve Figure 16. Minimizing ammonia damage 2 Leave the ballast valve open for one hour. You can continue to run samples while the pump is ballasting. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 87 Always purge the flow module with methane after flowing ammonia. The use C AU T I O N of ammonia reagent gas also requires that the foreline pump oil be replaced every two to three months instead of the usual six months. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 88: To Replace The Chemical Ionization Gas Purifier

    4 Install the new purifier. 5 Turn on the gas flow, and purge the new purifier. 6 Cap the old purifier, and prepare it to be sent for regeneration. See the instructions on the label. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 89: To Clean The Reagent Gas Supply Lines

    6 Repeat for any other pieces of tubing that need to be cleaned. 7 Reconnect the tubing to the gas supply, gas purifier, and MS. Follow the instructions on the gas purifier label. 8 Turn on the reagent gas supply. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 90: To Refill The Ci Calibration Vial

    7 The CI vial is located on the side of the instrument near the transfer line. 8 Turn the CI vial collar counterclockwise to loosen it (Figure 17 on page 91). Do not remove the collar. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 91 78. After removing a calibrant vial, you must purge the calibration valve. Failure to C AU T I O N do so will result in damage to the filaments and the electron multiplier. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 92 16 Turn off the Emission by selecting the check box. 17 Purge the calibration valve by selecting the CI Cal Valve check box to open the calibration valve. Close the CI Cal Valve after 30 seconds. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 93: Vacuum System

    Common Vacuum System Problems 97 Foreline Pump 98 Side Plate 110 Vacuum Seals 110 EI Calibration Valve 111 CI Calibration Valve 112 This chapter describes maintenance requirements of the Agilent 7250 Accurate Mass Q-TOF GC/MS vacuum system. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 94: Overview

    Operation at high pressures also would damage analyzer components. The Agilent 7250 Accurate-Mass GC/MS System uses four vacuum pumps to obtain the vacuum levels needed. Three turbomolecular (turbo) pumps create vacuum in the analyzer.
  • Page 95: Maintaining The Vacuum System

    Agilent 7250 Accurate-Mass Q-TOF GC/MS System Operating Manual. Most of the procedures in this chapter are illustrated with video clips on the Agilent GC/MS Hardware User Information & Instrument Utilities and 7250 Q-TOF GC/MS User Information disks. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 96: Vacuum System Components

    • Collision cell plate • Nitrogen purge and vent system • Side plate (analyzer door) • Vacuum seals • EI calibration valve • Vacuum control electronics • Vacuum gauges and gauge control electronics 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 97: Common Vacuum System Problems

    To restart the MS, find and correct the air leak, then switch the power off and on. Press on the side plates when turning on the MS power to ensure good seals. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 98: Foreline Pump

    Vacuum System Foreline Pump The 7250 can be used with either a standard oil-based rotary vane foreline pump (DS-202), or a dry scroll pump (IDP-15). Procedures for maintaining these pumps are provided on the following pages. Figure 18. Standard rotary vane foreline pump...
  • Page 99: To Disconnect The Foreline Hose From The Foreline Pump

    3 Remove the hose and o-ring from the filter inlet. To check the rotary vane pump oil mist filter Check the oil mist filter weekly for any damage and collected pump fluid. • If the oil mist filter is damaged, replace it. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 100: To Check The Rotary Vane Foreline Pump Fluid Level

    Record this procedure in the Maintenance Logbook, which was supplied with NOTE your instrument. To add oil to the rotary vane foreline pump Add pump oil when the pump oil level is low. Materials needed • Funnel • Gloves, clean, lint-free 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 101: To Replace The Oil In The Rotary Vane Foreline Pump

    Agilent 7250 Accurate-Mass Q-TOF GC/MS System Operating Manual. To replace the oil in the rotary vane foreline pump Replace the pump oil every six months or sooner if the oil appears dark or cloudy. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 102 5 Reinstall the drain plug. 6 Pour in new pump fluid until the fluid level is near, but not above the maximum mark beside the fluid level window. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 103: The Oil Pan Under The Foreline Pump Can Be A Fire Hazard

    1 Unscrew the wing nut on the clamp. (See Figure 19 on page 104.) 2 While supporting the silencer filter, remove the clamp. 3 Lift the filter and O-ring from the pump. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 104: To Install The Exhaust Silencer Filter

    104.) 2 Place the exhaust silencer filter against the O-ring. 3 Place the clamp over the O-ring and KF flanges. 4 Tighten the clamp using the long screw and wing nut. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 105: To Replace The Idp-15 Dry Pump Tip Seal

    IDP-15 tip seal maintenance kit (5190-9613)  Procedure  1 Vent the mass spectrometer (see the Agilent 7250 Accurate-Mass Q-TOF GC/MS System Operating Manual). The IDP pump operates at high temperatures. Do not touch any part until you WAR N IN G are sure it is cool.
  • Page 106 17 Rotate the front cowl over the exhaust port, and align it on the front of the pump. 18 Reattach the front cowl using the six screws and a 4 mm hex wrench. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 107: To Replace The Idp Pump Hepa Filter Cartridge

    4 Secure the lid using the three latches. To change the exhaust silencer filter cartridge Materials needed • Gloves, clean, lint-free • Large (8650-0030) • Small (8650-0029) • Exhaust silencer filter cartridge • large (REPLSLRFILTER1) 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 108: To Install The Idp Pump Ballast

     Procedure  1 Vent the mass spectrometer (see the Agilent 7250 Accurate-Mass Q-TOF GC/MS System Operating Manual). 2 Using a 4 mm hex wrench, unscrew the six screws securing the front cowl. 3 Rotate the cowl over the exhaust port.
  • Page 109: To Remove The Idp Pump Ballast

     Procedure  1 Vent the mass spectrometer (see the Agilent 7250 Accurate-Mass Q-TOF GC/MS System Operating Manual). 2 Using a 4 mm hex wrench, unscrew the six screws securing the front cowl. 3 Rotate the cowl over the exhaust port.
  • Page 110: Side Plate

    Three of the O-rings are lightly lubricated with Apiezon-L vacuum grease: the side plate O-rings and the vent valve O-ring. Contact Agilent to have these vacuum seals serviced. 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 111: Ei Calibration Valve

    A small O-ring provides a face seal. Perfluorotributylamine (PFTBA) is the most commonly used tuning compound for EI operation. PFTBA is required for automatic tuning of the MS. EI calibration vial EI calibration valve Figure 21. EI calibration valve 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 112: Ci Calibration Valve

    CI autotune or manual tuning, allowing the tuning compound, perfluoro-5,8-dimethyl-3,6,9-trioxidodecane (PFDTD), to diffuse through the GC/MS interface and into the ion source. CI Calibration valve CI Calibration vial Figure 22. CI calibration valve 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 113: Replacement Parts

    Additional CI Parts 131 This chapter lists parts that can be ordered for use in maintaining your 7250 Accurate-Mass Q-TOF GC/MS System. It includes most of the parts or assemblies in the MS. Most of the parts listed are not user-replaceable. They are listed here for use by Agilent Technologies service representatives.
  • Page 114: To Order Parts

    (after you receive the rebuilt assembly) you will receive a credit. If you cannot find a part you need If you need a part that is not listed in this chapter, check the Agilent Technologies Analytical Supplies Catalog or the online catalog on the Worldwide Web at http://www.agilent.com/chem.
  • Page 115: Electronics

    Power cord, Europe/S Korea, C19, 15 A, 250 V 8121-1222 Power cord, Thai 220 V, 15 A, 1.8 M, C19 8121-1301 Power cord, Brazil, C19, 250 V max 8121-1787 Power cord, US 240 V, C19, 15 amp 8121-0075 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 116 Cable, Turbo pump control module, AC G3850-60825 Cable, Wire lens - 5 G3850-60833 Cable, Rough pump AC output G3850-60837 Printed circuit boards Table 9 Printed circuit boards Description Part number Filament drive board G7250-67018 Collision cell board G7003-65914 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 117 Fuse (foreline pump) metric 12.5 A 250 V UL-LST CSA 2110-1398 Switch Bd PCA G1960-61000 Power switch button 5041-8381 Switch board cable G3850-60819 Circuit breaker External fuse External fuse Circuit breaker Figure 23. Fuses and circuit breakers 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 118: Vacuum System

    0100-2451 Analyzer ion gauge G1960-80303 Foreline ion gauge G1960-80101 O-ring, standard forepump fill plug 0905-1630 O-ring, ion gauge 0905-1627 O-ring, collision cell feedthrough 0905-1405 O-ring, collision cell plate 0905-1689 Side plate O-ring 0905-1690 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 119 IDP-15 tip seal maintenance kit 5190-9613 IDP-15 tip seal replacement kit X3815-67000 IDP-15 pump X3815-64010 HEPA filter SCRINTRPNW25 Exhaust silencer kit EXSLRSH110 Ballast Contact Agilent for this part Ballast plug Contact Agilent for this part 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 120 G3850-60800 Flex hose, metal, NW 25 G3850-20156 Thermal barrier G1969-20081 Power supply, TMH G3850-60600 CC gas flow module, 3-channel G7002-60044 • GC/MS QQQ flow weldment cap assembly G7000-80500 • 3-Channel QQQ EPC G7000-60506 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 121: Analyzer

    Mass filter contacts (qty 1) G1099-60142 Mass filter ceramic support, source end G7002-20057 Mass filter heater assembly G1099-60172 Pins for source and detector end mounting G1099-20137 brackets p-filter bridge G7000-60028 Side plate, weld assembly (support) G7002-67021 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 122 Ion focus lens (2) G7004-20068 Lens insulator/holder G7002-20074 M2 x 0.4 screw x 12 mm long gold plated screw G7002-20083 Source body G7002-20084 Post extractor lens 2 (3) G7004-20090 Post extractor lens 1 (4) G7004-20004 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 123 Ring heater/sensor assembly G7002-60043 Source mount G7002-60053 Repeller assembly G7002-67057 Complete LE-EI Ion Source, Half Ramp G7250-67170 * The number in parenthesis is the number engraved on the lens Figure 24. LE-EI ion source 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 124 Entrance lens assy, STD, Half-Ramped G7250-20075 HES CI Lens insulator G7250-20095 Locking ring for lens insulator G7002-20126 Screw, M2 × 6 Pan Head Torx, gold plated G7002-20109 Complete assembly Axial CI Ion Source Assy (Support) G7250-67404 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 125 Replacement Parts Figure 25. Axial CI ion source 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 126: Gc/Ms Interface

    G7005-20024 Welded interface assembly G3870-60301 Heater/sensor assembly G1099-60107 M3 set screw 0515-0236 not shown Fitting-face seal, 1/4 in cap sst 316 0100-2013 not shown VCR gasket, size 4, AG on Ni retainer 0100-1436 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 127 Replacement Parts Figure 26. GC/MS interface for the 8890 and 7890 GCs 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 128: Consumables And Maintenance Supplies

    Tool kit G7077-60566 Ball drivers, 1.5-mm 8710-1570 Ball drivers, 2.0-mm 8710-1804 Ball drivers, 2.5-mm 8710-1681 Hex nut driver, 5.5-mm 8710-1220 Pliers, long-nose (1.5-inch nose) 8710-0004 Screwdrivers Flat-blade, large 8730-0002 Screwdrivers Torx, T-10 8710-1623 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 129 0.37-mm id, 90%/10%, for 0.20-mm id columns 5062-3516 • 0.40-mm id, 90%/10%, for 0.25-mm id columns 5181-3323 • 0.47-mm id, 90%/10%, for 0.32-mm id columns 5062-3514 • 0.74-mm id, 90%/10%, for 0.53-mm id columns 5062-3512 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 130 Swagelok ferrule, front, 1/8-inch, 10/package 5180-4110 Swagelok ferrule, rear, 1/8-inch, 10/package 5180-4116 Swagelok nut, for 1/8-inch fitting, 10/package 5180-4104 Swagelok nut and ferrules, 10 set/package 5080-8751 Tubing cutter for SS tubing 8710-1709 Tubing cutter replacement blades 8710-1710 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 131: Additional Ci Parts

    Replacement Parts Additional CI Parts This section shows parts that may be required to maintain the 7250 Q-TOF GC/MS System with CI. (See Table 25.) The parts in this section are related directly to the CI accessory and are in addition to the Axial CI ion source parts...
  • Page 132 Replacement Parts 7250 Accurate-Mass Q-TOF Troubleshooting and Maintenance Manual...
  • Page 134  Agilent Technologies, Inc. 2019 First Edition, January 2019 *G7250-90007* G7250-90007...

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