Agilent 5977B Series MSD Troubleshooting and Maintenance Manual Notices © Agilent Technologies, Inc. 2019 No part of this manual may be reproduced in any form or by any means (including electronic storage and retrieval or translation into a foreign language) without prior agreement and written consent from Agilent Technologies, Inc. as governed by United States and international copyright laws. Manual Part Number G7077-90035 Edition First edition, January 2019 Printed in USA Agilent Technologies, Inc. 5301 Stevens Creek Boulevard Santa Clara, CA 95051 Warranty The material contained in this document is provided “as is,” and is subject to being changed, without notice, in future editions. Further, to the maximum extent permitted by applicable law, Agilent disclaims all warranties, either express or implied, with regard to this manual and any information contained herein, including but not limited to the implied warranties of merchantability and fitness for a particular purpose. Agilent shall not be liable for errors or for incidental or consequential damages in connection with the furnishing, use, or performance of this document or of any information contained herein. Should Agilent and the user have a separate written agreement with warranty terms covering the material in this document that conflict with these terms, the warranty terms in the separate agreement shall control. Safety Notices CAUTION A CAUTION notice denotes a hazard. It calls attention to an operating procedure, practice, or the like that, if not correctly performed or adhered to, could result in damage to the product or loss of important data. Do not proceed beyond a CAUTION notice until the indicated conditions are fully understood and met. WARNING A WARNING notice denotes a hazard. It calls attention to an operating procedure, practice, or the like that, if not correctly performed or adhered to, could result in personal injury or death. Do not proceed beyond a WARNING notice until the indicated conditions are fully understood and met. 5977B Series MSD Troubleshooting and Maintenance Manual 3 Contents 1 Introduction 5977B Series MSD Version 10 Abbreviations Used 11 The 5977B Series MSD 13 MSD Hardware Description 16 Electron ionization (EI) systems 17 Chemical ionization (CI) systems 17 Changing modes 18 Important Safety Warnings 19 Electrostatic discharge is a threat to MSD electronics 20 Hydrogen Safety 22 Precautions 25 Safety and Regulatory Certifications 27 Intended Use 31 Cleaning/Recycling the Product 31 Accidental Liquid Spillage 31 Moving or Storing the MSD 31 2 General Troubleshooting Instrument State 34 Troubleshooting Tips and Tricks 35 General Symptoms 36 Chromatographic Symptoms 38 Mass Spectral Symptoms 43 Pressure Symptoms 47 Temperature Symptoms 50 4 5977B Series MSD Troubleshooting and Maintenance Manual Error Messages 52 Air Leaks 58 Contamination 59 3 CI Troubleshooting Common CI-Specific Problems 62 Troubleshooting Tips and Tricks 63 Air Leaks 64 Pressure-Related Symptoms 68 Signal-Related Symptoms 71 Tuning-Related Symptoms 78 4 General Maintenance Before Starting 83 Maintaining the Vacuum System 88 To Separate the MSD from an 8890 or 7890 GC 89 To Separate the MSD from the 9000 GC 91 To Reconnect the MSD to an 8890 or 7890 GC 93 To Reconnect the MSD to the 9000 GC 94 To Move or Store the MSD when Connected to an 8890 or 7890 GC 96 To Move or Store the MSD when Connected to a 9000 GC 98 To Check the Foreline Pump Oil 100 To Drain the Foreline Pump 102 To Refill the Foreline Pump 103 To Change the Oil Mist Filter on the Foreline Pump 104 To Install the Exhaust Filter on the IDP3 Dry Pump 106 5977B Series MSD Troubleshooting and Maintenance Manual 5 To Change the Filter Cartridge on the IDP3 Dry Foreline Pump 108 To Check the DP Fluid 109 To Remove the DP 111 To Replace the DP Fluid 113 To Install the DP 115 To Remove the Foreline Gauge 117 To Install the Foreline Gauge 119 To Refill the EI Calibration Vial 120 To Purge the Calibration Valves 122 To Remove the EI Calibration and Vent Valve Assembly 123 To Install the EI Calibration and Vent Valve Assembly 124 To Replace the Fan for the High Vacuum Pump 125 To Remove the Ion Vacuum Gauge 127 To Install an Ion Vacuum Gauge 127 To Lubricate the Side Plate O-Ring 128 To Lubricate the Vent Valve O-Ring 130 Maintaining the Electronics 132 To Adjust the Quad Frequency 134 To Replace the Primary Fuses 136 5 CI Maintenance To Replace the Methane/Isobutane Gas Purifier 140 To Clean the Reagent Gas Supply Lines 141 To Refill the CI Calibration Vial 142 6 5977B Series MSD Troubleshooting and Maintenance Manual 6 Vacuum System Overview 146 Vacuum System Components 147 Common Vacuum System Problems 148 Foreline Pump 149 High Vacuum Pump 152 Diffusion pump system 152 Turbo pump system 152 Analyzer Chamber 153 Diffusion pump version 153 Turbo pump version 153 Side Plate 154 Vacuum Seals 157 Foreline Gauge 159 Diffusion Pump and Fan 160 Turbo Pump and Fan 166 Calibration Valves and Vent Valve 167 Micro-Ion Vacuum Gauge 170 7 Analyzer Overview 172 EI Ion Source 175 HES EI Ion Source 182 CI Ion Source 185 Filaments 188 Other Source Elements 190 Quadrupole Mass Filter 192 Detector 195 5977B Series MSD Troubleshooting and Maintenance Manual 7 Analyzer Heaters and Radiators 197 8 Electronics GC Control Panel, Power Switch, and Front Panel LED 202 Side Board 204 Electronics Module 205 LAN/MS Control Card 209 Power Supplies 210 Back Panel and Connectors 211 Interfacing to External Devices 214 9 Parts To Order Parts 218 Electronics 219 Vacuum System 219 Analyzer 226 Consumables and Maintenance Supplies 236 8 5977B Series MSD Troubleshooting and Maintenance Manual 5977B Series MSD Troubleshooting and Maintenance Manual 9 1 Introduction 5977B Series MSD Version 10 Abbreviations Used 11 The 5977B Series MSD 13 Physical description 15 Front Panel LED 15 Vacuum gauge 15 MSD Hardware Description 16 Important Safety Warnings 19 Many internal parts of the MSD carry dangerous voltages 19 Electrostatic discharge is a threat to MSD electronics 20 Many parts are dangerously hot 20 The oil pan under the standard foreline pump can be a fire hazard 21 Hydrogen Safety 22 Dangers unique to GC/MSD operation 22 Hydrogen accumulation in an MSD 23 Precautions 25 Safety and Regulatory Certifications 27 Information 28 Symbols 28 Sound emission declaration 30 The best way to keep your MSD functioning properly is to keep it pumped down and hot, with carrier gas flow. If you plan to move or store your MSD, a few additional precautions are required. The MSD must remain upright at all times; this requires special caution when moving. The MSD should not be left vented to the atmosphere for long periods. 31 This manual describes the troubleshooting and maintenance of the Agilent Technologies 5977B Series Mass Selective Detector (MSD). It assumes familiarity with the procedures and information detailed in the 5977B Series MSD or 5975/77 Series for OpenLAB CDS Operation Manual, and with the accompanying software. 1 Introduction 5977B Series MSD Version 10 5977B Series MSD Troubleshooting and Maintenance Manual 5977B Series MSD Version The 5977B Series MSDs are equipped with a turbomolecular (turbo) pump and a choice of three foreline pumps (Pfeiffer Duo, Pfeiffer MVP-070-3x, Agilent IDP-3 24V) or a diffusion (diff) pump paired with a Pfeiffer Duo foreline pump. There are three types of electron ionization (EI) sources available on the 5977B Series MSD, a standard EI stainless steel (SS) source, an EI Extractor (XTR) source available on the Inert+ MSD model, and a high efficiency source (HES). A CI ion source includes a reagent flow control system, a CI calibration system, and other required hardware features. The serial number label displays a product number (Table 1) that indicates what type of MSD you have. Table 1 Available high vacuum pumps Model name Product number Description Ionization mode/Type 5977B MSD Diff Pump G7080B Diffusion pump Electron ionization (EI)/Stainless Steel 5977B MSD Turbo Pump G7081B Turbo pump Electron ionization (EI)/Stainless Steel 5977B Inert+ EI MSD Turbo G7077B Turbo pump MSD Electron ionization (EI)/Extractor 5977B Inert+ EI/CI MSD Turbo G7078B Turbo pump MSD Electron ionization (EI) /Extractor Chemical ionization /PCI, NCI 5977B HES MSD G7079B Turbo pump MSD Electron ionization (EI)/High Efficiency 1 Introduction Abbreviations Used 5977B Series MSD Troubleshooting and Maintenance Manual 11 Abbreviations Used The abbreviations in Table 2 are used in discussing this product. They are collected here for convenience. Table 2 Abbreviations Abbreviation Definition AC Alternating current ALS Automatic liquid sampler BFB Bromofluorobenzene (calibrant) CI Chemical ionization DA Data analysis DC Direct current DFTPP Decafluorotriphenylphosphine (calibrant) Diff Diffusion (pump) DIP Direct insertion probe DP Diffusion pump DS Data system EI Electron impact ionization EM Electron multiplier (detector) EMV Electron multiplier voltage EPC Electronic pneumatic control eV Electron volt FW Firmware GC Gas chromatograph HED High-energy dynode (refers to detector and its power supply) HES High efficiency source id Inside diameter Inert+ Extractor source LAN Local Area Network 1 Introduction Abbreviations Used 12 5977B Series MSD Troubleshooting and Maintenance Manual LCP Local control panel (on the GC) LVDS Low voltage data signal m/z Mass-to-charge ratio MFC Mass flow controller MSD Mass selective detector NCI Negative CI OFN Octafluoronaphthalene (calibrant) PCI Positive CI PFDTD Perfluoro-5,8-dimethyl-3,6,9-trioxydodecane (calibrant) PFHT 2,4,6-tris(perfluoroheptyl)-1,3,5-triazine (calibrant) PFTBA Perfluorotributylamine (calibrant) Quad Quadrupole mass filter RF Radio frequency RFPA Radio frequency power amplifier SS Stainless steel Torr Unit of pressure, 1 mm Hg Turbo Turbomolecular (pump) WUI Web user interface XTR EI Extractor source Table 2 Abbreviations (continued) Abbreviation Definition 1 Introduction The 5977B Series MSD 5977B Series MSD Troubleshooting and Maintenance Manual 13 The 5977B Series MSD The 5977B Series MSD is a stand-alone capillary GC detector. The MSD features (See Table 3 on page 14.): • GC compatibility includes Agilent 8890, 9000, and 7890 GCs • WEB User Interface (WUI) for locally monitoring and operating the MSD • A turbo vacuum pump with one of three different foreline pumps (Pfeiffer Duo, Pfeiffer MVP-070-3x, Agilent IDP-3 24V) or a diffusion vacuum pump with a Pfeiffer Duo foreline pump • A high efficiency ion source (HES) • Three different non-HES types of independently heated MSD electron ionization (EI) sources available: standard source in both stainless steel and inert material, and an extractor source. • Field upgradeable to chemical ionization (PCI/NCI) modes that add a chemical ionization (CI) source, reagent gas flow controller and plumbing, and CI tuning calibration • An optional JetClean system for cleaning the ion source in place under vacuum • Independently MSD-heated hyperbolic quadrupole mass filter • High-energy dynode (HED) electron multiplier detector • Independently GC-heated GC/MSD interface • Direct insertion probe (DIP) capability (3rd party) 1 Introduction The 5977B Series MSD 14 5977B Series MSD Troubleshooting and Maintenance Manual Vacuum capability Table 3 5977B HES Series MSD features Feature High vacuum pump Diffusion Turbo Optimal He column flow mL/min 1 1 to 2 Maximum recommended gas flow mL/min* * Total gas flow into the MSD: column flow plus reagent gas flow (if applicable). Based on helium gas use. For other gases the maximum flow will vary. 1.5 4 Maximum gas flow, mL/min† † Expect degradation of spectral performance and sensitivity. 2 6.5 Max column id 0.25 mm (30 m) 0.53 mm (30 m) CI capability‡ ‡ Turbo pump models are field upgradeable to CI. No Yes Inert ion sources available Yes Yes GC compatibility 9000/8890/ 8860/7890 Series 9000/8890/ 8860/7890 Series Foreline pumps available Pfeiffer Duo Pfeiffer Duo, Pfeiffer MVP-070-3x, Agilent IDP-3 24V DIP** capability (3rd party) ** Direct insertion probe. Yes Yes 1 Introduction The 5977B Series MSD 5977B Series MSD Troubleshooting and Maintenance Manual 15 Physical description The 5977B HES Series MSD housing is approximately 41 cm high, 30 cm wide, and 54 cm deep. The weight is 39 kg for the diffusion pump models, and 46 kg for the EI/CI turbo pump mainframe. The weight is 41 kg for the EI turbo pump mainframe. The standard foreline (roughing) pump weighs an additional 11 kg (standard pump), and the dry foreline pump weighs 16 kg. The foreline pump is usually located on the floor behind the MSD. The basic components of the instrument are the: • Frame/cover assemblies • Vacuum system • GC/MSD interface • Electronics • Analyzer Front Panel LED The front panel LED allows the operator to monitor the MSD. The LED displays the instrument status with color codes and patterns described in “GC Control Panel, Power Switch, and Front Panel LED” on page 202. Vacuum gauge The MSD may be equipped with an ion vacuum gauge. The Data Acquisition software can be used to read the pressure (high vacuum) in the vacuum manifold. The gauge is required for chemical ionization (CI) operation. 1 Introduction MSD Hardware Description 16 5977B Series MSD Troubleshooting and Maintenance Manual MSD Hardware Description Figure 1 is an overview of a typical GC/MSD system. Figure 1. Agilent 5977B Series GC/MSD system shown with 8890 GC ALS Touchscreen 8890 GC 5977B Series MSD MSD power switch GC power switch System status LED 1 Introduction Electron ionization (EI) systems 5977B Series MSD Troubleshooting and Maintenance Manual 17 Electron ionization (EI) systems EI systems ionize sample molecules by bombarding them with electrons. The ions, including fragments, are drawn into the quadrupole analyzer where they are separated by their mass-to-charge (m/z) ratios and detected. There are three types of electron ionization sources available: the standard EI ion source, which is available in stainless steel or inert material, the extractor EI ion source (XTR) and the high efficiency ion source (HES). Chemical ionization (CI) systems CI systems use a reagent gas as an intermediate between the electrons and the sample. CI is more gentle than direct electron bombardment. The CI hardware allows the 5977B Series MSD to produce high-quality, classical CI spectra, which include molecular adduct ions. A variety of reagent gases can be used. In this manual, the term CI MSD refers to the upgraded G7077B, the upgraded G7078B, or the upgraded G7079B MSD. It also applies, unless otherwise specified, to the flow modules for these instruments. The 5977B Series GC/MSD CI system adds the following to the 5977B Series MSD: • An EI/CI GC/MSD interface • A reagent gas flow control module • A bipolar HED power supply for PCI and NCI operation A required methane/isobutane gas purifier is provided. It removes oxygen, water, hydrocarbons, and sulfur compounds. A high vacuum gauge controller (G3397B) required for CI MSD is also recommended for EI. The MSD CI system has been optimized to achieve the relatively high source pressure required for CI, while still maintaining a high vacuum in the quadrupole and detector. Special seals along the flow path of the reagent gas and very small openings in the ion source keep the source gases in the ionization volume long enough for the appropriate reactions to occur. The CI interface has special plumbing for reagent gas. 1 Introduction Changing modes 18 5977B Series MSD Troubleshooting and Maintenance Manual Changing modes Switching back and forth between CI and EI ion sources takes less than an hour, although a 1- to 2-hour wait is required to purge the reagent gas lines and bake out water and other contaminants. Switching from PCI to NCI requires about 2 hours for the ion source to cool. 1 Introduction Important Safety Warnings 5977B Series MSD Troubleshooting and Maintenance Manual 19 Important Safety Warnings There are several important safety notices to keep in mind when using the MSD. Many internal parts of the MSD carry dangerous voltages If the MSD is connected to a power source, even if the power switch is off, potentially dangerous voltages exist on: • The wiring between the MSD power cord and the AC power supply, the AC power supply itself, and the wiring from the AC power supply to the power switch. With the power switch on, potentially dangerous voltages also exist on: • All electronics boards in the instrument • The internal wires and cables connected to these boards • The wires for any heater (oven, detector, inlet, or valve box) If one of the primary fuses has failed, the MSD will already be off, but for safety, switch off the MSD and unplug the power cord. It is not necessary to allow air into the analyzer chamber. WARNING All these parts are shielded by covers. With the covers in place, it should be difficult to accidentally make contact with dangerous voltages. Unless specifically instructed to, never remove a cover unless the detector, inlet, or oven are turned off. WARNING If the power cord insulation is frayed or worn, the cord must be replaced. Contact your Agilent service representative. WARNING Never replace the primary fuses while the MSD is connected to a power source. 1 Introduction Electrostatic discharge is a threat to MSD electronics 20 5977B Series MSD Troubleshooting and Maintenance Manual Electrostatic discharge is a threat to MSD electronics The printed circuit boards in the MSD 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. Wear a grounded wrist strap any time you remove the MSD right side cover. Many parts are dangerously hot Many parts of the GC/MSD operate at temperatures high enough to cause serious burns. These parts include, but are not limited to the: • GC inlets • GC oven and its contents, including the column nuts attaching the column to a GC inlet, GC/MSD interface, or GC detector • GC detector • GC valve box • Foreline pump • Diffusion pump • Heated MSD ion source GC/MSD, interface, and quadrupole Always cool these areas of the system to room temperature before working on them. They will cool faster if you first set the temperature of the heated zone to room temperature. 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. WARNING Be careful when working behind the instrument. During cooldown cycles, the GC emits hot exhaust which can cause burns. WARNING The insulation around the inlets, detectors, valve box, and the insulation cups is made of refractory ceramic fibers. To avoid inhaling fiber particles, we recommend the following safety procedures: ventilate your work area; wear long sleeves, gloves, safety glasses, and a disposable dust/mist respirator; dispose of insulation in a sealed plastic bag; wash your hands with mild soap and cold water after handling the insulation. 1 Introduction Electrostatic discharge is a threat to MSD electronics 5977B Series MSD Troubleshooting and Maintenance Manual 21 The oil pan under the 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 MSD. WARNING Combustible materials (or flammable/nonflammable wicking material) placed 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. 1 Introduction Hydrogen Safety 22 5977B Series MSD Troubleshooting and Maintenance Manual Hydrogen Safety Hydrogen is a commonly used GC carrier gas, detector fuel gas, and reactive cleaning gas for the optional JetClean system. Hydrogen is potentially explosive and has other dangerous characteristics. • Hydrogen is combustible over a wide range of concentrations. At atmospheric pressure, hydrogen is combustible at concentrations from 4% to 74.2% by volume. • Hydrogen has the highest burning velocity of any gas. • Hydrogen has a very low ignition energy. • Hydrogen that is allowed to expand rapidly from high pressure can self-ignite. • Hydrogen burns with a nonluminous flame which can be invisible under bright light. Additional information can be found in the Hydrogen Safety Guide which is included on this Agilent 5977B HES Series MSD User Information media. Dangers unique to GC/MSD operation Hydrogen presents a number of dangers. Some are general, others are unique to GC or GC/MSD operation. Dangers include, but are not limited to: • Combustion of leaking hydrogen WARNING The use of hydrogen as a GC carrier gas, detector fuel gas, or in the optional JetClean system, is potentially dangerous. WARNING When using hydrogen (H2) as the carrier gas or fuel gas, be aware that hydrogen can flow into the GC oven and create an explosion hazard. Therefore, ensure that the supply is turned off until all connections are made, and that the inlet and detector column fittings are either connected to a column or capped at all times when hydrogen is supplied to the instrument. Hydrogen is flammable. Leaks, when confined in an enclosed space, may create a fire or explosion hazard. In any application using hydrogen, leak test all connections, lines, and valves before operating the instrument. Always turn off the hydrogen supply at its source before working on the instrument. 1 Introduction Hydrogen Safety 5977B Series MSD Troubleshooting and Maintenance Manual 23 • Combustion due to rapid expansion of hydrogen from a high-pressure cylinder • Accumulation of hydrogen in the GC oven and subsequent combustion (see your GC documentation and the label on the top edge of the GC oven door) • Accumulation of hydrogen in the MSD and subsequent combustion Hydrogen accumulation in an MSD All users should be aware of the mechanisms by which hydrogen can accumulate (Table 4) and know what precautions to take if they know or suspect that hydrogen has accumulated. Note that these mechanisms apply to all mass spectrometers, including the MSD. WARNING The MSD cannot detect leaks in inlet or detector gas streams. For this reason, it is vital that column fittings should always be either connected to a column, or have a cap or plug installed. WARNING The MS cannot detect leaks in the valves for the optional JetClean system. It is possible that hydrogen can leak into the MS from this cleaning system. Always turn off the JetClean system, close the manual hydrogen shutoff valve to the JetClean MFC, and ensure good vacuum before venting the MS. Table 4 Hydrogen accumulation mechanisms Mechanism Results Mass spectrometer turned off A mass spectrometer can be shut down deliberately. It can also be shut down accidentally by an internal or external failure. There is a safety feature that will shutdown the flow of carrier gas in the event of an MSD foreline pump shutdown. However, if this feature fails, hydrogen may slowly accumulate in the mass spectrometer. Mass Spectrometer automated shutoff valves closed The mass spectrometers are equipped with automated shutoff valves for the calibration vial, optional JetClean system, and the reagent gases. Deliberate operator action or various failures can cause the shutoff valves to close. Shutoff valve closure does not shut off the flow of carrier gas. As a result, hydrogen may slowly accumulate in the MS. 1 Introduction Hydrogen Safety 24 5977B Series MSD Troubleshooting and Maintenance Manual Mass spectrometer automated shutoff valves closed Some mass spectrometers are equipped with automated diffusion pump shutoff valves. In these instruments, deliberate operator action or various failures can cause the shutoff valves to close. Closing the shutoff valves does not shut off the flow of carrier gas. As a result, hydrogen may slowly accumulate in the mass spectrometer. Mass spectrometer manual shutoff valves closed Some mass spectrometers are equipped with manual diffusion pump shutoff valves. In these instruments, the operator can close the shutoff valves. Closing the shutoff valves does not shut off the flow of carrier gas. As a result, hydrogen may slowly accumulate in the mass spectrometer. GC off A GC can be shut down deliberately. It can also be shut down accidentally by an internal or external failure. Different GCs react in different ways. If an 8890 or 7890 GC equipped with Electronic Pressure Control (EPC) is shut off, the EPC stops the flow of carrier gas. If the carrier flow is not under EPC control, the flow increases to its maximum. This flow may be more than some mass spectrometers can pump away, resulting in the accumulation of hydrogen in the mass spectrometer. If the mass spectrometer is shut off at the same time, the accumulation can be fairly rapid. Power failure If the power fails, both the GC and mass spectrometer shut down. The carrier gas, however, is not necessarily shut down. As described previously, in some GCs a power failure may cause the carrier gas flow to be set to maximum. As a result, hydrogen may accumulate in the mass spectrometer. Table 4 Hydrogen accumulation mechanisms (continued) Mechanism Results WARNING Once hydrogen has accumulated in a mass spectrometer, extreme caution must be used when removing it. Incorrect startup of a mass spectrometer filled with hydrogen can cause an explosion. WARNING After a power failure, the mass spectrometer may start up and begin the pumpdown process by itself. This does not guarantee that all hydrogen has been removed from the system, or that the explosion hazard has been removed. 1 Introduction Precautions 5977B Series MSD Troubleshooting and Maintenance Manual 25 Precautions Take the following precautions when operating a GC/MSD system or GC/MS system with hydrogen carrier gas or when operating the MSD with the JetClean option that supplies hydrogen to the MSD from an MFC located on the MS. General laboratory precautions • Avoid leaks in the carrier gas lines. Use leak-checking equipment to periodically check for hydrogen leaks. • Eliminate from your laboratory as many ignition sources as possible (open flames, devices that can spark, sources of static electricity, etc.). • Do not allow hydrogen from a high pressure cylinder to vent directly to atmosphere (danger of self-ignition). • Use a hydrogen generator instead of bottled hydrogen. Operating precautions • Turn off the hydrogen at its source every time you shut down the GC or MSD. • Turn off the hydrogen at its source every time you vent the MSD (do not heat the capillary column without carrier gas flow). • Turn off the hydrogen at its source every time shutoff valves in an MSD are closed (do not heat the capillary column without carrier gas flow). • Turn off the hydrogen at its source if a power failure occurs. • If a power failure occurs while the GC/MSD system is unattended, even if the system has restarted by itself: 1 Immediately turn off the hydrogen at its source. 2 Turn off the GC. 3 Turn off the MSD, and allow it to cool for 1 hour. WARNING You MUST ensure the front side-plate thumbscrew is fastened finger-tight. Do not overtighten the thumbscrew; it can cause air leaks. WARNING You must remove the analyzer window cover on the front of a 5977B Series MSD. In the unlikely event of an explosion, this cover may dislodge. WARNING Failure to secure your MSD as described above greatly increases the chance of personal injury in the event of an explosion. 1 Introduction Precautions 26 5977B Series MSD Troubleshooting and Maintenance Manual 4 Eliminate all potential sources of ignition in the room. 5 Open the vacuum manifold of the MSD to atmosphere. 6 Wait at least 10 minutes to allow any hydrogen to dissipate. 7 Start up the GC and MSD as normal. When using hydrogen, check the system for leaks to prevent possible fire and explosion hazards based on local Environmental Health and Safety (EHS) requirements. Always check for leaks after changing a tank or servicing the gas lines. Always make sure the vent line is vented into a fume hood. 1 Introduction Safety and Regulatory Certifications 5977B Series MSD Troubleshooting and Maintenance Manual 27 Safety and Regulatory Certifications The 5977B HES Series MSD conforms to the following safety standards: • Canadian Standards Association (CSA): CAN/CSA-C222 No. 61010-1-04 • CSA/Nationally Recognized Test Laboratory (NRTL): UL 61010–1 • International Electrotechnical Commission (IEC): 61010–1 • EuroNorm (EN): 61010–1 The 5977B HES Series MSD conforms to the following regulations on Electromagnetic Compatibility (EMC) and Radio Frequency Interference (RFI): • CISPR 11/EN 55011: Group 1, Class A • IEC/EN 61326 • AUS/NZ This ISM device complies with Canadian ICES-001. Cet appareil ISM est conforme a la norme NMB—001 du Canada. EMC declaration for South Korea This equipment has been evaluated for its suitability for use in a commercial environment. When used in a domestic environment, there is a risk of radio interference. 사용자안내문 이 기기는 업무용 환경에서 사용할 목적으로 적합성평가를 받은 기기로서 가정용 환 경에서 사용하는 경우 전파간섭의 우려가 있습니다 . ※ 사용자 안내문은 ” 업무용 방송통신기자재 ” 에만 적용한다 . The 5977B Series MSD is designed and manufactured under a quality system registered to ISO 9001. The 5977B HES Series MSD is RoHS compliant. 1 Introduction Safety and Regulatory Certifications 28 5977B Series MSD Troubleshooting and Maintenance Manual Information The 5977B Series MSD meets the following IEC (International Electro-technical Commission) classifications: Equipment Class I, Laboratory Equipment, Installation Category II, Pollution Degree 2. This unit has been designed and tested in accordance with recognized safety standards, and is designed for use indoors. If the instrument is used in a manner not specified by the manufacturer, the protection provided by the instrument may be impaired. Whenever the safety protection of the MSD has been compromised, disconnect the unit from all power sources, and secure the unit against unintended operation. Refer servicing to qualified service personnel. Substituting parts or performing any unauthorized modification to the instrument may result in a safety hazard. Symbols Warnings in the manual or on the instrument must be observed during all phases of operation, service, and repair of this instrument. 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. See accompanying instructions for more information. Indicates a hot surface. Indicates hazardous voltages. Indicates earth (ground) terminal. Indicates potential explosion hazard. Indicates radioactivity hazard. or 1 Introduction Safety and Regulatory Certifications 5977B Series MSD Troubleshooting and Maintenance Manual 29 Indicates electrostatic discharge hazard. Indicates that you must not discard this electrical/electronic product in domestic household waste. 1 Introduction Safety and Regulatory Certifications 30 5977B Series MSD Troubleshooting and Maintenance Manual Electromagnetic compatibility This device complies with the requirements of CISPR 11. Operation is subject to the following two conditions: • This device may not cause harmful interference. • This device must accept any interference received, including interference that may cause undesired operation. If this equipment does cause harmful interference to radio or television reception, which can be determined by turning the equipment off and on, the user is encouraged to try one or more of the following measures: • Relocate the radio or antenna. • Move the device away from the radio or television. • Plug the device into a different electrical outlet, so that the device and the radio or television are on separate electrical circuits. • Make sure that all peripheral devices are also certified. • Make sure that appropriate cables are used to connect the device to peripheral equipment. • 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. Schalldruckpegel Schalldruckpegel Lp <70 dB am nach EN 27779:1991. 1 Introduction Intended Use 5977B Series MSD Troubleshooting and Maintenance Manual 31 Intended Use Agilent products must be used only in the manner described in the Agilent product user guides. Any other use may result in damage to the product or personal injury. Agilent is not responsible for any damages caused, in whole or in part, by improper use of the products, unauthorized alterations, adjustments, or modifications to the products, failure to comply with procedures in Agilent product user guides, or use of the products 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 Agilent sales office. Accidental Liquid Spillage Do not spill liquids on the MSD. If liquid is accidentally spilled on the MSD, first, cut the power. Once the MSD is disconnected from all power sources, dry all affected parts. If the liquid spillage affects the electronics, wait at least 24 hours, depending upon the ambient humidity. While waiting for the parts to dry, please call your local Agilent service representative. Moving or Storing the MSD The best way to keep your MSD functioning properly is to keep it pumped down and hot, with carrier gas flow. If you plan to move or store your MSD, a few additional precautions are required. The MSD must remain upright at all times; this requires special caution when moving. The MSD should not be left vented to the atmosphere for long periods. 1 Introduction Moving or Storing the MSD 32 5977B Series MSD Troubleshooting and Maintenance Manual 5977B Series MSD Troubleshooting and Maintenance Manual 33 2 General Troubleshooting Instrument State 34 Troubleshooting Tips and Tricks 35 General Symptoms 36 Chromatographic Symptoms 38 Mass Spectral Symptoms 43 Pressure Symptoms 47 Temperature Symptoms 50 Error Messages 52 Air Leaks 58 Contamination 59 This chapter discusses how to identify the symptoms and causes of the most common problems experienced by users with your MSD. See “CI Troubleshooting” on page 61 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 chapter does not include corrective actions for the possible causes listed. Some of the corrective actions required may be dangerous if performed incorrectly. Do not attempt any corrective actions unless you are sure of the correct procedure and the dangers involved. See the Troubleshooting section in the online help and the other chapters in this manual for more information If the material in this chapter and in the online help does not to help you diagnose your problem, contact your Agilent Technologies service representative. 2 General Troubleshooting Instrument State 34 5977B Series MSD Troubleshooting and Maintenance Manual Instrument State Through the front panel LED, the operator can see the current status of the instrument through color codes. See Table 5 for a description of the MSD state. Table 5 Front panel Instrument Status LED codes Instrument status LED code Ready Solid green Acquiring data Blinking green (<2 sec) Not ready Solid yellow JetClean Acquire & Clean operation Blinking magenta JetClean Clean Only operation Solid magenta Not connected to DS Blinking yellow (<2 sec) Ready and not connected to DS Solid yellow for 3 sec, quick double blink Start up (prior to FW load) Blinking red (<2 sec) Fault Solid red 2 General Troubleshooting Troubleshooting Tips and Tricks 5977B Series MSD Troubleshooting and Maintenance Manual 35 Troubleshooting Tips and Tricks Rule 1: Look for what has been changed. Many problems are introduced accidentally by human actions. Every time any system is disturbed, there is a chance of introducing a new problem. • If the MSD was just pumped down after maintenance, suspect air leaks or incorrect assembly. • If carrier gas or helium gas purifier were just changed, suspect leaks or contaminated or incorrect gas. • If the GC column was just replaced, suspect air leaks or contaminated or bleeding column. Rule 2: If complex is not working, go back to simple. A complex task is not only more difficult to perform but also more difficult to troubleshoot. If you are having trouble detecting your sample, verify that autotune is successful. Rule 3: Divide and conquer. This technique is known as half-split troubleshooting. If you can isolate the problem to only part of the system, it is much easier to locate. • To determine whether an air leak is in the GC or the MSD, you can vent the MSD, remove the column, and install the blank interface ferrule. If the leak goes away, it was in the GC. 2 General Troubleshooting General Symptoms 36 5977B Series MSD Troubleshooting and Maintenance Manual General Symptoms This section describes symptoms you might observe when first turning on the GC/MSD system, and their possible causes. Any of these symptoms would prevent operation of the system. GC does not turn on Nothing happens when the GC is switched on. The GC fans do not turn on, and the GC control panel or touchscreen does not light. • Disconnected GC power cord • No voltage or incorrect voltage at the electrical outlet • Failed fuse in the GC • GC power supply is not working correctly MSD does not turn on 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. • Disconnected MSD power cord • No voltage or incorrect voltage at the electrical outlet • Failed primary fuses • MSD electronics are not working correctly Foreline pump is not operating The MSD is receiving power (the fan is operating), but the foreline pump is not operating. • Large air leak (usually the analyzer door open) has caused pumpdown failure. See “Pumpdown failure shutdown” on page 148. You must power cycle the MSD to recover from this state. • Disconnected foreline pump power cord • Malfunctioning foreline pump • Check power switch on foreline pump 2 General Troubleshooting General Symptoms 5977B Series MSD Troubleshooting and Maintenance Manual 37 MSD turns on, but then the foreline pump shuts off MSDs will shut down both the foreline pump and the high vacuum pump if the system fails to pump down correctly. This is usually because of a large air leak: either the sideplate has 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 shutdown” on page 148. You must power cycle the MSD to recover from this state. 2 General Troubleshooting Chromatographic Symptoms 38 5977B Series MSD Troubleshooting and Maintenance Manual Chromatographic Symptoms These are symptoms you may observe in the chromatograms generated by data acquisition. In general, these symptoms do not prevent you from operating your GC/MSD system. They indicate, however, that the data you are acquiring may not be the best data obtainable. These symptoms can be caused by instrument malfunctions, but are more likely caused by incorrect chromatographic technique. The following symptoms also apply to mass spectral data: • If sensitivity is low • If repeatability is poor 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 missing from the ALS, or not installed correctly • Injection accidentally made in split mode instead of splitless mode • Empty or almost empty sample vial • Dirty GC inlet • Leaking GC inlet† • Loose column nut at the GC inlet† † 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 2 General Troubleshooting Chromatographic Symptoms 5977B Series MSD Troubleshooting and Maintenance Manual 39 • Very dirty ion source • Calibration valve is not working correctly • Bad signal cable connection • Filament has failed, or is not connected correctly • Bad ion source wiring connection • Bad detector wiring connection • Failed electron multiplier horn Peaks are tailing • Active sites in the sample path • Injection is too large • Incorrect GC inlet 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 too low • Active sites in the sample path • 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 • Electron multiplier voltage is too high • Gain is too high 2 General Troubleshooting Chromatographic Symptoms 40 5977B Series MSD Troubleshooting and Maintenance Manual Peaks have split tops • Bad injection technique • Injection is too large Baseline is rising • 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 baseline 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 is not properly swept, resulting in excess solvent on the column and slow solvent decay) Baseline wanders • Insufficient carrier gas supply pressure† • Malfunctioning flow or pressure regulator† • Intermittent leak in the GC inlet† † These could cause a fault condition in the GC that would prevent the GC from operating. 2 General Troubleshooting Chromatographic Symptoms 5977B Series MSD Troubleshooting and Maintenance Manual 41 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 GC inlet† † This could cause a fault condition in the GC that would prevent the GC from operating. 2 General Troubleshooting Chromatographic Symptoms 42 5977B Series MSD Troubleshooting and Maintenance Manual Poor sensitivity • Incorrect tuning • Tune file that does not match the type of analysis • Repeller voltage is too low • Incorrect temperatures (oven, GC/MSD 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 • Excessive 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 GC inlet • Leaking GC inlet† • Injection is too large • Loose column connections • 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. 2 General Troubleshooting Mass Spectral Symptoms 5977B Series MSD Troubleshooting and Maintenance Manual 43 Mass Spectral Symptoms This section describes symptoms you might observe in mass spectra. Some of these symptoms will appear in the mass spectra of samples. Others you will observe only in a tune report. Some of these symptoms have causes that can be corrected by the operator. Others, however, require service by an Agilent Technologies service representative. The following symptoms listed under Chromatic symptoms also apply to mass spectra: • If sensitivity is low • If repeatability is poor No peaks • Ion source cables not connected • Bad connections to or from the detector • HED power supply output cable has failed • Other electronics failure • Incorrect tune file (inappropriate parameters) 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 2 General Troubleshooting Mass Spectral Symptoms 44 5977B Series MSD Troubleshooting and Maintenance Manual High background • Pressure in the analyzer chamber is too high • Air leak • Contamination High abundances at m/z H2O [18], N2 [28], O2 [32], and CO2 [44] or at m/z 14 and 16 • System was recently vented (residual air and water) • Air leak, large peaks at m/z 14 and 16 are symptomatic of especially large leaks. Mass assignments are incorrect Small shape changes at the top of the mass peaks can cause 0.1 m/z shifts in mass assignments. Shifts greater than 0.2 m/z indicate a possible malfunction. • MSD has not had enough time to reach thermal equilibrium • Scan speed is too fast • Large variations in the temperature of the laboratory • MSD has not been tuned recently, or at the temperature at which it is operating • Incorrect tune file (inappropriate parameters) • No voltage to extractor lens (if using an extractor ion source) Peaks have precursors The tune report lists the size of the precursors for the tune masses. Small precursors are not unusual. 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 2 General Troubleshooting Mass Spectral Symptoms 5977B Series MSD Troubleshooting and Maintenance Manual 45 Peak widths are inconsistent • MSD has not had enough time to reach thermal equilibrium • Large variations in the temperature of the laboratory • Incorrect tuning • Calibration vial(s) empty or almost empty • Calibration valve(s) not working correctly • Dirty ion source • Electron multiplier is nearing the end of its useful lifetime • Ground loop problems Relative abundance of m/z 502 is less than 3% Autotune should give an m/z 502 relative abundance greater than 3%. The relative abundance of m/z 502 can, however, vary a great deal depending on column flow, ion source temperature, and other variables. As long as relative abundance is above 3%, the stability of the relative abundance is more important than the absolute value. If you observe significant changes in the relative abundance of m/z 502 for a fixed set of operating parameters, there may be a problem. The charts in the MSD Data Acquisition software are useful for identifying changes. Low relative abundance of m/z 502 should not be confused with low absolute abundances at high masses. 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” on page 46. Tune programs other than autotune have different relative abundance targets. The DFTPP and BFB target tune programs tune the MSD to achieve about a 0.8% ratio of m/z 502/69. • Tune program/tune file has a different relative abundance target (3% only applies to Autotune) • Not enough time for the MSD to warm up and pump down • Analyzer chamber pressure is too high • Ion source temperature is too high • Column (carrier gas) flow is too high • Poor filament operation 2 General Troubleshooting Mass Spectral Symptoms 46 5977B Series MSD Troubleshooting and Maintenance Manual • Dirty ion source • Air leak • Incorrect DC polarity on the quadrupole mass filter Spectra look different from those acquired with other MSDs Ion ratios are different from those in older models MSDs. This is due to the HED detector, and is normal. High mass sensitivity is poor This refers to a condition where the absolute abundance at the upper end of the mass range is poor. Absolute abundance should not be confused with the 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 • Analyzer chamber pressure is too high • Column (carrier gas) flow is too high • Poor filament operation • Dirty ion source • Air leak • Incorrect DC polarity on the quadrupole mass filter • No voltage to the extractor lens (is using an extractor EI ion source) 2 General Troubleshooting Pressure Symptoms 5977B Series MSD Troubleshooting and Maintenance Manual 47 Pressure Symptoms This section describes unusual pressure readings and their possible causes. The symptoms in this section are based on typical pressures. At typical column flow rates (0.1 to 2.0 mL/minute), the foreline pressure will be approximately 20 to 100 mTorr. The analyzer chamber pressure will be approximately 1 × 10-6 to 1.4 × 10-4 Torr. These pressures can vary widely from instrument to instrument so it is very important that you are familiar with the pressures that are typical for your instrument at given carrier gas flows. The analyzer chamber 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 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) • Foreline pump oil level is low or oil is contaminated (standard foreline pump) • Foreline hose is constricted • Foreline pump is not working correctly Analyzer chamber pressure is too high (EI operation) If the pressure you observe is above 1.0 × 10-4 Torr, 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 • Foreline pump is not working correctly (see “Foreline pressure is too high” on page 47) • Turbo pump is not working correctly 2 General Troubleshooting Pressure Symptoms 48 5977B Series MSD Troubleshooting and Maintenance Manual Foreline pressure is too low If the pressures you observe are below 20 mTorr, check for the following: • Column (carrier gas) flow is too low • Column plugged or crushed by an overtightened nut • Empty or insufficient carrier gas supply† • Bent or pinched carrier gas tubing† • Foreline gauge is not working correctly † These could create a fault condition in the GC that would prevent the GC from operating. Analyzer chamber pressure is too low If the pressures you observe are below 1 × 10-6 Torr, check 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 analyzer chamber is above 8 × 10-3 Torr. • Solvent peak from an on-column injection • MSD has not had enough time to pump down • Excessive foreline pressure • Vacuum gauge has failed • Line voltage too low • Turbo pump is not working correctly 2 General Troubleshooting Pressure Symptoms 5977B Series MSD Troubleshooting and Maintenance Manual 49 Power indicator on the gauge controller does not light • Unplugged gauge controller power cord • Incorrect or inadequate line voltage (24 V supply) • Failed gauge controller fuse 2 General Troubleshooting Temperature Symptoms 50 5977B Series MSD Troubleshooting and Maintenance Manual Temperature Symptoms • The MSD has three heated zones: • Ion source • Mass filter • GC/MSD interface Each heated zone has a heater and temperature sensor. The ion source and mass filter are powered and controlled by the MSD. The GC/MSD interface is powered and controlled by the GC. For the 7820A Series GC’s, the heater is either connected to the rear inlet thermal zone for the single inlet models or connected to the manual valve thermal zone for dual inlet models. 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 or shorted to ground)† • Ion source temperature sensor failed† • Source power cable is not connected to the side board† • MSD electronics are not working correctly † These will cause an error message. Mass filter (quad) heater will not heat up • High vacuum pump is off or has not reached normal operating conditions† • Incorrect temperature setpoint • Mass filter has not had enough time to reach temperature setpoint • Mass filter heater cartridge is not connected† • Mass filter temperature sensor is not connected† • Mass filter heater failed (burned out or shorted to ground)† 2 General Troubleshooting Temperature Symptoms 5977B Series MSD Troubleshooting and Maintenance Manual 51 • Mass filter temperature 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(s) • 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 cable is not connected† • GC/MSD interface heater failed (burned out)† • GC/MSD interface sensor failed† • GC electronics are not working correctly† † These will cause a GC error message. GC error messages are described in the documentation supplied with your GC. 2 General Troubleshooting Error Messages 52 5977B Series MSD Troubleshooting and Maintenance Manual Error Messages Sometimes, a problem in your MSD will cause an error message to appear in the MSD Data Acquisition software. Some error messages appear only during tuning. Other messages may appear during tuning or data acquisition. Some error messages are latched. Latched 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 analyzer chamber is too high • RFPA is not adjusted correctly • Mass filter (quad) contacts are shorted or otherwise not working correctly • Mass filter is not working correctly • MSD electronics are not working correctly Difficulty with the electron multiplier supply • Large peak, such as the solvent peak, eluted while the analyzer was on • Pressure in the analyzer chamber is too high • MSD electronics are not working correctly Difficulty with the fan If a cooling fan fault occurs, the vacuum control electronics automatically shut off the high vacuum pump, the ion source, and the mass filter heaters. The message: The system is in vent state may also appear. It is important to note that even though the high vacuum pump is off, the analyzer chamber may not actually be vented. See “The system is in vent state” on page 56 for precautions to take. • One of the fans is disconnected • One of the fans has failed • MSD electronics are not working correctly 2 General Troubleshooting Error Messages 5977B Series MSD Troubleshooting and Maintenance Manual 53 Difficulty with the HED supply The only time this error occurs is if the output of the supply cannot get to its destination (the HED). • Large peak, such as the solvent peak, eluted while the analyzer was on • Pressure in the analyzer chamber is too high • Detector is not working correctly • MSD electronics are not working correctly Difficulty with the high vacuum pump In an MSD with a turbo pump, this indicates the pump failed to reach 50% of full speed within 7 minutes, or experienced a fault. You must switch the MSD off and back on to remove this error message. The message will reappear if the underlying problem has not been corrected. • Large vacuum leak is preventing the turbo pump from reaching 80% of full speed • Laboratory temperature is too high (generally above 35 °C) • Foreline pump is not working correctly • Turbo pump is not working correctly • Turbo pump controller is not working correctly • MSD electronics are not working correctly High foreline pressure • Excessive carrier gas flow (typically > 5 mL/min) • Excessive solvent volume injected • Large vacuum leak • Severely degraded foreline pump oil (standard foreline pump) • Collapsed or kinked foreline hose • Foreline pump is not working correctly 2 General Troubleshooting Error Messages 54 5977B Series MSD Troubleshooting and Maintenance Manual 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 amplifier ADC error • MSD electronics are not working correctly Data acquisition communication error The gas chromatographs and mass spectrometers supported by Data Acquisition GC/MS Acquisition Software require IPv4 Internet Protocol (IP) addresses. IPv6 IP addresses are not supported. Therefore, any data system computer (PC), router, switch, or hub that handles data packets to and from the instruments must use the IPv4 IP protocol and IPv4 IP addresses for the network interface used for the connections to the gas chromatographs and mass spectrometers. If required for other applications, the PC may also have the IPv6 Protocol configured as an optional configuration for the same network interface card, or a second network interface card. • LAN cable disconnected • Incorrect IP configuration • Incorrect IP address entered for the GC or MSD No peaks found • Emission current was set to 0 • Electron multiplier voltage is too low • Amu gain or offset is too high • Poor mass axis calibration • Calibration vial(s) empty or almost empty • Excessive pressure in the analyzer chamber 2 General Troubleshooting Error Messages 5977B Series MSD Troubleshooting and Maintenance Manual 55 • Air leak • Signal cable is not connected • Electrical leads to the detector are not connected correctly • HED power supply output cable failed • Electrical leads to the ion source are not connected correctly • Filament shorted to the source body Temperature control disabled • One of the heater fuses has failed • MSD electronics are not working correctly Temperature control fault This indicates that something has gone wrong with the temperature control of either the ion source or mass filter (quad) heater. The cause can be further isolated by selecting mp Status/MS TeCtlr Status in the Tune and Vacuum Control view. One of the following should be displayed as the cause: • Source temperature sensor is open • Source temperature sensor is shorted • Mass filter (quad) temperature sensor is open • Mass filter (quad) temperature sensor is shorted • No heater voltage (heater fuse has probably failed) • 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 • Source heater is open • Source heater is shorted • Mass filter heater is open • Mass filter heater is shorted 2 General Troubleshooting Error Messages 56 5977B Series MSD Troubleshooting and Maintenance Manual The high vacuum pump is not ready • Turbo pump is on but has not had enough time (5 minutes) to reach 80% of its normal operating speed • Turbo pump is not working correctly • MSD electronics are not working correctly The system is in standby This message is triggered by a shutdown signal on the remote start cable. It is usually caused by a GC fault, an ALS fault, or a bad cable connection. Once the cause of the fault is corrected, selecting MS ON or checking MSD status should remove the message. The system is in vent state Wait at least 30 minutes after seeing this message before you actually vent the MSD. • System was vented on purpose (no problem) • Fan fault has turned off the high vacuum pump (power cycle the MSD to clear the fault) • Fuse for the high vacuum pump has failed • MSD electronics are not working correctly There is no emission current • Filament is not connected properly; try the other filament • Filament has failed; try the other filament • MSD electronics are not working correctly There is not enough signal to begin tune • Corrupted tune file CAUTION Venting the MSD too soon after this message appears can damage the turbo pump. 2 General Troubleshooting Error Messages 5977B Series MSD Troubleshooting and Maintenance Manual 57 • Poor mass axis calibration • Amu gain or offset is too high • Calibration vial(s) empty or almost empty • Excessive pressure in the analyzer chamber • Air leak • Electron multiplier voltage is too low • Signal cable is not connected • 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 • Column inserted too far into source 2 General Troubleshooting Air Leaks 58 5977B Series MSD Troubleshooting and Maintenance Manual Air Leaks Air leaks are a problem for any instrument that requires a vacuum to operate. Leaks are generally caused by vacuum seals that are damaged or not fastened correctly. Symptoms of leaks include: • Higher than normal analyzer chamber pressure or foreline pressure • Higher than normal background • Peaks characteristic of air (m/z 18, 28, 32, and 44 or m/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 MSD. The most likely point for an air leak is a seal you recently opened. In the GC, most leaks occur in: • GC inlet septum • GC inlet column nut • Broken or cracked capillary column Leaks can occur in many more places in the MSD: • GC/MSD interface column nut • Side plate O-ring (all the way around) • Vent valve O-ring • Calibration valve(s) • GC/MSD interface O-ring (where the interface attaches to the analyzer chamber) • Front and rear end plate O-rings • Diffusion pump KF seal • Diffusion pump baffle adapter O-ring • Turbo pump O-ring 2 General Troubleshooting Contamination 5977B Series MSD Troubleshooting and Maintenance Manual 59 Contamination Contamination is usually identified by excessive background in the mass spectra. It can come from the GC or from the MSD. The source of the contamination can sometimes be determined by identifying the contaminants. Some contaminants are much more likely to originate in the GC. Others are more likely to originate in the MSD. 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 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 • Foreline pump oil (standard foreline pump) • Fingerprints (improper handling of clean parts) Table 6 on page 60 lists some of the more common contaminants, the ions characteristic of those contaminants, and the likely sources of those contaminants. 2 General Troubleshooting Contamination 60 5977B Series MSD Troubleshooting and Maintenance Manual Table 6 Common contaminants Ions (m/z) Compound Possible source 18, 28, 32, 44 or 14, 16 H20, N2, O2, CO2 or N, O Residual air and water, air leaks, outgassing from Vespel ferrules 31, 51, 69, 100, 119, 131, 169, 181, 214, 219, 264, 376, 414, 426, 464, 502, 576, 614 PFTBA and related ions PFTBA (tuning compound) 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 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 149 Plasticizer (phthalates) Vacuum seals (O-rings) damaged by high temperatures, vinyl gloves Peaks spaced 14 m/z apart Hydrocarbons Fingerprints, foreline pump oil 5977B Series MSD Troubleshooting and Maintenance Manual 61 3 CI Troubleshooting Common CI-Specific Problems 62 Troubleshooting Tips and Tricks 63 Air Leaks 64 Pressure-Related Symptoms 68 Signal-Related Symptoms 71 Tuning-Related Symptoms 78 This chapter outlines troubleshooting 5977B Series MSDs equipped with the chemical ionization (CI) ion source. Most of the troubleshooting information in the previous chapter also applies to CI MSDs. 3 CI Troubleshooting Common CI-Specific Problems 62 5977B Series MSD Troubleshooting and Maintenance Manual Common CI-Specific Problems Because of the added complexity of the parts required for CI, there are many potential problems added. The greatest number of, and most serious problems with CI are associated with leaks or contamination in the reagent gas introduction system. NCI is especially sensitive to the presence of air; small leaks that cause no problems in PCI can destroy NCI sensitivity. As with EI, if the MSD 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 reagent gas inlet port • Wrong ions entered in tune file • Wrong tune file selected • Not enough bakeout time has elapsed since vent (background is too high) • Wrong column positioning (extending > 2 mm past tip of interface) • Interface tip seal not installed • EI ion source installed in CI mode • EI filament or other EI ion source parts in CI ion source • Air leaks in reagent gas flow path • CI filament has stretched and sagged: • High EMV • Linear (no inflection point) electron energy (EIEnrgy) ramp 3 CI Troubleshooting Troubleshooting Tips and Tricks 5977B Series MSD Troubleshooting and Maintenance Manual 63 Troubleshooting Tips and Tricks Rule 1: Look for what has been changed. Many problems are introduced accidentally by human actions. Every time any system is disturbed, there is a chance of introducing a new problem. • If the MSD was just pumped down after maintenance, suspect air leaks or incorrect assembly. • If the reagent gas bottle or gas purifier were just changed, suspect leaks or contaminated or incorrect gas. • If the GC column was just replaced, suspect air leaks or contaminated or bleeding column. • If you have just switched ion polarity or reagent gas, suspect the tune file you have loaded in memory. Is it the appropriate file for your mode of operation? Rule 2: If complex is not working, go back to simple. A complex task is not only more difficult to perform, but also more difficult to troubleshoot as well. For example, CI requires more parts to work correctly than EI does. • If you are having trouble with NCI, verify that PCI still works. • If you are having trouble with other reagent gases, verify that methane still works. • If you are having trouble with CI, verify that EI still works. Rule 3: Divide and conquer. This technique is known as half-split troubleshooting. If you can isolate the problem to only part of the system, it is much easier to locate. • To isolate an air leak, select Shutoff valve. If the abundance of m/z 32 decreases, the problem is not in the flow module. 3 CI Troubleshooting Air Leaks 64 5977B Series MSD Troubleshooting and Maintenance Manual Air Leaks How do I know if I have an air leak? Large air leaks can be detected by vacuum symptoms: loud gurgling noise from the foreline pump, inability of the turbo pump to reach 95% speed, or, in the case of smaller leaks, high pressure readings on the high vacuum gauge controller. The mass flow controller is calibrated for methane, and the high vacuum gauge controller is 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 vacuum or gas flow problem. Always look for small air leaks when setting up methane flow. Select Methane Pretune from the Setup menu in the Agilent MassHunter GC/MS Acquisition software and follow the system prompts. See the software online help for additional information. The abundance of m/z 19 (protonated water) should be less than 50% of m/z 17 for acceptable PCI performance. For NCI, the abundance of m/z 19 (protonated water) should be less than 25% that of m/z 17. If the MSD was just pumped down, look for the abundance of m/z 19 to be decreasing. 3 CI Troubleshooting Air Leaks 5977B Series MSD Troubleshooting and Maintenance Manual 65 There should not be any peak visible at m/z 32 (O2). This almost always indicates an air leak. Special NCI notes Since NCI is so extremely sensitive, air leaks that are not detectable in EI or PCI can cause sensitivity problems in NCI. To check for this kind of air leak in NCI, inject OFN. The 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 on page 67 and Table 7 on page 67. 2 Look for the last seal that was disturbed. • If you just pumped down the MSD, press on the sideplate to check for proper seal. Poor alignment between the analyzer and the GC/MSD interface seal can prevent the sideplate from sealing. • If you just replaced the reagent gas bottle or gas purifier, check the fittings you just opened and refastened. Figure 2. Looking for air leaks 3 CI Troubleshooting Air Leaks 66 5977B Series MSD Troubleshooting and Maintenance Manual 3 Check for tightness of seals at GC inlet and interface column nuts. Ferrules for capillary columns often loosen after several heat cycles. Do not overtighten the interface nut. 4 If any of the fittings inside the flow module (VCR fittings) were loosened and then retightened, the gasket must be replaced. These gaskets are good for one use only. 5 Remember that most small air leaks visible in CI mode are located in either the carrier gas or reagent gas 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 select valves (Gas A then Gas B), then close the shutoff valve. See Figure 3 on page 67 and Table 7 on page 67. • Cool and vent the MSD, remove the GC column, and cap off the interface. Using argon or other introduced gas to find air leaks does not work well for the reagent gas flow system. It takes as long as 15 minutes for the peak to reach the ion source if the leak is at the inlet to the flow module. CAUTION Do not loosen the nuts on any VCR fittings unless you intend to replace the gaskets. Otherwise, you will create an air leak. 3 CI Troubleshooting Air Leaks 5977B Series MSD Troubleshooting and Maintenance Manual 67 Figure 3. Schematic of CI flow control module Gas A (methane) supply Gas B (other) supply Gas A select valve Gas B select valve MFC Calibration valve Restrictor Calibration vial Shutoff valve GC/MSD interface GC column CI source Table 7 Flow module valve state diagram Result Gas A flow Gas B flow Purge with Gas A Purge with Gas B Pump out flow module Standby, vented, or EI mode Gas A Open Closed Open Closed Closed Closed Gas B Closed Open Closed Open Closed Closed MFC 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 3 CI Troubleshooting Pressure-Related Symptoms 68 5977B Series MSD Troubleshooting and Maintenance Manual Pressure-Related Symptoms The following symptoms are all related to high vacuum pressure. Each symptom is discussed in more detail in the following pages. The mass flow controller is calibrated for methane, and the high vacuum gauge controller is calibrated for nitrogen, so these measurements are not accurate in absolute terms (Table 8). They are intended as a guide to typical observed readings. They were taken with the following set of conditions: Poor vacuum without reagent gas flow Excess water in the background Scan from 10 to 40 m/z. A large peak at m/z 19 (>m/z 17) indicates water in the background. If water is present, allow the instrument to bake out more, and flow reagent gas through the lines to purge any accumulated water. Source temperature 250 °C Quad temperature 150 °C GC/MSD Interface temperature 280 °C Helium carrier gas flow 1 mL/min Table 8 Pressure measurements Pressure (Torr) MFC (%) Methane Ammonia 10 5.5 × 10–5 5.0 × 10–5 15 8.0 × 10–5 7.0 × 10–5 20 1.0 × 10–4 8.5 × 10–5 25 1.2 × 10–4 1.0 × 10–4 30 1.5 × 10–4 1.2 × 10–4 35 2.0 × 10–4 1.5 × 10–4 40 2.5 × 10–4 2.0 × 10–4 3 CI Troubleshooting Pressure-Related Symptoms 5977B Series MSD Troubleshooting and Maintenance Manual 69 Air leak In PCI mode, select Methane Pretune from the Setup menu in the Agilent MassHunter GC/MS Acquisition software, and follow the system prompts. See the software online help for additional information. A visible peak at m/z 32 indicates air in the system. Check for, and correct any leaks. See “Air Leaks” on page 64. 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 pump, it may be necessary to replace the pump. Contact your local Agilent Technologies Customer Engineer. The turbo pump is not working properly Check the pump speed. It should be at least 95%. Contact your local Agilent Technologies service representative. High pressure with reagent gas flow The reagent gas flow rate is too high On the flow controller, turn down reagent gas flow as appropriate. Verify that reagent ion ratios are correct. Air leak Select Methane Pretune from the Setup menu in the Agilent MassHunter GC/MS Acquisition software, and follow the system prompts. See the software online help for additional information. A visible peak at m/z 32 indicates air in the system. Check for, and correct any leaks. See “Air Leaks” on page 64. Interface tip seal is not installed Check the source storage box. If the seal is not in the box, vent the MSD and verify that the seal is correctly installed. CAUTION Use of ammonia as reagent gas can shorten the life of the foreline pump oil (with standard pump) and possibly of the foreline pump itself. 3 CI Troubleshooting Pressure-Related Symptoms 70 5977B Series MSD Troubleshooting and Maintenance Manual Pressure does not change when reagent flow is changed The reagent gas regulator is closed Check and, if necessary, open the reagent gas regulator. The reagent gas regulator is set to the wrong pressure Set the reagent gas regulator to 10 psi (70 kPa) for methane or to 3 to 10 psi (20 to 70 kPa) for isobutane 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 reagent gas supply. Reagent lines kinked, bent, pinched, or disconnected Inspect the reagent lines, and repair any defects. Check especially to ensure the reagent line is connected to the rear of the flow module. Ensure the methane line is connected to the Gas A inlet. GC/MSD interface clogged or damaged Check for flow, and repair or replace components as indicated. 3 CI Troubleshooting Signal-Related Symptoms 5977B Series MSD Troubleshooting and Maintenance Manual 71 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 page 71. • No or low reagent gas signal, see page 73. • No or low PFDTD signal, see page 75. • Excessive noise, see page 76. • Low signal-to-noise ratio, see page 76. • Large peak at m/z 19, see page 76. • Peak at m/z 32, see page 77. 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 the MSD 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 page 68. 3 CI Troubleshooting Signal-Related Symptoms 72 5977B Series MSD Troubleshooting and Maintenance Manual If the MSD was recently switched from EI to CI • Isolation tip not installed • No reagent gas flow • Analyzer not sealed (big air leak) • Wrong tune file loaded or tune file corrupted • Ion source not assembled or connected correctly • Wrong reagent gas selected for the tune file (looking for wrong ions) No PFDTD peaks in PCI • Incorrect reagent gas. There are no PCI PFDTD peaks created with isobutane or ammonia. Switch to methane. • Analyzer 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 ions instead. • Verify tune parameters. • If no background ions are visible, go back to methane PCI. No PFDTD calibrant peaks in NCI • Look for background ions: 17 (OH–), 35 (Cl–), and 235 (ReO3–). • Verify tune parameters. • Go back to methane PCI. No sample peaks in NCI • Look for background ions: 17 (OH–), 35 (Cl–), and 235 (ReO3–). • Go back to methane PCI. • Poor quality reagent gas (purity less than 99.99%). 3 CI Troubleshooting Signal-Related Symptoms 5977B Series MSD Troubleshooting and Maintenance Manual 73 Large peak at m/z 238 in NCI OFN spectrum • Look for background ions: 17 (OH–), 35 (Cl–), and 235 (ReO3–). • Find and fix your small air leak. No or low reagent gas signal If you have just installed the CI ion source and have an air leak or large amounts of water in the system after running one or more autotunes, the ion source is probably dirty. Fix the air leak. Clean the ion source, and bake out for 2 hours before tuning. See the Agilent 5977B Series MSD Operating Manual. The wrong reagent gas is flowing. Turn on the correct reagent gas for your tune file. Ion polarity is set to Negative. No reagent gas ions are formed in NCI. Switch to Positive ionization mode. The reagent gas flow is set too low. Increase the reagent gas flow. 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. Ensure that the filament 1 wires are connected to the CI ion source filament, and that the filament 2 wires are connected to the dummy filament. Carbon has built up on the filament, or the filament has sagged out of alignment. Inspect the filament, if necessary, replace the filament. 3 CI Troubleshooting Signal-Related Symptoms 74 5977B Series MSD Troubleshooting and Maintenance Manual Too much air or water in the system. In PCI mode, select Methane Pretune from the Setup menu in the Agilent MassHunter GC/MS Acquisition software, and follow the system prompts. See the software online help for additional information. Peaks at m/z 32 and 19 usually indicate air and water, respectively. Bake out and purge the instrument until there is no visible peak at m/z 32, and the peak at m/z 19 is reduced to a very low level. If the peak at m/z 32 does not decrease, an air leak is likely. See“Air Leaks” on page 64 for more information. The signal cable is not connected. Check and, if necessary, reconnect the signal cable. The filament or filament support is shorted to the ion source body or repeller. Inspect the filament, if necessary, realign the filament support arms. The electron inlet hole is blocked. Inspect the electron inlet hole and, if necessary, clean the hole with a clean toothpick and a slurry of aluminum oxide powder and methanol. If the electron inlet hole is that dirty, the entire ion source probably needs to be cleaned. Ion source wires are not connected, or incorrectly connected. Inspect the repeller. Ensure the repeller lead is firmly attached to the repeller. Inspect the wires to the ion focus and entrance lenses. If the connections are reversed, correct the problem. One of the detector leads (in the analyzer chamber) is not connected. Check and, if necessary, reconnect the electron multiplier leads. Saturated methane/isobutane gas purifier Replace the gas purifier. Poor quality methane (purity below 99.99%) Replace the methane with high-purity methane. If necessary, clean and purge the reagent gas lines and clean the ion source. 3 CI Troubleshooting Signal-Related Symptoms 5977B Series MSD Troubleshooting and Maintenance Manual 75 No or low PFDTD signal, but reagent ions are normal You are using any reagent gas but methane in PCI. Switch to methane. Wrong or corrupted tune file loaded Check your tune file. No PFDTD in the calibrant vial Inspect the calibration vial on the back of the flow controller. If necessary, fill the vial with PFDTD. Do not fill the vial completely; keep the level at least 0.5 cm from the top of the vial. The pressure of the methane entering the flow controller is too high. Ensure the regulator on the methane supply is set to 10 psig (70 kPa). The CI ion source is dirty. Clean the ion source. The calibration valve was not purged after the vial was refilled. Purge the calibration valve as described in “To Purge the Calibration Valves” on page 122. Then clean the ion source. The calibrant vial was overfilled. Excess PFDTD can quench the chemical ionization reactions. Check the level of the PFDTD in the calibration vial. It should be below the end of the inside tube in the vial. Poor quality methane (purity below 99.99%) Replace the methane with high-purity methane. If necessary, clean and purge the reagent gas lines and clean the ion source. 3 CI Troubleshooting Signal-Related Symptoms 76 5977B Series MSD Troubleshooting and Maintenance Manual Excessive noise or low signal-to-noise ratio The GC inlet needs maintenance. Refer to the GC manual. The CI ion source is dirty. Clean the ion source. Poor vacuum Check the pressure on the high vacuum gauge controller. Air leak In PCI mode, select Methane Pretune from the Setup menu in the Agilent MassHunter GC/MS Acquisition software, and follow the system prompts. See the software online help for additional information. A large peak at m/z 32 indicates air in the system. Check for, and correct any leaks. See “Air Leaks” on page 64. Saturated methane/isobutane gas purifier Replace the gas purifier. Poor quality methane (purity below 99.99%) Replace the methane with high-purity methane. If necessary, clean and purge the reagent gas lines and clean the ion source. Reagent gas flows too high (in EI/PCI MSDs) Verify that the reagent gas setup is correct. Large peak at m/z 19 If the abundance of the peak at m/z 19 is more than half abundance of the peak at m/z 17, there probably is too much water in the system. The system was not baked out sufficiently after it was last vented. Bake out the system as described in the Maintenance chapter of this manual. 3 CI Troubleshooting Signal-Related Symptoms 5977B Series MSD Troubleshooting and Maintenance Manual 77 Moisture left over in the reagent gas supply tubing and flow module Purge the reagent gas supply lines for at least 60 minutes. Contaminated reagent gas supply Replace the reagent gas supply, and purge the lines and flow module. Saturated methane/isobutane gas purifier Replace the gas purifier. Peak at m/z 32 A visible peak at m/z 32 in methane pretune often indicates air in the system. Residual air from recent venting — check for water indicated by a large peak at m/z 19. To eliminate water, bake out the system under vacuum. New or dirty reagent gas supply tubing Purge the reagent gas supply lines and flow module for at least 60 minutes. See the Agilent 5977B Series MSD Operating Manual. Air leak Check for leaks, and correct any that you find. See“Air Leaks” on page 64. After all leaks have been corrected, clean the ion source. Contaminated reagent gas supply. Suspect this if you have recently replaced your gas tank, and you have ruled out air leaks. Replace the reagent gas supply. The capillary column is broken or disconnected. Inspect the capillary column. Ensure it is not broken and it is installed correctly. Saturated methane/isobutane gas purifier Replace the gas purifier. 3 CI Troubleshooting Tuning-Related Symptoms 78 5977B Series MSD Troubleshooting and Maintenance Manual Tuning-Related Symptoms This section 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 adjust or unstable • High electron multiplier voltage • Cannot complete autotune • Peak widths are unstable Reagent gas ion ratio is difficult to adjust or unstable The interface tip seal is incorrectly placed, damaged, or missing. Inspect the Isolation tip. If necessary, remove and reinstall it to ensure a good seal with the CI ion source. Replace it if it is damaged. Install it if it is missing. Residual air and water in the MSD or in the reagent gas supply lines In PCI mode, select Methane Pretune from the Setup menu in the Agilent MassHunter GC/MS Acquisition software, and follow the system prompts. See the software online help for additional information. Air will appear as a peak at m/z 32 and excessive water as a peak at m/z 19 > m/z 17. If either of these conditions is present, purge the reagent gas supply lines and bake out the MSD. See “To Clean the Reagent Gas Supply Lines” on page 141. 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 leak In PCI mode, select Methane Pretune from the Setup menu in the Agilent MassHunter GC/MS Acquisition software, and follow the system prompts. See the software online help for additional information. Large peak at m/z 32 indicates air in the system. Check for and correct any leaks. See“Air Leaks” on page 64. 3 CI Troubleshooting Tuning-Related Symptoms 5977B Series MSD Troubleshooting and Maintenance Manual 79 The reagent gas supply is at the wrong pressure. Check the regulator on the reagent gas supply. It should be adjusted to 20 psi (140 kPa). A leak in the reagent gas delivery path. This is especially likely if you have set the methane flow much higher than normal and the ratio is still too low. Check the reagent gas path. Tighten fittings. The CI ion source is dirty. Clean the ion source. High electron multiplier voltage The electron multiplier voltage can range from a few hundred volts to 3,000 V. If the CI autotune program consistently sets the electron multiplier voltage at or above 2,600 V but can still find peaks and complete the tune, it may indicate a problem. The filament is worn out. The CI filament may wear out without actually breaking. Check the Electron Energy ramp; the curve should have a definite maximum with an 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 source body, and most electrons are not getting into the source. Replace the filament. The analyzer is not at the proper operating temperature. Verify the ion source and quadrupole temperatures. The default source temperature is 250 °C for PCI and 150 °C for NCI. The quadrupole temperature is 150 °C for both CI modes. The CI ion source is dirty. Clean the ion source. The electron multiplier (detector) is failing. Switch to EI mode and confirm. Replace the electron multiplier. 3 CI Troubleshooting Tuning-Related Symptoms 80 5977B Series MSD Troubleshooting and Maintenance Manual Cannot complete Autotune Wrong or corrupted tune file Check the tune parameters. 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 5977B Series MSD Operating Manual. The CI ion source is dirty. Clean the source. Too much air or water in the system See“Air Leaks” on page 64. After eliminating these problems, clean the ion source. Peak widths are unstable Wrong or corrupted tune file Check the tune parameters. The CI ion source is dirty. Clean the ion source. Air leak In PCI mode, select Methane Pretune from the Setup menu in the Agilent MassHunter GC/MS Acquisition software, and follow the system prompts. See the software online help for additional information. A visible peak at m/z 32 indicates air in the system. Check for and correct any leaks. See“Air Leaks” on page 64”. After eliminating all air leaks, clean the ion source. 5977B Series MSD Troubleshooting and Maintenance Manual 81 4 General Maintenance Before Starting 83 Maintaining the Vacuum System 88 To Separate the MSD from an 8890 or 7890 GC 89 To Separate the MSD from the 9000 GC 91 To Reconnect the MSD to an 8890 or 7890 GC 93 To Reconnect the MSD to the 9000 GC 94 To Move or Store the MSD when Connected to an 8890 or 7890 GC 96 To Move or Store the MSD when Connected to a 9000 GC 98 To Check the Foreline Pump Oil 100 To Drain the Foreline Pump 102 To Refill the Foreline Pump 103 To Change the Oil Mist Filter on the Foreline Pump 104 To Install the Exhaust Filter on the IDP3 Dry Pump 106 To Change the Filter Cartridge on the IDP3 Dry Foreline Pump 108 To Check the DP Fluid 109 To Remove the DP 111 To Replace the DP Fluid 113 To Install the DP 115 To Remove the Foreline Gauge 117 To Install the Foreline Gauge 119 To Refill the EI Calibration Vial 120 To Purge the Calibration Valves 122 To Remove the EI Calibration and Vent Valve Assembly 123 To Install the EI Calibration and Vent Valve Assembly 124 4 General Maintenance 82 5977B Series MSD Troubleshooting and Maintenance Manual To Replace the Fan for the High Vacuum Pump 125 To Remove the Ion Vacuum Gauge 127 To Install an Ion Vacuum Gauge 127 To Lubricate the Side Plate O-Ring 128 To Lubricate the Vent Valve O-Ring 130 Maintaining the Electronics 132 To Adjust the Quad Frequency 134 To Replace the Primary Fuses 136 4 General Maintenance Before Starting 5977B Series MSD Troubleshooting and Maintenance Manual 83 Before Starting For your safety, read all of the information in this introduction before performing any maintenance tasks. Scheduled maintenance Performing common maintenance tasks when scheduled can reduce operating problems, prolong system life, and reduce overall operating costs. (See Table 9.) Keep a record of system performance (tune reports) and maintenance operations performed. This makes it easier to identify variations from normal operation, and to take corrective action. Table 9 Maintenance schedule Task Every week Every 6 months Every year As needed Tune the MSD X Check the foreline pump oil level X Check the calibration vial(s) X Replace the foreline pump oil* X Replace the DP fluid X Check the dry foreline pump X Change the dry foreline pump tip seal X Change the foreline pump oil mist filter X Clean the ion source X Check the carrier gas trap(s) on the GC and MSD X Replace the worn out parts X Lubricate sideplate or vent valve O-rings† X Replace CI Reagent gas supply X Replace GC gas supplies X * Every 3 months for CI MSDs using ammonia 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. 4 General Maintenance Before Starting 84 5977B Series MSD Troubleshooting and Maintenance Manual Tools, spare parts, and supplies Some of the required tools, spare parts, and supplies are included in the GC shipping kit, MSD shipping kit, or MSD tool kit. You must supply others yourself. Each maintenance procedure includes a list of the materials required for that procedure. (See “Consumables and Maintenance Supplies” on page 236.) High voltage precautions Whenever the MSD is plugged in, even if the power switch is off, potentially dangerous voltage (120 VAC or 200/240 VAC) exists on: • The wiring and fuses between where the power cord enters the instrument and the power switch When the power switch is on, potentially dangerous voltages exist on: • Electronic circuit boards • Toroidal transformer • 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 accidentally make contact with dangerous voltages. Some procedures in this chapter require access to the inside of the MSD while the power switch is on. Do not remove any of the electronics safety covers in any of these procedures. To reduce the risk of electric shock, follow the procedures carefully. WARNING Do not perform maintenance with the MSD turned on or plugged into its power source unless you are instructed by one of the procedures in this chapter to do so. 4 General Maintenance Before Starting 5977B Series MSD Troubleshooting and Maintenance Manual 85 Dangerous temperatures Many parts in the MSD operate at, or reach, temperatures high enough to cause serious burns. These parts include, but are not limited to the: • GC inlets • GC oven and its contents, including the column nuts attaching the column to a GC inlet, GC/MSD interface, or GC detector • GC detector • GC valve box • Foreline pump • Diffusion pump • Heated MSD ion source, GC/MSD interface, and quadrupole The GC inlets 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. WARNING Never touch these parts while your MSD is on. After the MSD is turned off, give these parts enough time to cool before handling them. WARNING The GC/MSD interface heater is powered by a heated zone on the GC. The interface heater can be on, and at a dangerously high temperature, even though the MSD is off. The GC/MSD interface is well insulated. Even after it is turned off, it cools very slowly. WARNING The foreline pump can cause burns if touched when operating. It has a safety shield to prevent the user from touching it. 4 General Maintenance Before Starting 86 5977B Series MSD Troubleshooting and Maintenance Manual Chemical residue Only a small portion of your sample is ionized by the ion source. The majority of any sample passes through the ion source without being ionized. It is pumped away by the vacuum system. As a result, the exhaust from the foreline pump will contain traces of the carrier gas and your samples. Exhaust from the standard foreline pump also contains tiny droplets of foreline pump oil. An oil trap is supplied with the standard foreline pump. This trap stops only pump oil droplets. It does not trap any other chemicals. If you are using toxic solvents or analyzing toxic chemicals, do 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 standard foreline pump, this requires removing the oil trap. Comply with your local air quality regulations. The fluids in the DP and standard foreline pump also collect traces of the samples being analyzed. All used pump fluid should be considered hazardous and handled accordingly. Dispose of used fluid correctly, as specified by your local regulations. Electrostatic discharge 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 electronics boards to which they are connected. This is especially true of the mass filter (quadrupole) contact wires which can carry ESD to sensitive components on the side board. ESD damage may not cause immediate failure, but it will gradually degrade the performance and stability of your MSD. When you work on or near 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 precautions. The wrist strap should be connected to a known good earth ground. WARNING The oil trap supplied with the standard foreline pump 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 have a CI MSD. Install a hose to take the foreline pump exhaust outside or to a fume hood. WARNING When replacing pump fluid, use appropriate chemical-resistant gloves and safety glasses. Avoid all contact with the fluid. 4 General Maintenance Before Starting 5977B Series MSD Troubleshooting and Maintenance Manual 87 If that is not possible, it should be connected to a conductive (metal) part of the assembly being worked on, but not to electronic components, exposed wires or traces, or pins on connectors. Take extra precautions, such as a grounded antistatic mat, if you must work on components or assemblies that have been removed from the MSD. This includes the analyzer. CAUTION To be effective, an antistatic wrist strap must fit snugly (not tight). A loose strap provides little or no protection. 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. 4 General Maintenance Maintaining the Vacuum System 88 5977B Series MSD Troubleshooting and Maintenance Manual Maintaining the Vacuum System Periodic maintenance Some maintenance tasks for the vacuum system must be performed periodically. (See Table 9 on page 83.) These include: • Checking the foreline pump oil (every week) • Checking the calibration vial (every 6 months) • Replacing the foreline pump oil (every 6 months; every 3 months for CI MSDs using ammonia reagent gas, standard foreline pump) • Tightening the foreline pump oil box screws (first oil change after installation, standard foreline pump) • Changing the foreline pump exhaust filters • Replacing the DP fluid (once a year) • Changing the dry foreline pump tip seal (once a year) Failure to perform 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 a Micro-Ion vacuum gauge should be performed only when needed. (See“General Troubleshooting” on page 33.) Refer to the online help in the Agilent MassHunter GC/MS Acquisition software for symptoms that indicate this type of maintenance is required. More information is available If you need more information about the locations or functions of vacuum system components. (See“Vacuum System” on page 145.) Most of the procedures in this chapter are illustrated with video clips on the 5977B Series MSD User Information media. 4 General Maintenance To Separate the MSD from an 8890 or 7890 GC 5977B Series MSD Troubleshooting and Maintenance Manual 89 To Separate the MSD from an 8890 or 7890 GC Materials needed • Wrench, open-end, 1/4-inch × 5/16-inch (8710-0510) Procedure 1 Vent the MSD. 2 Turn off the GC. 3 Remove the capillary column from the GC/MSD interface. 4 The foreline pump may be located on the floor, on the lab bench next to or behind the MSD, or under the analyzer chamber at the back of the MSD. Move it as needed to provide slack in the tubing and cables. 5 Move the MSD away from the GC until you have access to the GC/MSD interface cable. (See Figure 4.) WARNING Ensure the GC/MSD interface and GC oven have cooled before you remove the column. Figure 4. Separating and connecting the MSD and GC The Agilent 7890 GC has a front and a back location for the MSD interface. The Agilent 7820A GC has only one location for the MSD interface. Interface cable LVDS cable 4 General Maintenance To Separate the MSD from an 8890 or 7890 GC 90 5977B Series MSD Troubleshooting and Maintenance Manual 6 Place a column nut with a blank ferrule on the end of the interface. This will help keep contamination out of the MSD. 7 Disconnect the GC/MSD interface cable and the LVDS cable (if applicable). LVDS cable position will vary on different models of GC. Disconnecting either cable with the GC on can cause a fault condition. 8 Continue to move the MSD until you have access to the part requiring maintenance. 4 General Maintenance To Separate the MSD from the 9000 GC 5977B Series MSD Troubleshooting and Maintenance Manual 91 To Separate the MSD from the 9000 GC Materials needed • Screwdriver, T-20 Torx (8710-1615) Procedure Separate the MSD and 9000 GC 1 Remove the 9000 GC/MSD Tail. Refer to the Agilent 5977B Series MSD Operating Manual. 2 Power off the GC. 3 Using a T-20 Torx screwdriver, loosen the lock plate by turning the lock plate screw clockwise. 4 The foreline pump may be located on the floor, on the lab bench next to or behind the MSD, or under the analyzer chamber at the back of the MSD. Move it as needed to provide slack in the tubing and cables. 5 Slide the MSD backwards, and then away from the GC until you have access to the GC/MSD cables. (See Figure 5 on page 92.) WARNING Ensure the GC/MSD interface and the analyzer zones are cool (below 100 °C) before you vent the MSD. A temperature of 100 °C is hot enough to burn skin; always wear cloth gloves when handling analyzer parts. WARNING If you are using hydrogen as a carrier gas, the carrier gas flow must be closed before turning off the MSD power. If the foreline pump is off, hydrogen will accumulate in the MSD and an explosion may occur. Before operating the MSD with hydrogen carrier gas read the hydrogen safety information. (See“Hydrogen Safety” on page 22.) CAUTION Ensure the GC heated zones and the GC/MSD interface are cool before turning off carrier gas flow. WARNING Ensure the GC/MSD interface and GC heated zones have cooled before you remove the 9000 GC/MSD Tail. 4 General Maintenance To Separate the MSD from the 9000 GC 92 5977B Series MSD Troubleshooting and Maintenance Manual 6 Disconnect the GC/MSD interface heater cables, and the LVDS cable. Disconnecting the interface heater cables with the GC on can cause a fault condition. 7 Continue to move the MSD until you have access to the part requiring maintenance. Figure 5. GC/MSD interface heater cables and LVDS cable Interface cables LVDS cable 4 General Maintenance To Reconnect the MSD to an 8890 or 7890 GC 5977B Series MSD Troubleshooting and Maintenance Manual 93 To Reconnect the MSD to an 8890 or 7890 GC Materials needed • Wrench, open-end, 1/4-inch × 5/16-inch (8710-0510) Procedure 1 Position the MSD so the end of the GC/MSD interface is near the GC. 2 Reconnect the GC/MSD interface and the LVDS cables (if applicable). 3 Slide the MSD to its regular position next to the GC. Be careful not to damage the GC/MSD interface as it passes into the GC. Ensure the end of the GC/MSD interface extends into the GC oven. 4 The foreline pump may be located on the floor, on the lab bench next to or behind the MSD, or under the analyzer chamber at the back of the MSD. 5 Reinstall the capillary column. 6 Pump down the MSD. 7 Turn on the MS and GC. Enter appropriate temperature setpoints for the GC/MSD interface and GC oven. 4 General Maintenance To Reconnect the MSD to the 9000 GC 94 5977B Series MSD Troubleshooting and Maintenance Manual To Reconnect the MSD to the 9000 GC This procedure starts with both instruments shut down and at room temperature. Procedure 1 Position the MSD so the end of the GC/MSD interface is near the GC. (See Figure 5 on page 92.) 2 Tighten the thumb screw at the top of the interface heater clamp. If the thumb screw is loose when reconnecting the GC/MSD, it will be difficult to retighten when installing the 9000 GC/MSD Tail. 3 Connect the GC/MSD interface heater cables and LVDS cable. 4 Slide the MSD against the GC with the transfer line entering the GC side opening, and the metal brackets entering their slots in the base of the GC. Be careful not to damage the GC/MSD interface as it passes into the GC. 5 Open the GC front door. 6 Slide the MS forward until the GC/MSD interface lightly contacts the bus. (See Figure 6.) Figure 6. GC/MSD interface and bus 4 General Maintenance To Reconnect the MSD to the 9000 GC 5977B Series MSD Troubleshooting and Maintenance Manual 95 7 Using a T-20 Torx screwdriver, tighten the lock plate by turning the lock plate screw counter clockwise. 8 Install the 9000 GC/MSD Tail. 9 If the MSD is equipped with an MFC, attach the MFC gas lines. CAUTION Do not turn on any GC heated zones until carrier gas flow is on. Heating a column with no carrier gas flow will damage the column. CAUTION During pumpdown, do not push on the filament board safety cover while pressing on the analyzer boards. This cover was not designed to withstand this type of pressure. WARNING Ensure your MSD meets all the conditions listed in the Pumpdown section of the Agilent 5977B Series MSD Operating Manual before starting up and pumping down the MSD. Failure to do so can result in personal injury. 4 General Maintenance To Move or Store the MSD when Connected to an 8890 or 7890 GC 96 5977B Series MSD Troubleshooting and Maintenance Manual To Move or Store the MSD when Connected to an 8890 or 7890 GC Materials needed • Ferrule, blank (5181-3308) • Interface column nut (05988-20066) • Wrench, open-end, 1/4-inch × 5/16-inch (8710-0510) Procedure 1 Move the MSD away from the GC. (See “To Separate the MSD from an 8890 or 7890 GC” on page 89.) 2 Tighten the vent valve. 3 Install the interface nut and blank ferrule on the GC end of the GC/MSD interface. 4 Open the analyzer cover. 5 Finger-tighten the side plate thumbscrews. (See Figure 7 on page 97.) 6 Plug the MSD power cord in. 7 Switch the MSD on for 5 minutes to establish a rough vacuum. 8 Switch the MSD off. 9 Close the analyzer cover. 10 Disconnect the LAN, remote, and power cables. CAUTION Do not overtighten the side plate thumbscrews. Overtightening will strip the threads in the analyzer chamber. It will also warp the side plate and cause leaks. 4 General Maintenance To Move or Store the MSD when Connected to an 8890 or 7890 GC 5977B Series MSD Troubleshooting and Maintenance Manual 97 The MSD can now be stored or moved. The foreline pump cannot be disconnected; it must be moved with the MSD. Ensure the MSD remains upright, and is never tipped on its side or inverted. Figure 7. Side plate thumbscrews Front thumbscrew Rear thumbscrew CAUTION The MSD must remain upright at all times. If you need to ship your MSD to another location, contact your Agilent Technologies service representative for advice about packing and shipping. 4 General Maintenance To Move or Store the MSD when Connected to a 9000 GC 98 5977B Series MSD Troubleshooting and Maintenance Manual To Move or Store the MSD when Connected to a 9000 GC Materials needed • Ferrule, blank (5181-3308) • Interface column nut (05988-20066) • 7/16-inch open-end wrench Procedure 1 Separate the MSD and the 9000 GC. (See “To Separate the MSD from the 9000 GC” on page 91.) 2 Install a blank ferrule and interface column nut on the GC end of the GC/MSD interface. 3 Tighten the vent valve. 4 Open the analyzer cover. 5 Finger-tighten the side plate thumbscrews. (See Figure 7 on page 97.) 6 Plug the MSD power cord in. 7 Switch the MSD on for 5 minutes to establish a rough vacuum. 8 Switch the MSD off. 9 Close the analyzer cover. 10 Disconnect the LAN, remote, and power cables. CAUTION Do not overtighten the side plate thumbscrews. Overtightening will strip the threads in the analyzer chamber. It will also warp the side plate and cause leaks. 4 General Maintenance To Move or Store the MSD when Connected to a 9000 GC 5977B Series MSD Troubleshooting and Maintenance Manual 99 The MSD can now be stored or moved. The foreline pump cannot be disconnected; it must be moved with the MSD. Ensure the MSD remains upright, and is never tipped on its side or inverted. Figure 8. Side plate thumbscrews Front thumbscrew Rear thumbscrew CAUTION The MSD must remain upright at all times. If you need to ship your MSD to another location, contact your Agilent Technologies service representative for advice about packing and shipping. 4 General Maintenance To Check the Foreline Pump Oil 100 5977B Series MSD Troubleshooting and Maintenance Manual To Check the Foreline Pump Oil Standard foreline pumps only Materials needed • Foreline pump oil (6040-0621) • Funnel (9301-6461) • Hex key to remove drain plug (5 mm for Pfeiffer pump, 8710-1838) • Screwdriver, flat-blade, to remove fill cap Procedure Always replace the oil if it is dark or cloudy or due for replacement instead of adding oil. (See“To Drain the Foreline Pump” on page 102 and“To Refill the Foreline Pump” on page 103.) 1 Examine the oil level window (Figure 9 on page 101). 2 Note the two lines on the pump left of the window. The oil level should be between the lines. The foreline pump oil should be almost clear. If the oil level is near or below the lower line, add foreline pump oil. (See“To Refill the Foreline Pump” on page 103, starting at step four.) WARNING The foreline pump can cause burns if touched when operating. It has a safety shield to prevent the user from touching it. WARNING Never add oil while the foreline pump is on. 4 General Maintenance To Check the Foreline Pump Oil 5977B Series MSD Troubleshooting and Maintenance Manual 101 Figure 9. Pfeiffer Duo foreline pump Fill cap Oil level line Drain plug Oil mist filter 4 General Maintenance To Drain the Foreline Pump 102 5977B Series MSD Troubleshooting and Maintenance Manual To Drain the Foreline Pump Standard foreline pump only Materials needed • Book or other solid object approximately 5 cm thick • Container for catching old pump oil, 500 mL • Gloves, oil- and solvent-resistant • Screwdriver, flat-blade, large (8730-0002) • Hex key to remove drain plug (5 mm for Pfeiffer pump, 8710-1838) Procedure 1 Vent the MSD. 2 If necessary, slide the foreline pump to a safe, accessible location. The foreline pump may be located on the floor, on the lab bench next to or behind the MSD, or under the analyzer chamber at the back of the MSD. 3 Remove the fill cap. (See Figure 9 on page 101.) 4 Place a container under the drain plug. 5 Remove the drain plug. Allow the pump oil to drain out. The oil drains faster if it is still warm. If necessary, you can place a book or other object under the pump motor to tilt it up slightly. 6 Reinstall the drain plug after draining the oil. WARNING The foreline pump can cause burns if touched when operating. It has a safety shield to prevent the user from touching it. WARNING The old pump oil may contain toxic chemicals. Treat it as hazardous waste. 4 General Maintenance To Refill the Foreline Pump 5977B Series MSD Troubleshooting and Maintenance Manual 103 To Refill the Foreline Pump Standard foreline pump only Materials needed • Foreline pump oil (6040-0621) – approximately 0.28 L required • Funnel (9301-6461) • Gloves, oil- and solvent-resistant • Screwdriver, flat-blade, large (8730-0002) • Drain plug O-ring (if required) (0905-1515) • Hex key to remove drain plug (5 mm for Pfeiffer pump, 8710-1838) Procedure 1 Drain the foreline pump. (See“To Drain the Foreline Pump” on page 102.) 2 Reinstall the drain plug. If the old O-ring appears worn or damaged, replace it. 3 Remove the propping object from under the 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 L of oil. 5 Wait a few minutes for the oil to settle. If the oil level drops, add oil 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 bench next to or behind the MSD, or under the analyzer chamber at the back of the MSD. 8 Pump down the MSD. WARNING The foreline pump can cause burns if touched when operating. It has a safety shield to prevent the user from touching it. 4 General Maintenance To Change the Oil Mist Filter on the Foreline Pump 104 5977B Series MSD Troubleshooting and Maintenance Manual To Change the Oil Mist Filter on the Foreline Pump Materials needed • Oil mist filter (G1099-80039) • Gloves, oil-resistant Procedure 1 Unscrew the filter from the top of pump. 2 Screw the replacement filter on to the pump. WARNING The foreline pump can cause burns if touched when operating. It has a safety shield to protect the user from touching it. WARNING Do not breathe the pump exhaust; it may contain traces of pump oil vapor, solvents, and analytes. Do not replace the trap while samples are being analyzed. WARNING The oil mist filter may contain traces of oil, solvents, and analytes. Treat it as hazardous. Dispose of the oil trap in accordance with local environmental and safety regulations. 4 General Maintenance To Change the Oil Mist Filter on the Foreline Pump 5977B Series MSD Troubleshooting and Maintenance Manual 105 Figure 10. Foreline pump with oil mist filter Oil mist filter 4 General Maintenance To Install the Exhaust Filter on the IDP3 Dry Pump 106 5977B Series MSD Troubleshooting and Maintenance Manual To Install the Exhaust Filter on the IDP3 Dry Pump Materials needed • Exhaust filter (G7077-67017) Procedure 1 Disconnect the foreline pump exhaust hose from the adapter. 2 Unscrew the adapter from the pump. 3 Screw the filter on to the pump. WARNING Do not breathe the pump exhaust; it may contain traces of solvents and analytes. Do not install the exhaust filter while samples are being analyzed. 4 General Maintenance To Install the Exhaust Filter on the IDP3 Dry Pump 5977B Series MSD Troubleshooting and Maintenance Manual 107 Figure 11. IDP3 pump with exhaust filter Exhaust filter Exhaust hose Hose adapter 4 General Maintenance To Change the Filter Cartridge on the IDP3 Dry Foreline Pump 108 5977B Series MSD Troubleshooting and Maintenance Manual To Change the Filter Cartridge on the IDP3 Dry Foreline Pump Materials needed • Exhaust filter cartridge (REPLSLRFILTER2) • Gloves, oil-resistant Procedure 1 Unscrew the cap from the exhaust filter. (See Figure 11 on page 107.) 2 Pull the filter cartridge out of the filter cap. 3 Install a new filter cartridge. 4 Align the cap onto the filter and rotate the cap counterclockwise to lock in place. WARNING Do not breathe the pump exhaust; it may contain traces of solvents and analytes. Do not install the exhaust filter while samples are being analyzed. WARNING The exhaust filter cartridge may contain traces of solvents and analytes. Treat it as hazardous. Dispose of the filter cartridge in accordance with local environmental and safety regulations. 4 General Maintenance To Check the DP Fluid 5977B Series MSD Troubleshooting and Maintenance Manual 109 To Check the DP Fluid Materials needed • Screwdriver, Torx T-20 (8710-1615) Procedure 1 Remove the analyzer window cover. 2 Vent the MSD. 3 Remove the side cover. 4 Check the DP fluid level. (See Figure 12 on page 110.) The DP fluid level can be seen through the window below the fan at the front of the MSD. The DP fluid level should be between the top and bottom of one of the FULL ranges. There are two sets of marks. Use the HOT marks if the DP is on and is at its normal operating 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 DP fluid. Do not just add fluid. The pump fluid should be clear or almost clear. Dark or cloudy pump fluid indicates an air leak or excessive heat. If the pump fluid appears dark or cloudy, replace it. Then, check for an air leak. The DP fluid should be replaced at least once a year, or more often if the pump fluid level is low, or if the fluid is dark or cloudy. WARNING Do not remove any other covers. Removing other covers may expose hazardous voltages. WARNING Keep your hair away from the cooling fan if the MSD is turned on. WARNING The diffusion pump operates at a dangerously high temperature. Do not touch it. 4 General Maintenance To Check the DP Fluid 110 5977B Series MSD Troubleshooting and Maintenance Manual Figure 12. DP Fan Fluid level window (sight glass) 4 General Maintenance To Remove the DP 5977B Series MSD Troubleshooting and Maintenance Manual 111 To Remove the DP Materials needed • Aluminum foil, clean • Gloves, oil-resistant Procedure 1 Vent the MSD. 2 Separate the MSD from the GC. (See“To Separate the MSD from an 8890 or 7890 GC” on page 89.) 3 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.) 4 Disconnect the DP temperature sensor wires from the wiring harness. 5 Support the DP with one hand. WARNING Treat the DP fluid as hazardous, as it may contain traces of toxic chemicals. WARNING The diffusion pump operates at a dangerously high temperature. Make sure it has cooled before touching it. 4 General Maintenance To Remove the DP 112 5977B Series MSD Troubleshooting and Maintenance Manual 6 Remove the KF50 clamp. (See Figure 13.) 7 Lower the DP. 8 Remove the O-ring assembly from the top of the DP. The O-ring will have DP fluid on it, and will be very sticky. Place the O-ring on clean aluminum foil (shiny side down) to keep your lab bench and the O-ring clean. 9 Remove the DP through the side of the MSD. You may have to tilt the pump slightly to remove it. Do not tilt the pump past 45 degrees if the pump is warm. 10 Disconnect the foreline gauge assembly from the DP outlet. The foreline gauge cable can be disconnected or can remain connected to the foreline gauge. Figure 13. Removing the DP Foreline gauge assembly KF50 clamp DP 4 General Maintenance To Replace the DP Fluid 5977B Series MSD Troubleshooting and Maintenance Manual 113 To Replace the DP Fluid Materials needed • Aluminum foil, clean • Cloths, clean, lint-free (05980-60051) • Container for old DP fluid • DP fluid, 18.5 mL (6040-0809) – Two bottles are required • Gloves • Oil- and solvent-resistant • Thermally insulated Procedure 1 Remove the DP from the MSD. (See“To Remove the DP” on page 111.) Remove the O-ring assembly from the top of the DP. 2 Cover the top of the DP with aluminum foil (shiny side up). 3 Heat the DP at 60 °C for 15 minutes. (If the pump will fit, you can use the GC oven.) 4 Pour the old DP fluid out the top of the pump. Even after heating, the pump fluid pours very slowly. 5 Check the color of the pump fluid. If the DP has been heated with insufficient pump fluid (or with a large air leak in the MSD), the remaining pump fluid may be severely charred and blackened. Blackened pump fluid may also be baked onto the internal parts (stack) of the pump. If so, you may have to remove the DP stack and clean WARNING The pump and pump fluid will be hot. Wear protective gloves when you remove the pump from the oven. WARNING Treat the old pump fluid as hazardous. It may contain traces of toxic chemicals. WARNING Methylene chloride is a hazardous solvent. Work in a fume hood and take all appropriate precautions. 4 General Maintenance To Replace the DP Fluid 114 5977B Series MSD Troubleshooting and Maintenance Manual its parts, and the interior of the pump, with methylene chloride. Be very careful when reinstalling the stack. Misalignment of stack components can seriously reduce DP performance. 6 Clean the DP flange on the analyzer chamber. 7 Preheat the new DP fluid following the instructions on the bottle. 8 Pour new DP fluid into the DP until the fluid level is within the FULL COLD range. The recommended charge for this pump is 30 mL. It will require approximately 1.5 of the bottles (18.5 mL each) of DP fluid. Pour the fluid between the center stack and the side wall. Watch the sight glass while pouring. Do not overfill. 9 Reinstall the DP. (See “To Install the DP” on page 115.) Figure 14. Filling the DP with fluid Only use about half of the second bottle 4 General Maintenance To Install the DP 5977B Series MSD Troubleshooting and Maintenance Manual 115 To Install the DP Materials needed • Gloves, oil-resistant • Vacuum cleaner, non-ESD generating (92175V or equivalent) This procedure works best with two people, one to hold the pump, and one to install the clamp. Procedure 1 Vacuum the fan that cools the DP. Keeping the fan clean helps ensure maximum cooling. This is one of the few times you will have convenient access to the pump side of the fan. 2 Slide the DP into the MSD. You may have to tilt the pump slightly to get it into the MSD. Do not tilt it past 45 degrees. 3 Install the O-ring assembly on the DP. (See Figure 15 on page 116.) 4 Lift the DP into its normal position. 5 Install the KF50 clamp. 6 Reconnect the DP temperature sensor wires to the wiring harness. 7 Reconnect the high vacuum power cable to the HIVAC POWER connector on the back panel of the MSD. This is the thick black cable that emerges near the bottom of the pump. 8 Reconnect the foreline gauge fitting to the outlet of the DP. If you disconnected the foreline gauge cable, reconnect it to the foreline gauge. 9 Move the MSD back to its normal position. 4 General Maintenance To Install the DP 116 5977B Series MSD Troubleshooting and Maintenance Manual Figure 15. Installing the DP Foreline gauge assembly KF50 clamp O-ring assembly DP DP outlet 4 General Maintenance To Remove the Foreline Gauge 5977B Series MSD Troubleshooting and Maintenance Manual 117 To Remove the Foreline Gauge Materials needed • Screwdriver, flat-blade, large (8730-0002) Procedure 1 Vent the MSD. 2 Separate the MSD from the GC and disconnect the transfer line temperature sensor. (See“To Separate the MSD from an 8890 or 7890 GC” on page 89.) 3 Unplug the foreline gauge cable from the foreline gauge. 4 Disconnect the foreline gauge assembly from the DP outlet. 5 Loosen the hose clamp. 6 Pull the foreline gauge assembly out of the foreline hose. (See Figure 16 on page 118.) WARNING The foreline pump and DP may still be hot. CAUTION Ensure the MSD is vented to atmosphere before breaking the seal at the foreline gauge. Never vent the MSD at the pump end; use the vent valve. 4 General Maintenance To Remove the Foreline Gauge 118 5977B Series MSD Troubleshooting and Maintenance Manual Figure 16. Foreline gauge assembly Foreline gauge 4 General Maintenance To Install the Foreline Gauge 5977B Series MSD Troubleshooting and Maintenance Manual 119 To Install the Foreline Gauge Materials needed • Foreline gauge assembly (G1099-60545) • Screwdriver, flat-blade, large (8730-0002) Procedure 1 Connect a new foreline gauge assembly to the foreline hose. 2 Tighten the hose clamp. 3 Connect the foreline gauge assembly to the DP outlet. 4 Connect the foreline gauge cable to the foreline gauge. 5 Reconnect the MSD to the GC. (See “To Reconnect the MSD to an 8890 or 7890 GC” on page 93.) 6 If necessary, slide the foreline pump back under the analyzer chamber. The foreline pump may be located on the floor, on the lab bench next to or behind the MSD, or under the analyzer chamber at the back of the MSD. 7 Pump down the MSD. 4 General Maintenance To Refill the EI Calibration Vial 120 5977B Series MSD Troubleshooting and Maintenance Manual To Refill the EI Calibration Vial Materials needed • PFTBA (05971-60571) Procedure 1 Stop any tuning or data acquisition. 2 Turn off the analyzer. (See MassHunter software online help.) 3 If your MSD is equipped with a vacuum gauge, turn off the gauge. 4 Remove the analyzer window cover. 5 Loosen the calibration vial collar by turning it counterclockwise. (See Figure 17.) Do not remove the collar. 6 Pull the calibration vial out. You may feel some resistance due to O-ring friction and residual vacuum. 7 Syringe or pipette PFTBA into the vial. With the vial vertical, the liquid should be just below the end of the internal tube, approximately 70 µL. 8 Push the calibration vial into the valve as far as possible. 9 Withdraw the vial 1 mm. This prevents damage when you tighten the collar. Figure 17. Removing the EI calibration vial Calibration vial Collar 4 General Maintenance To Refill the EI Calibration Vial 5977B Series MSD Troubleshooting and Maintenance Manual 121 10 Turn the collar clockwise to tighten it. 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. 11 Reinstall the analyzer window cover. 12 Purge the EI calibration valve. (See“To Purge the Calibration Valves” on page 122.) CAUTION Failure to purge the calibration valve will result in damage to the filaments and detector. 4 General Maintenance To Purge the Calibration Valves 122 5977B Series MSD Troubleshooting and Maintenance Manual To Purge the Calibration Valves EI calibration valve After adding new PFTBA to the EI calibration vial, you must purge the air out of the vial and valve. 1 If the vacuum gauge controller is on, turn it off. 2 In Tune and Vacuum Control view, select Purge Calibrant Valve under the Vacuum menu. This will open the EI calibration valve for several minutes with all analyzer voltages turned off. CI calibration valve After adding new PFDTD to the CI calibration vial, you must purge the air out of the vial and valve. 1 If the vacuum gauge controller is on, turn it off. 2 Verify that PCICH4.U is loaded. 3 In Tune and Vacuum Control view, select Purge Calibrant Valve under the Vacuum menu. This will open the CI calibration valve for several minutes with all analyzer voltages turned off. CAUTION After removing a calibration vial, you must purge the calibration valve. Failure to do so will result in damage to the filaments and the electron multiplier. 4 General Maintenance To Remove the EI Calibration and Vent Valve Assembly 5977B Series MSD Troubleshooting and Maintenance Manual 123 To Remove the EI Calibration and Vent Valve Assembly Materials needed • Screwdriver, Torx T-20 (8710-1615) Procedure 1 Vent the MSD. 2 Trace the calibration valve cable to the connector next to the fan, and disconnect it. 3 Loosen the collar, and remove the calibration vial. (See Figure 17 on page 120.) Just loosen the collar, do not remove it. 4 Remove the two screws holding the valve assembly to the top of the analyzer chamber. Do not lose the O-ring under it. CAUTION Removing the valve with the vial installed can result in liquid calibrant getting into the restrictor of the valve. Liquid in the restrictor will prevent diffusion of PFTBA into the analyzer chamber for tuning. Replace the valve if this happens. 4 General Maintenance To Install the EI Calibration and Vent Valve Assembly 124 5977B Series MSD Troubleshooting and Maintenance Manual To Install the EI Calibration and Vent Valve Assembly Materials needed • Calibration valve • Diffusion (G7077-60211) • Turbo (G7077-60204) • O-ring for calibration valve (0905-1217) • PFTBA (05971-60571) or other tuning compound • Screwdriver, Torx T-20 (8710-1615) Procedure 1 Remove the old valve assembly. (See“To Remove the EI Calibration and Vent Valve Assembly” on page 123 and Figure 17 on page 120.) 2 Ensure the valve O-ring is in place. If it is worn or damaged, replace it. 3 Install the calibration and vent valve assembly, and tighten the screws that hold it in place. 4 Reconnect the calibration valve cable to the connector next to the fan. 5 Remove the vial from the new calibration valve. (See“To Refill the EI Calibration Vial” on page 120.) The valve is supplied with a vial already installed. 6 Fill and reinstall the calibration vial. 7 Pump down the MSD. 8 Purge the calibration valve. (See “To Purge the Calibration Valves” on page 122.) CAUTION Failure to purge the calibration valve will damage the filaments and detector. 4 General Maintenance To Replace the Fan for the High Vacuum Pump 5977B Series MSD Troubleshooting and Maintenance Manual 125 To Replace the Fan for the High Vacuum Pump Materials needed Fan (G7005-60564) Screwdriver, Torx T-20 (8710-1615) Procedure 1 Vent the MSD. 2 Remove the left side MSD cover. 3 Disconnect the fan wiring from the connector on the MSD frame. (See Figure 18 on page 126.) 4 Remove the four fan screws and the safety grill. Remove the fan. Keep the screws. 5 Install the new fan with the flow arrow on the side pointing toward the pump. The wires should be at the upper left, close to the connector. 6 Add the safety grill and the four screws. Tighten the screws firmly. 7 Connect the fan wiring to the fan connector on the MSD frame. 8 Reinstall the MSD covers. 9 Pump down the MSD. WARNING Do not touch the high vacuum pump. The pump could still be hot enough to burn you. WARNING Ensure the safety grill that shields the fan blades is in place. 4 General Maintenance To Replace the Fan for the High Vacuum Pump 126 5977B Series MSD Troubleshooting and Maintenance Manual Figure 18. Replacing the pump fan (DP shown) Fan wiring Fan wiring connector 4 General Maintenance To Remove the Ion Vacuum Gauge 5977B Series MSD Troubleshooting and Maintenance Manual 127 To Remove the Ion Vacuum Gauge Procedure 1 Vent the MSD. 2 Disconnect the cable on the back of the ion vacuum gauge. 3 Unscrew the red plastic thumbnut on the gauge clamp. 4 Remove the long screw from the clamp. 5 While supporting the gauge body, remove the clamp from the mounting flange. 6 Remove the gauge. 7 If you will not be replacing the gauge soon, install the blanking plate provided with the gauge and secure it with the clamp, screw, and thumbnut. To Install an Ion Vacuum Gauge Material needed • KF16 O-ring (0905-1463) Procedure 1 Place the KF16 O-ring in the groove on the analyzer chamber flange. Replace it if it is worn or damaged. 2 Hold the gauge flange against the chamber flange with the O-ring. Push the clamp over both flanges. 3 Insert the long screw, add the thumbnut, and tighten. 4 Attach the communication cable to the back of the gauge and connect the other end to the back of the MS. 4 General Maintenance To Lubricate the Side Plate O-Ring 128 5977B Series MSD Troubleshooting and Maintenance Manual To Lubricate the Side Plate O-Ring Materials needed • Cloths, clean (05980-60051) • Gloves, clean, lint-free • Large (8650-0030) • Small (8650-0029) • Grease, Apiezon L, high vacuum (6040-0289) The side plate O-ring needs a thin coat of grease to ensure a good vacuum seal. If the side plate O-ring appears dry or does not seal correctly, lubricate it using this procedure. A good test is to wipe off the side plate with methanol, then close the analyzer chamber. If the O-ring has enough grease on it, it will leave a faint trace on the side plate. Procedure 1 Vent the MSD. 2 Open the analyzer chamber. (See “To Open the Analyzer Chamber” in the 5977B Series MSD Operating Manual.) 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. (See Figure 19 on page 129.) CAUTION 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. WARNING The analyzer, GC/MSD interface, and other components in the analyzer chamber operate at very high temperatures. Do not touch any part until you are sure it is cool. CAUTION Always wear clean gloves to prevent contamination when working in the analyzer chamber. CAUTION Make sure you use an antistatic wrist strap, and take other antistatic precautions before touching analyzer components. 4 General Maintenance To Lubricate the Side Plate O-Ring 5977B Series MSD Troubleshooting and Maintenance Manual 129 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 analyzer chamber. 6 Pump down the MSD. CAUTION Do not use anything except the recommended vacuum grease. Excess grease can trap air and dirt. Grease on the surface of the O-ring other than the exposed surface can trap air, resulting in air spikes during operation. Figure 19. Side plate O-ring Side plate O-ring 4 General Maintenance To Lubricate the Vent Valve O-Ring 130 5977B Series MSD Troubleshooting and Maintenance Manual To Lubricate the Vent Valve O-Ring Materials needed • Cloths, clean (05980-60051) • Gloves, clean, lint-free • Large (8650-0030) • Small (8650-0029) • Grease, Apiezon L, high vacuum (6040-0289) • O-ring, vent valve (0905-1217). Replace if the old O-ring is worn or damaged The vent valve O-ring needs a thin coat of lubrication to ensure a good vacuum seal and smooth operation. If the vent valve O-ring does not turn smoothly or does not seal correctly, lubricate it using this procedure. Procedure 1 Vent the MSD. 2 Completely remove the vent valve knob. (See Figure 20 on page 131.) 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 CAUTION 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 function. CAUTION Excess grease can trap air and dirt. Grease on surfaces of the O-ring other than the exposed surface can trap air, resulting in air spikes during operation. 4 General Maintenance To Lubricate the Vent Valve O-Ring 5977B Series MSD Troubleshooting and Maintenance Manual 131 6 Reinstall the vent valve knob. 7 Pump down the MSD. Figure 20. Vent valve O-ring Vent valve knob CAUTION Be very careful when reinstalling the vent valve knob. It is possible to cross thread the knob and damage the threads in the valve body. Ensure the O-ring stays in place. 4 General Maintenance Maintaining the Electronics 132 5977B Series MSD Troubleshooting and Maintenance Manual Maintaining the Electronics Scheduled maintenance None of the electronic components of the MSD need to be replaced on a regular schedule. None of the electronic components in the MSD need to be adjusted or calibrated on a regular schedule. Avoid unnecessary handling of the MSD electronics. Electronic components Very few of the electronic components are operator serviceable. The primary fuses can be replaced by the operator. The RF coils can be adjusted by the operator. All other maintenance of the electronics should be performed by your Agilent Technologies service representative. Electrostatic precautions 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 ESD to sensitive components on the side board. ESD damage may not cause immediate failure, but it will gradually degrade the performance and stability of your MSD. When you work on or near 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 precautions. The wrist strap should be connected to a known good earth ground. WARNING Improper use of these procedures could create a serious safety hazard. Improper use of these procedures could also result in serious damage to, or incorrect operation of, the MSD. WARNING Vent the MSD and disconnect its power cord before performing any of these procedures except adjusting the RF coils. 4 General Maintenance Maintaining the Electronics 5977B Series MSD Troubleshooting and Maintenance Manual 133 If that is not possible, it should be connected to a conductive (metal) part of the assembly being worked on, but not to electronic components, exposed wires or traces, or pins on connectors. Take extra precautions, such as a grounded antistatic mat, if you must work on components or assemblies that have been removed from the MSD. This includes the analyzer. More information is available More information about the functions of electronic components section is found later in this manual. (See Chapter 8, “Electronics,” starting on page 201.) Most of the procedures in this chapter are illustrated with video clips. CAUTION To be effective, an antistatic wrist strap must fit snugly (not tight). A loose strap provides little or no protection. CAUTION Antistatic precautions are not 100% effective. Handle electronic circuit boards as little as possible and then only by the edges. Never touch the components, exposed traces, or pins on connectors and cables. 4 General Maintenance To Adjust the Quad Frequency 134 5977B Series MSD Troubleshooting and Maintenance Manual To Adjust the Quad Frequency Materials needed • Screwdriver, flat-blade, large (8730-0002) Procedure 1 Ensure the MSD is at thermal equilibrium. It takes at least 2 hours after all heated zones have reached their setpoints for the MSD to reach thermal equilibrium. 2 Open the analyzer cover. 3 Ensure the RF cover on the side board is secure and no screws are missing. A loose RF cover or missing screw can significantly affect coil adjustment. 4 In the Tune and Vacuum Control view, select Optimize Quadrupole Frequency from the Execute menu. 5 Enter an m/z value of 100. 6 Slowly turn the quad frequency adjustment screws to minimize the voltage displayed. (See Figure 21 on page 135.) Turn the adjustment screws alternately. Turn each screw only a little bit at a time. Keep the screws at equal extension. 7 When the voltage is minimized, click Stop. WARNING Do not remove any other covers. Dangerous voltages are present under these covers. CAUTION Do not use a coin to adjust the screws. If you drop it, it could fall into the electronics fan and cause significant damage. 4 General Maintenance To Adjust the Quad Frequency 5977B Series MSD Troubleshooting and Maintenance Manual 135 8 Repeat steps 4 through 7 for m/z 650. 9 Exit the Optimize Quadrupole Frequency program. 10 Select MS OFF from the Execute menu. 11 Close the analyzer cover. 12 Tune the MSD. Figure 21. Adjusting the quad frequency RF cover Quad frequency adjustment screws 4 General Maintenance To Replace the Primary Fuses 136 5977B Series MSD Troubleshooting and Maintenance Manual To Replace the Primary Fuses Materials needed • Fuse, T12.5A, 250 V (2110-1398) – two required • Screwdriver, flat-blade (8730-0002) The most likely cause of failure of the primary fuses is a problem with the foreline pump. If the primary fuses in your MSD fail, check the foreline pump. Procedure 1 Vent the MSD, and unplug the power cord from the electrical outlet. If one of the primary fuses has failed, the MSD will already be off, but for safety you should switch off the MSD, and unplug the power cord. It is not necessary to allow air into the analyzer chamber. 2 Turn one of the fuse holders counterclockwise until it pops out. (See Figure 22 on page 137.) The fuse holders are spring loaded. 3 Remove the old fuse from the fuse holder. 4 Install a new fuse in the fuse holder. 5 Reinstall the fuse holder. WARNING Never replace the primary fuses while the MSD is connected to a power source. WARNING If you are using hydrogen as a GC carrier gas, a power failure may allow it to accumulate in the analyzer chamber. In that case, further precautions are required. (See“Hydrogen Safety” on page 22.) 4 General Maintenance To Replace the Primary Fuses 5977B Series MSD Troubleshooting and Maintenance Manual 137 6 Repeat steps 2 through 5 for the other fuse. Always replace both fuses. 7 Reconnect the MSD power cord to the electrical outlet. 8 Pump down the MSD. Figure 22. Primary fuses (turbo model shown) Primary fuses in holders 4 General Maintenance To Replace the Primary Fuses 138 5977B Series MSD Troubleshooting and Maintenance Manual 5977B Series MSD Troubleshooting and Maintenance Manual 139 5 CI Maintenance To Replace the Methane/Isobutane Gas Purifier 140 To Clean the Reagent Gas Supply Lines 141 To Refill the CI Calibration Vial 142 This chapter describes maintenance procedures and requirements that are unique to 5977B Series MSDs equipped with the Chemical Ionization hardware. 5 CI Maintenance To Replace the Methane/Isobutane Gas Purifier 140 5977B Series MSD Troubleshooting and Maintenance Manual To Replace the Methane/Isobutane Gas Purifier Materials needed • Methane/Isobutane gas purifier (G1999-80410) • Front ferrule for 1/8-inch tubing (5180-4110) • Rear ferrule for 1/8-inch tubing (5180-4116) • Tubing cutter (8710-1709) The methane/isobutane gas purifier needs to be replaced after four tanks of reagent gas. This frequency may vary depending on purity of the gas and care taken in uncapping and installing the gas purifier. A large leak upstream from the gas purifier can quickly exhaust the reduced 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 fittings on the old filter. 3 Remove the ferrules from the tubing at the outlet of the gas purifier. Using the tubing cutter, cut off the end of the tubing with the ferrules. 4 Install the new filter. 5 Purge the new filter. 6 Cap the old filter and prepare it to be sent for regeneration. See the instructions on the label. CAUTION Do not remove the caps until you are ready to install the gas purifier. Only remove the caps in the gas flow to prevent contamination by air. WARNING Methane is flammable. Extinguish all flames in the area before turning on gas flow. 5 CI Maintenance To Clean the Reagent Gas Supply Lines 5977B Series MSD Troubleshooting and Maintenance Manual 141 To Clean the Reagent Gas Supply Lines Materials needed • Clean, dry nitrogen • Heat gun • Tubing cutter (8710-1709) Procedure If the reagent gas lines become contaminated, they can be cleaned. 1 Disconnect the reagent gas tubing from the gas supply, the gas purifier, and the MSD. 2 Cap the gas purifier following the instructions on the label. 3 Connect one end of the tubing to a supply of clean, dry nitrogen and turn on the gas flow. 4 Use the heat gun to warm the tubing, starting at the supply end and working your way to the free end. 5 Repeat for any other pieces of tubing that need to be cleaned. 6 Reconnect the tubing to the gas supply, gas purifier, and MSD. Follow the instructions on the gas purifier label. WARNING Do not heat the gas tubing when reagent gas is flowing. CAUTION Do not put liquids into the tubing. Do not heat the tubing when it is connected to the MSD. 5 CI Maintenance To Refill the CI Calibration Vial 142 5977B Series MSD Troubleshooting and Maintenance Manual To Refill the CI Calibration Vial Materials needed • PFDTD calibrant (8500-8510) Procedure 1 Set the reagent gas flow to Gas Off. 2 Vent the MSD. 3 Remove the capillary column from the GC/MSD interface. 4 Pull the MSD away from the GC to expose the calibration vial and valve. See“To Separate the MSD from an 8890 or 7890 GC” on page 89. 5 Loosen the calibration vial collar by turning it counterclockwise. Do not remove the collar. 6 Remove the calibration vial. See Figure 23 on page 143. 7 Fill the vial no higher than the bottom of the internal tube with fresh PFDTD calibrant (8500-8510). 8 Replace the vial and tighten the collar. 9 Reposition the MSD next to the GC. See “To Reconnect the MSD to an 8890 or 7890 GC” on page 93. 10 Reinstall the capillary column. 11 Pump down the MSD. 12 Purge the calibration valve. See“To Purge the Calibration Valves” on page 122. CAUTION Do not rinse the vial with any solvents. Never expose the inside of the vial to chlorinated solvents or isopropyl alcohol or water — this will result in severe loss of CI sensitivity. CAUTION After 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. 5 CI Maintenance To Refill the CI Calibration Vial 5977B Series MSD Troubleshooting and Maintenance Manual 143 Figure 23. CI calibration valve and vial Calibration valve Calibration vial Collar 5 CI Maintenance To Refill the CI Calibration Vial 144 5977B Series MSD Troubleshooting and Maintenance Manual 5977B Series MSD Troubleshooting and Maintenance Manual 145 6 Vacuum System Overview 146 Vacuum System Components 147 Common Vacuum System Problems 148 Foreline Pump 149 High Vacuum Pump 152 Analyzer Chamber 153 Side Plate 154 Vacuum Seals 157 Face seals 157 KF (NW) seals 157 Compression seals 158 High voltage feedthrough seal 158 Foreline Gauge 159 Diffusion Pump and Fan 160 Turbo Pump and Fan 166 Calibration Valves and Vent Valve 167 Micro-Ion Vacuum Gauge 170 This chapter describes components of the MSD vacuum system. 6 Vacuum System Overview 146 5977B Series MSD Troubleshooting and Maintenance Manual Overview The vacuum system creates the high vacuum (low pressure) required for the MSD to operate. Without the vacuum, the molecular mean free path would be very short and ions would collide with air molecules before they could reach the detector. Operation at high pressures also would damage analyzer components. The 5977B Series MSDs use two vacuum pumps to obtain the vacuum levels needed. One of two foreline pumps (standard or dry) creates a low vacuum, then a high vacuum pump engages to create the vacuum needed for operation. The 5977B Series MSD uses one of two kinds of high vacuum pumps: a diffusion pump or a turbomolecular pump. The pump type determines the maximum column flow supported by the MSD. The 5977B HES Series MSD model G7079B uses a turbomolecular (turbo) pump for high vacuum. It has a maximum column flow rate of 4.0 mL/min. Most vacuum system operation is automated. Operator interaction is through the data system or control panel. Monitor the vacuum system through the data system or GC control panel. Table 10 Recommended maximum flow rates by model Model number Description Maximum recommended column flow G7080B Diffusion pump, EI 1.5 mL/min G7077B Turbo pump, EI 4.0 mL/min G7078B Turbo pump, EI 4.0 mL/min G7081B Turbo pump, EI 4.0 mL/min G7079B Turbo pump, EI HES 4.0 mL/min 6 Vacuum System Vacuum System Components 5977B Series MSD Troubleshooting and Maintenance Manual 147 Vacuum System Components The parts of the vacuum system are identified in Figure 24. • Foreline (rough) pump • High vacuum pump (diffusion or turbo pump) • Analyzer chamber • Side plate (analyzer door), and front and rear end plates • Vacuum seals • Calibration valve(s) and vent valve • Vacuum control electronics • Vacuum gauges and gauge control electronics Each of these is discussed in more detail in this chapter. Figure 24. Vacuum system components (MSD with turbo pump shown) High vacuum High vacuum Analyzer GC/MSD Ion vacuum gauge (if present) CI flow control Vent valve cooling fan pump pump interface chamber (not shown) 6 Vacuum System Common Vacuum System Problems 148 5977B Series MSD Troubleshooting and Maintenance Manual Common Vacuum System Problems Air leak symptoms The most common problems associated with any vacuum system are air leaks. Symptoms of air leaks include: • Loud gurgling noise from the foreline pump (very large leak) • Inability of the turbo pump to reach 95% speed • High foreline pressure in diffusion pump MSDs • Higher than normal high vacuum gauge controller readings The 5977B Series MSD will not pump down successfully unless you press on the side plate (analyzer door) when you turn on the MSD power. Continue to press until the sound from the foreline pump becomes quieter. Pumpdown failure shutdown The system will shut down both the high vacuum and the foreline pump if the system fails to pump down correctly. Two conditions that trigger shutdown are: • Diffusion pump MSDs, shutdown occurs if the foreline pressure is above 300 mTorr after 7 minutes. • Turbo pump MSDs speed below 80% after 7 minutes. This is usually because of a large air leak: either the side plate has 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. To restart the MSD, find and correct the air leak, then switch the power off and on. Press on the side plate when turning on the MSD power to ensure a good seal. 6 Vacuum System Foreline Pump 5977B Series MSD Troubleshooting and Maintenance Manual 149 Foreline Pump The foreline pump reduces the pressure in the analyzer chamber so the high vacuum pump can operate. It also pumps away the gas load from the high vacuum pump. The foreline pump is connected to the high vacuum pump by a 130-cm hose called the foreline hose. There are four different types of foreline pumps, the Pfeiffer DUO (Figure 25), the MVP-070-3 (Figure 26 on page 150), the MVP-070-3C (not shown), and the IDP3 (Figure 27 on page 150). The dry foreline pumps are not supported with diffusion pump base MSDs. Figure 25. Pfeiffer Duo foreline pump Hose to vacuum pump Ballast control Fill cap Exhaust outlet Power switch Oil level window with oil mist filter Drain plug (on front) 6 Vacuum System Foreline Pump 150 5977B Series MSD Troubleshooting and Maintenance Manual Figure 26. MVP-070-3 dry foreline pump Exhaust outlet Power switch Hose to vacuum pump Figure 27. IDP3 dry foreline pump Power cord Exhaust filter CAUTION Agilent does not recommend using hydrogen as a carrier gas on systems equipped with an IDP3 dry foreline pump. 6 Vacuum System Foreline Pump 5977B Series MSD Troubleshooting and Maintenance Manual 151 The standard foreline pump is a two-stage rotary-vane pump. An optional dry pump is also available. The pump turns on when the MSD power is turned on. The foreline pump has a built-in antisuckback valve to help prevent backstreaming in the event of a power failure. The foreline pump can be placed under the analyzer chamber at the rear of the MSD (with the exhaust outlet to the rear) or on the floor below the MSD. An oil mist filter is available for the standard pump that can be used to filter pump oil out of the foreline pump exhaust. This filter stops only pump oil. Do not use the filter if you are analyzing toxic chemicals or using toxic solvents or if you have a CI MSD. Instead, install an 11-mm id hose to remove the exhaust from your lab. A window (sight glass) in the front of the standard 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 lower mark, add foreline pump oil. The oil pan under the foreline pump can be a fire hazard (standard pump) Oily rags, paper towels, and similar absorbents in the oil pan could ignite and damage the pump and other parts of the MSD. WARNING The oil mist filter supplied with the standard foreline pump 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 filter if you have a CI MSD. Install a hose to take the foreline pump exhaust outside or to a fume hood. CAUTION Do not place the foreline pump near any equipment that is sensitive to vibration. CAUTION The ballast control knob controls the amount of air allowed into the pump. Keep the ballast control closed (fully clockwise) at all times, except when ballasting the pump. WARNING Combustible materials (or flammable/nonflammable wicking material) placed 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. 6 Vacuum System High Vacuum Pump 152 5977B Series MSD Troubleshooting and Maintenance Manual High Vacuum Pump Diffusion pump system The diffusion pump supports a maximum flow rate of 1.5 mL/min into the MSD. The diffusion pump uses baffling to prevent vapor from migrating into the analyzer chamber. Foreline pressure is monitored by the foreline gauge. The AC board controls the diffusion pump heater. Turbo pump system The 5977B Series MSD supports a turbo pump. The turbo pump has a screen 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. 6 Vacuum System Analyzer Chamber 5977B Series MSD Troubleshooting and Maintenance Manual 153 Analyzer Chamber The analyzer chamber (Figure 28) is where the analyzer operates. The manifold is extruded and machined from an aluminum alloy. Large openings in the side, front, and rear of the analyzer chamber are closed by plates. O-rings provide the seals between the plates and the manifold. Ports in the manifold and the plates provide attachment points for the Micro-Ion vacuum gauge, calibration valve, vent valve, GC/MSD interface, and high vacuum pump. Diffusion pump version 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 baffle cool so the vapor will condense on it. Turbo pump version The turbo pump and the mounting bracket for the turbo controller are clamped directly to the manifold. Figure 28. Analyzer chamber Vacuum gauge baffle GC/MSD interface To high vacuum pump Calibration and vent valves Analyzer window Side plate O-ring 6 Vacuum System Side Plate 154 5977B Series MSD Troubleshooting and Maintenance Manual Side Plate The side plate for the HES version (See Figure 29 on page 155) or the non-HES version (See Figure 30 on page 156) covers the large opening in the side of the analyzer chamber. It is attached to the manifold with a hinge. The analyzer assembly is attached to the side plate inside the analyzer chamber. The hinge allows the side plate to swing away from the manifold for easy access to the analyzer. Several electrical feedthroughs are built into the side plate. Wires connect the feedthroughs 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. CAUTION Fasten both side plate thumbscrews for shipping or storage only. For normal operation, both thumbscrews should be loose. For operation with hydrogen carrier gas, or with flammable or explosive CI reagent gases, the front thumbscrew should be fastened just finger-tight. Overtightening will warp the side plate and cause air leaks. Do not use a tool to tighten the side plate thumbscrews. CAUTION When you turn on the power to pump down the MSD, press on the side board to ensure a good seal. 6 Vacuum System Side Plate 5977B Series MSD Troubleshooting and Maintenance Manual 155 Figure 29. Side plate feedthroughs (HES version) High voltage (HED) Detector focus Ion source and heater Mass Filter (quadrupole) Signal (detector output) EM voltage PE1, PE2, and Ext feedthroughs 6 Vacuum System Side Plate 156 5977B Series MSD Troubleshooting and Maintenance Manual Figure 30. Side plate feedthroughs (non-HES version) High voltage (HED) Detector focus Ion source and heater Mass filter (quadrupole) Screws for radiator mounting brackets Signal (detector output) EM voltage (2 of 4) 6 Vacuum System Vacuum Seals 5977B Series MSD Troubleshooting and Maintenance Manual 157 Vacuum Seals Vacuum seals are shown in Figure 31 on page 158. Several types of Viton elastomer O-ring seals are used to prevent air leaks into the analyzer chamber. All these O-rings, and the surfaces to which they seal, must be kept clean and protected from nicks and scratches. A single hair, piece of lint, or scratch can produce a serious vacuum leak. Two of the O-rings, the side plate O-ring and the vent valve O-ring, are lightly lubricated with Apiezon-L vacuum grease. Face seals A face seal is an O-ring that fits in a shallow groove. The sealing surface is usually a flat plate. The manifold side plate and end plate O-rings fit into grooves around the large openings in the analyzer chamber. The side plate swings into place against the side plate O-ring, and must be held in place when the MSD is turned on for pump down 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/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 to the manifold with four claw grips. KF (NW) seals Most of the seals for the high vacuum pumps, foreline gauge, and foreline pump are KF seals. KF seals have an O-ring supported by a centering ring. The centering ring can be either on the inside or outside of the O-ring. The clamp presses two flanges against the O-ring, making a seal. KF clamps must not be overtightened. 6 Vacuum System Vacuum Seals 158 5977B Series MSD Troubleshooting and Maintenance Manual Compression seals A compression fitting consists of a threaded fitting on the analyzer chamber and a threaded collar with a ferrule and O-ring. A cylindrical part fits inside the collar. Tightening the collar presses the ferrule, compressing the O-ring around the part. The calibration vials use compression seals. High voltage feedthrough seal The high voltage (HED) feedthrough seal is an O-ring that is compressed against the side plate by a threaded collar. Figure 31. Vacuum seals Side plate O-ring seal KF seal with internal centering ring KF seal with external centering ring Compression seal (clamp not shown) (clamp not shown) 6 Vacuum System Foreline Gauge 5977B Series MSD Troubleshooting and Maintenance Manual 159 Foreline Gauge The foreline gauge monitors the pressure (vacuum) at the exit of the diffusion pump. The primary function of the foreline gauge is diffusion pump control. When the foreline pump has reduced the pressure in the analyzer chamber to below 300 mTorr (0.3 Torr), the diffusion pump is automatically switched on. If the foreline pressure rises above 400 mTorr (0.4 Torr), the AC board switches off the diffusion pump heater and the analyzer electronics. Monitor the foreline pressure from the data system or the LCP. The foreline gauge is used only with diffusion pump MSDs. 6 Vacuum System Diffusion Pump and Fan 160 5977B Series MSD Troubleshooting and Maintenance Manual Diffusion Pump and Fan The diffusion pump in the MSD is an air-cooled vapor diffusion pump with 90 L/s capacity. It mounts with a KF50 fitting to a baffle adapter clamped to the bottom of the analyzer chamber. The diffusion pump has a cylindrical body surrounded by fins to help dissipate heat. Its inlet is open to the interior of the analyzer chamber, through the adapter and baffle. A structure called the stack is located at the center of the pump body. An electric heater is located at the bottom of the stack. See Figure 32 on page 160 and Figure 33 on page 161 . Figure 32. Diffusion pump with fan 6 Vacuum System Diffusion Pump and Fan 5977B Series MSD Troubleshooting and Maintenance Manual 161 The diffusion pump transports gas by momentum transfer. The heater boils a special fluid (a polyphenyl ether) inside the stack. As the vapor pressure increases, the pump fluid vapor is forced out and downward through nozzles in the stack. The vapor forced out of these nozzles strikes the gas molecules that are present. This forces the gas 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. Figure 33. Diffusion pump parts 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 6 Vacuum System Diffusion Pump and Fan 162 5977B Series MSD Troubleshooting and Maintenance Manual A cooling fan is located between the diffusion pump and 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, and would diffuse into the analyzer chamber. The foreline pump is connected by the foreline hose to the outlet of the diffusion pump. It removes the gas molecules that reach the outlet. The diffusion pump operation is controlled by the AC board. The AC board automatically turns on the diffusion pump heater as soon as the foreline pump lowers the pressure in the analyzer chamber below approximately 300 mTorr (0.3 Torr). Until the foreline pressure drops below 300 mTorr, the diffusion pump heater will not turn on. If the pressure does not drop below 300 mTorr within 7 minutes of turning the MSD on, the foreline pump will shut off. During operation, if the foreline pressure rises above 400 mTorr, the diffusion pump heater will turn off. The AC board allows the analyzer electronics to turn on when the diffusion pump is hot. The diffusion pump typically maintains an indicated pressure below 1.0 × 10-4 Torr for GC helium carrier gas flows up to 2 mL/min. High vacuum (manifold) pressure can only be measured if your MSD is equipped with the optional gauge controller. The small size of the diffusion pump allows it to heat up and cool down quickly. This simplifies pumpdown and venting. From initial power-on, the system can pump down to operating pressure in approximately 15 minutes. If the power fails, the diffusion pump fluid stops boiling before the analyzer chamber pressure begins to rise significantly. This helps prevent back diffusion of pump fluid into the analyzer chamber. Your data system has pumpdown and venting programs to guide you through these procedures. Follow the instruction carefully. Two thermal switches monitor diffusion pump operational readiness. See Table 11. Table 11 Diffusion pump thermal switches Thermal switch Too cold Too hot Normal state Normally open Normally closed Changes at 170 °C rising; 140 °C falling 365 °C rising Function Keeps analyzer turned off until the pump is hot enough to for adequate vacuum. Prevents analyzer damage Shuts off diffusion pump and analyzer if the pump overheats. Prevents damage to the pump and analyzer. 6 Vacuum System Diffusion Pump and Fan 5977B Series MSD Troubleshooting and Maintenance Manual 163 Check the condition and level of the diffusion pump fluid through the window (sight glass) near the base of the front of the pump. See Figure 34 on page 164. If the level drops below the appropriate marker (there are separate ranges for hot and cold conditions) or if the fluid turns dark brown or black, replace the fluid. Otherwise, replace the fluid once a year. Message The high vacuum pump is not ready Difficulty with the high vacuum pump What it means Normal during pumpdown Always indicates a problem What to do Wait for pump to heat up Check the level and conditions of the fluid. Make sure pump is cool, and power-cycle MSD to reset. Table 11 Diffusion pump thermal switches (continued) 6 Vacuum System Diffusion Pump and Fan 164 5977B Series MSD Troubleshooting and Maintenance Manual Figure 34. The diffusion pump Inlet Cooling fins Too cold sensor Too hot sensor Diffusion pump outlet Cold fluid level marker Diffusion pump heater cable Hot fluid level marker Fluid level window 6 Vacuum System Diffusion Pump and Fan 5977B Series MSD Troubleshooting and Maintenance Manual 165 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 Vacuum System” on page 88. • The troubleshooting sections of the MSD Data Acquisition online help. 6 Vacuum System Turbo Pump and Fan 166 5977B Series MSD Troubleshooting and Maintenance Manual Turbo Pump and Fan The turbo pump is clamped directly to the bottom of the analyzer chamber. The turbo pump has a cylindrical body with its inlet open to the interior of the analyzer chamber. Inside the pump body is a central shaft or cylinder. Sets of small blades (airfoils) radiate from the central shaft. The shaft spins at up to 60,000 revolutions per minute (rpm) in the turbo pump. Turbo pumps move gas by momentum transfer. The turbine blades are angled so that when they strike a gas molecule it is deflected downward. Each set of blades pushes the gas molecules further down toward the pump outlet. The foreline pump is connected by a hose to the outlet of the turbo pump. It removes the gas molecules that reach the outlet. 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 MSD. The fan draws air from outside the MSD and blows it over the pump. The turbo pump automatically turns on when the MSD power is switched on. The system allows the analyzer to be turned on when the turbo pump is greater than 80% speed, but the pump normally operates at 100% speed. Turbo pump MSDs typically maintain an indicated pressure below 8 × 10-5 Torr for helium column flows up to 4 mL/minute for the performance turbo pump, and up to 2 mL/minute for the standard turbo pump. Pressure (vacuum) can only be measured if your MSD is equipped with the optional gauge controller. The turbo pump spins up (starts) and spins down (stops) quickly. This simplifies pumpdown and venting. From initial power-on, the system can pump down to operating pressure in 5 to 10 minutes. See Also • “To pump down the MSD in the Operating Manual” in the Agilent 5977B Series MSD Operating Manual • “To vent the MSD” in the Agilent 5977B Series MSD Operating Manual • “Turbo pump control” on page 207 6 Vacuum System Calibration Valves and Vent Valve 5977B Series MSD Troubleshooting and Maintenance Manual 167 Calibration Valves and Vent Valve Calibration valves A calibration valve (See Figure 35 on page 168) is an electromechanical valve with a vial to hold the tuning compound. When a calibration valve is opened, tuning compound in the vial diffuses into the ion source. EI MSDs have one calibration valve; CI MSDs have a second calibration valve for the CI tuning compound. The valves are controlled by the MSD Data Acquisition software. EI calibration valve The EI calibration valve is held onto the top of the analyzer chamber by two screws. A small O-ring provides a face seal. The diffusion pump has a calibration valve with less restriction than that in the turbo MSD; this allows the correct diffusion of calibrant for each vacuum system. Perfluorotributylamine (PFTBA) is the most commonly used tuning compound for EI operation. PFTBA is required for automatic tuning of the MSD. Other compounds can be used for manual tuning. 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 reagent gas flow control module. It is controlled by the Data Acquisition software. It opens automatically during CI autotune or manual tuning, allowing PFDTD to diffuse through the GC/MSD interface and into the ion source. Vent valve The vent valve knob (See Figure 36 on page 169) screws into a threaded port in the front of the calibration valve. An O-ring is compressed between the knob and the valve to form a seal. The threaded end of the knob has an air passage inside it, allowing air to flow into the manifold when the knob is partially unscrewed. If you turn the knob too far, the O-ring can come out of its slot. 6 Vacuum System Calibration Valves and Vent Valve 168 5977B Series MSD Troubleshooting and Maintenance Manual Figure 35. Calibration valves EI calibration valve EI calibration vial Vent valve knob CI calibration valve CI calibration vial EI calibration above analyzer window CI calibration right side of MSD 6 Vacuum System Calibration Valves and Vent Valve 5977B Series MSD Troubleshooting and Maintenance Manual 169 Figure 36. Vent valve Vent valve knob O-ring Air passage Valve closed Valve open Valve open too far 6 Vacuum System Micro-Ion Vacuum Gauge 170 5977B Series MSD Troubleshooting and Maintenance Manual Micro-Ion Vacuum Gauge The G3397B Micro-Ion vacuum gauge is standard on CI MSDs and optional on EI MSDs. It consists of the sensing element (an ionization-type gauge) and the necessary electronics to support it. Both parts are mounted in a single package. The ionization gauge creates a current when energized electrons collide with gas molecules. The electronics provide the voltages required, measure the current produced, and produce an output signal that is used by the MSD software. The Micro-Ion vacuum gauge mounts on the end of the analyzer chamber and is open to it. This allows you to monitor chamber pressure in daily operation and in troubleshooting. The gauge is calibrated for nitrogen (N2). The carrier gas is usually helium, which does not ionize as readily as nitrogen. Therefore, the indicated pressure for helium is approximately six times lower than the absolute pressure. For example, a reading of 2.0 × 10-5 Torr versus an absolute pressure of 1.2 × 10-4 Torr. In a CI MSD, the indicated pressure reflects the contribution of both the carrier gas and the reagent gas. The distinction between indicated and absolute pressure is not important for normal operation of the MSD. Of greater concern are changes in pressure from hour to hour or day to day. These changes can indicate air leaks or other problems with the vacuum system. All the pressures listed in this manual are indicated pressures for helium carrier gas. The gauge controller setpoints are also indicated pressures. 5977B Series MSD Troubleshooting and Maintenance Manual 171 7 Analyzer Overview 172 EI Ion Source 175 HES EI Ion Source 182 CI Ion Source 185 Filaments 188 Other Source Elements 190 Magnet 190 Repeller 190 Drawout plate and cylinder 190 Ion focus 191 Entrance lens 191 Quadrupole Mass Filter 192 AMU gain 193 AMU offset 193 219 width 193 DC polarity 194 Mass (axis) gain 194 Mass (axis) offset 194 Quadrupole maintenance 194 Detector 195 Detector ion focus 195 High energy dynode 195 EM horn 195 Analyzer Heaters and Radiators 197 7 Analyzer Overview 172 5977B Series MSD Troubleshooting and Maintenance Manual Overview The analyzer with an XTR source (See Figure 38 on page 174) or the analyzer with a HES (See Figure 43 on page 183) is the heart of the MSD. It ionizes the sample, filters the ions, and detects them. The sample components exiting the GC column flow into the ion source. In the ion source, the sample molecules are ionized and fragmented. The resulting ions are repelled from the ion source into the quadrupole mass filter. The mass filter allows selected ions to pass through 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 for easy access. 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 the analyzer is discussed in the following material. The analyzer has four basic components The analyzer consists of the following components (See Figure 38 on page 174) or (See Figure 37 on page 173): • Ion source • Mass filter • Detector • Heaters and radiators 7 Analyzer Overview 5977B Series MSD Troubleshooting and Maintenance Manual 173 Figure 37. The analyzer with an HES Feedthrough board Mass filter heater assembly Detector Ion source (inside radiator) Mass filter (inside radiator) 7 Analyzer Overview 174 5977B Series MSD Troubleshooting and Maintenance Manual Figure 38. The analyzer with an XTR source Detector Mass filter contact cable Mass filter heater assembly Feedthrough board Mass filter contact Ion source (inside radiator) Mass filter (inside radiator) 7 Analyzer EI Ion Source 5977B Series MSD Troubleshooting and Maintenance Manual 175 EI Ion Source The EI ion source (See Figure 39 on page 176) operates by electron ionization. The sample enters the ion source from the GC/MSD interface. Electrons emitted by a filament enter the ionization chamber, guided by a magnetic field. The high-energy electrons interact with the sample molecules, ionizing and fragmenting them. The positive 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 into the mass filter. Ion source body The ion source body (See Figure 39 on page 176 and Figure 40 on page 177) is a cylinder. It holds the other parts of the ion source, including the lens stack. With the repeller, and in the SST/Inert ion source, the drawout plate, it forms the ionization chamber. The ionization chamber is the space where the ions are formed. Slots in the source body help the vacuum system to pump away carrier gas and unionized sample molecules or fragments. 7 Analyzer EI Ion Source 176 5977B Series MSD Troubleshooting and Maintenance Manual Figure 39. SST/Inert ion source structure Entrance lens Filament Drawout cylinder Drawout plate Repeller Ion focus lens Lens insulation 7 Analyzer EI Ion Source 5977B Series MSD Troubleshooting and Maintenance Manual 177 Figure 40. Extractor ion source structure Entrance lens Filament Extractor lens Ceramic insulator Repeller Ion focus lens Lens insulation 7 Analyzer EI Ion Source 178 5977B Series MSD Troubleshooting and Maintenance Manual Figure 41. SST/Inert ion source 1 2 8* 15 14 2* 2* 16 8* 12* 10 2* 8* 8* 7* 17 18 3 8 8 7 12 13 4 6 5 11 9 Table 12 Parts list for the standard or inert EI ion source (Figure 41 on page 178) Item number Item description Part number (SSL) Part number (Inert) 1 Gold plated set screw G1999-20022 G1999-20022 2 Gold plated screw G3870-20021 G3870-20021 3 Interface socket G1099-20136 G1099-20136 4 Source body G1099-20130 G2589-20043 5 Drawout cylinder G1072-20008 G1072-20008 6 Drawout plate 05971-20134 G2589-20100 7 Filament G7005-60061 G7005-60061 7 Analyzer EI Ion Source 5977B Series MSD Troubleshooting and Maintenance Manual 179 8 Spring washer 3050-1374 3050-1374 8 Flat washer 3050-0982 3050-0982 9 Lens insulator G3170-20530 G3170-20530 10 Entrance lens G3170-20126 G3170-20126 11 Ion focus lens 05971-20143 05971-20143 12 Repeller insulator G1099-20133 G1099-20133 13 Repeller G3870-60172 G3870-60173 14 Flat washer 3050-0627 3050-0627 15 Belleville spring washer 3050-1301 3050-1301 16 Repeller nut 0535-0071 0535-0071 17 Source heater block assembly G3870-60180 G3870-60179 18 Repeller block insert G3870-20135 G3870-20125 Table 12 Parts list for the standard or inert EI ion source (Figure 41 on page 178) (continued) Item number Item description Part number (SSL) Part number (Inert) 7 Analyzer EI Ion Source 180 5977B Series MSD Troubleshooting and Maintenance Manual Figure 42. Extractor ion source Table 13 Parts list for extractor ion source (Figure 42 on page 180) Item number Item description Part number 1 Setscrews G3870-20446 2 Screws G3870-20021 3 Source body G3870-20440 4 Extractor lens G3870-20444 5 Extractor lens insulator G3870-20445 6 Filament G7005-60061 7 Spring washer 3050-1301 7 Analyzer EI Ion Source 5977B Series MSD Troubleshooting and Maintenance Manual 181 The CI ion source is similar in design, but critical dimensions are different. Do not interchange parts. 7 Flat washer 3050-0982 8 Lens insulator G3870-20530 9 Entrance lens assembly, Extended G7000-20026 10 Ion focus lens 05971-20143 11 Repeller insulator G1099-20133 12 Repeller G3870-60171 13 Flat washer 3050-0891 14 Belleville spring washer 3050-1301 15 Repeller nut 0535-0071 16 Source heater block assembly G3870-60177 17 Insert, Repeller block G3870-20135 Table 13 Parts list for extractor ion source (Figure 42 on page 180) (continued) Item number Item description Part number 7 Analyzer HES EI Ion Source 182 5977B Series MSD Troubleshooting and Maintenance Manual HES EI Ion Source The HES EI ion source operates by electron impact ionization. The sample enters the ion source from the GC/MSD interface. Electrons emitted by a filament enter the ionization chamber, guided by a magnetic field. The high-energy electrons interact with the sample molecules, ionizing and fragmenting them. The positive 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, directed into the mass filter. Ion source body The ion source body is a cylinder. It holds the other parts of the ion source, including the lens stack. The repeller, source mount, and filament block form the ionization chamber. The ionization chamber is the space where the ions are formed. Slots in the source body help the vacuum system to pump away carrier gas and un-ionized sample molecules or fragments. 7 Analyzer HES EI Ion Source 5977B Series MSD Troubleshooting and Maintenance Manual 183 Figure 43. HES ion source 1 2 8 16 17 15 9 4 3 11 10 6 5 7 13 12 14 8 12 Table 14 Parts list for HES EI ion source Item number Item description Part number 1 Source finger grip G7002-20008 2 Filament block G7002-20019 3 Extractor lens (5)* , with 3 mm opening G7004-20061 4 Ceramic insulator for extractor G7002-20064 5 Entrance lens assembly, Extended, HES (1)* G7004-20065 6 Ion focus lens (2)* G7004-20068 7 Lens insulator/holder G7002-20074 7 Analyzer HES EI Ion Source 184 5977B Series MSD Troubleshooting and Maintenance Manual 8 M2 x 0.4 screw x 12 mm long gold plated screw G7002-20083 9 Source body G7002-20084 10 Post extractor lens 2 (3)* G7004-20090 11 Post extractor lens 1 (4)* G7004-20004 12 M2 x 6 mm gold plated screw G7002-20109 13 Locking ring lens insulator G7002-20126 14 High efficiency dual filament G7002-60001 15 Ring heater/sensor assembly G7002-60043 16 Source mount 1.5 mm G7002-60053 17 Repeller assembly G7002-67057 * The number in parenthesis is the number engraved on the lens Table 14 Parts list for HES EI ion source (continued) Item number Item description Part number 7 Analyzer CI Ion Source 5977B Series MSD Troubleshooting and Maintenance Manual 185 CI Ion Source The CI ion source is similar in shape to the traditional EI ion source, but only has one part in common with the EI ion source — the entrance lens. The single CI filament has a straight wire and a reflector. A “dummy” filament provides 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 plate are at repeller potential, electrically isolated from the radiator and the interface tip. The seal for the interface tip (Figure 45 on page 186) ensures a leak-tight seal and electrical isolation between the CI interface and ion source. Ion source body Figure 44. CI ion source structure Entrance lens Filament Drawout cylinder Drawout plate Dummy filament Ion focus lens Lens insulation Repeller 7 Analyzer CI Ion Source 186 5977B Series MSD Troubleshooting and Maintenance Manual Figure 45. Interface tip seal Interface tip seal Figure 46. CI ion source 15 16 7 Analyzer CI Ion Source 5977B Series MSD Troubleshooting and Maintenance Manual 187 Table 15 Parts list for the CI ion source (Figure 46 on page 186) Item number Item description Part number 1 Setscrew G1999-20022 2 Filament screw G1999-20021 Not shown CI interface tip seal G3870-20542 4 CI repeller insulator G1999-20433 5 CI lens insulator G3170-20540 6 CI drawout cylinder G1999-20444 7 CI drawout plate G1999-20446 8 CI ion source heater block assembly G3870-60415 9 Entrance lens G3170-20126 10 CI ion source body G3170-20430 11 CI ion focus lens G1999-20443 12 CI repeller G7077-20432 13 CI filament G7005-60072 14 Dummy filament G1999-60454 15 Curved washer 3050-1374 16 Flat washer 3050-9082 7 Analyzer Filaments 188 5977B Series MSD Troubleshooting and Maintenance Manual Filaments For an HES two filaments are located within the ion source mount of the EI ion source. For a non-HES, two filaments are located on opposite sides of the outside of the EI ion source. The active filament carries an adjustable AC emission current. The emission current heats the filament causing it to emit electrons which ionize the sample molecules. In addition, both filaments have an adjustable DC bias voltage. The bias voltage determines the energy on the electrons, usually –70 eV for a non-HES source and 120eV for the HES. The CI ion source has only one filament of a different design from the standard or extractor EI filaments. A dummy filament provides connections for the Filament 2 wire. The filament is shut off automatically if there is a general instrument shutdown. Three parameters affect the filaments: filament selection (Filament), filament emission (Emission) current, and electron energy (EIEnrgy). Filament selection The filament selection parameter (Filament) selects which filament in the ion source is active. In the CI ion source, it is always Filament 1. Sometimes, one EI filament will give better performance than the other does. To select the better of the two filaments, run two autotunes, one with each filament. Use the filament that gives the best results. Emission current The filament emission current (Emission) is variable between 0 and 315 µA, but should be set to the software default for normal operation. Electron energy The electron energy (EIEnrgy) is the amount of energy on the ionizing electrons. It is determined by the bias voltage; –70 VDC bias on the filament causes emitted electrons to possess –70 eV (electron volts). This value is adjustable from –5 to –241 VDC, but for normal operation, set this parameter to 70 for a non-HES source and 120 for the HES. 7 Analyzer Filaments 5977B Series MSD Troubleshooting and Maintenance Manual 189 Filament care Similar to the filaments in incandescent light bulbs, the ion source filaments will eventually burn out. Certain practices reduce the chance of early failure: • If you have an optional G3397B Micro-Ion vacuum gauge, use it to verify that the system has an adequate vacuum before turning on the analyzer, especially after any maintenance was performed. • If you are controlling your MSD from the Manual Tune screen, always select MSOff before changing any of the filament parameters. • When setting up data acquisition parameters, set the solvent delay so that the analyzer will not turn on while the solvent peak is eluting. • When the software prompts Override solvent delay? at the beginning of a run, always select NO. • Higher emission current reduces filament life. • Higher electron energy reduces filament life. • Leaving the filament on for short times (≤1 minute) during data acquisition reduces filament life. 7 Analyzer Other Source Elements 190 5977B Series MSD Troubleshooting and Maintenance Manual Other Source Elements Magnet The field created by the magnet directs the electrons emitted by the filament into and across the ionization chamber. The HES magnet assembly is a permanent magnet with a charge of 650 gauss in the center of the field. The non-HES and CI source 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 repeller pushes positively-charged ions out of the source through a series of lenses. The repeller voltage is also known as the ion energy, although the ions only receive about 20% of the repeller energy. The repeller voltage can be varied from 0 to +42.8 VDC. Some tune programs use a fixed repeller voltage. Others ramp the repeller voltage to find the 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 resolution. Drawout plate and cylinder The drawout plate forms another wall of the ionization chamber. The ion beam passes through the hole in the drawout plate and into the drawout cylinder. The drawout cylinder is slotted. The slots correspond to slots in the source body. These slots allow carrier gas and unionized sample molecules or fragments to be pulled away by the vacuum system. The drawout plate and drawout cylinder are both at ground potential. These are used in the standard, inert, and CI ion sources only. Extractor lens A voltage is applied to the extractor lens to increase ion focusing through the source. 7 Analyzer Other Source Elements 5977B Series MSD Troubleshooting and Maintenance Manual 191 HES Post extractor lens 1 and 2 The post extractor lenses are part of the lens stack in the EI HES source only. A voltage is applied to the two lenses to increase ion focusing through the source. Ion focus The voltage on the ion focus lens can be varied from 0 to –127 VDC. A typical voltage is between –70 and –90 VDC. In general: • Increasing the ion focus voltage improves sensitivity at lower masses. • Decreasing the ion focus voltage improves sensitivity at higher masses. • Incorrect ion focus adjustment results in poor high mass response. Entrance lens The entrance lens is at the entrance to the quadrupole mass filter. This lens minimizes the fringing fields of the quadrupole which discriminate against high-mass ions. Entrance lens offset The entrance lens offset (EntOff) controls the fixed voltage applied to the entrance lens. It can be varied from 0 to –64 VDC (–20 V is typical). Increasing the entrance lens offset generally increases the abundance of ions at low masses without substantially decreasing the abundance of high mass ions. Entrance lens gain Entrance lens gain (EntLens) controls the variable voltage applied to the entrance lens. It determines how many volts are applied for each m/z. It can be varied from 0 to –128 mV/(m/z). A typical range is 0 to –40 mV/amu. 7 Analyzer Quadrupole Mass Filter 192 5977B Series MSD Troubleshooting and Maintenance Manual Quadrupole Mass Filter The mass filter separates ions according to their mass-to-charge ratio (m/z). At a given time, only ions of a selected m/z can pass through the filter to the detector. The mass filter in the MSD is a quadrupole (See Figure 47 on page 193). The quadrupole is a fused-silica (quartz) tube coated with a thin layer of gold. The four hyperbolic surfaces create the complex electric fields necessary for mass selection. Opposing segments are connected; adjacent segments are electrically isolated. One pair has positive voltages applied, the other has negative voltages applied. A combined direct current (DC) and radio frequency (RF) signal is applied to the two pairs of segments. The magnitude of the RF voltage determines the m/z of the ions that pass through the mass filter and reach the detector. The ratio of DC-to-RF 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 can be manually adjusted in the Edit Tune Parameters dialog. • AMU gain (AmuGain) • AMU offset (AmuOffs) • 219 width (Wid219) • DC polarity (DC Pol) • Mass (axis) gain (MassGain) • Mass (axis) offset (MassOffs) • MS quad temp 7 Analyzer Quadrupole Mass Filter 5977B Series MSD Troubleshooting and Maintenance Manual 193 AMU gain AMU gain (AmuGain) affects the ratio of DC voltage to RF frequency on the mass filter. This controls the widths of the mass peaks. • Higher gain yields narrower peaks. • AMU gain affects peaks at high masses more than peaks at low masses. AMU offset AMU offset (AmuOffs) also affects the ratio of DC voltage to RF frequency on the mass filter. • Higher offset yields narrower peaks. • AMU offset generally affects peak widths equally at 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 Autotune, or set it to 0. Figure 47. Quadrupole mass filter 7 Analyzer Quadrupole Mass Filter 194 5977B Series MSD Troubleshooting and Maintenance Manual DC polarity The DC polarity (DC Pol) parameter selects the orientation of the direct current applied to the quadrupole mass filter. The DC Pol that works best for your MSD is determined at the factory. It is listed on the final test sheet accompanying your MSD. It is also listed on a label on the cover over the RF coils. This cover can be viewed by removing the upper MSD cover. Mass (axis) gain Mass gain (MassGain) controls the mass assignment, that is, assignment of a particular 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 offset generally affects peaks equally at all masses. Quadrupole maintenance The mass filter requires no periodic maintenance. It should not be removed from 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 Using the nonpreferred DC polarity may result in very poor performance. Always use the factory-specified polarity. CAUTION Never put the quadrupole in an ultrasonic cleaner. Never change the physical orientation of the quadrupole mass filter. The fused-quartz quadrupole is fragile and will break if dropped or handled roughly. The material in the cusps of the quadrupole is very hygroscopic. If exposed to water, the quadrupole must be dried very slowly to prevent damage. 7 Analyzer Detector 5977B Series MSD Troubleshooting and Maintenance Manual 195 Detector The detector (See Figure 48 on page 196) in the MSD analyzer is a high energy conversion dynode (HED) coupled to an electron multiplier (EM). The detector is located at the exit end of the quadrupole mass filter. It receives the ions that have passed through the mass filter. The detector generates an electronic signal proportional to the number of ions striking it. The detector has three main components: the detector ion focus, the HED, and the EM horn. Detector ion focus The detector ion focus directs the ion beam into the HED, which is located off axis. The voltage on the detector focus lens is fixed at –600 V. High energy dynode The HED operates at –10,000 V for EI and PCI, and +10,000 V for NCI. It is located off-axis from the 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 attracted to the more positive EM horn. Do not touch the insulator. EM horn The EM horn carries a voltage of up to –3,000 V at its opening and 0 V at the other end. The electrons emitted by the HED strike the EM horn and cascade through the horn, liberating more electrons as they go. At the far end of the horn, the current generated by the electrons is carried through a shielded cable outside the analyzer to the signal amplifier board. The voltage applied to the EM horn determines the gain. The voltage is adjustable from 0 to –3,000 VDC. Use the EM voltage found in autotune as a baseline for the EM voltage setting. • To increase signal gain, increase the EM voltage. • For concentrated samples where less signal gain is needed, decrease the EM voltage. As the EM horn ages, the voltage (EMVolts) required increases over time. If the EM voltage must always be set at or near –3,000 VDC to complete Autotune, with no other probable cause, it may need to be replaced. Check your tune charts 7 Analyzer Detector 196 5977B Series MSD Troubleshooting and Maintenance Manual for gradual degradation, which indicates wearing out. Select the Tune Plot icon from the Program menu of your desktop to see the tune plots. Sudden changes usually indicate a different type of problem. See Also • Troubleshooting in the online help for more information about symptoms that may indicate EM problems. Figure 48. The detector HED high voltage EM horn 7 Analyzer Analyzer Heaters and Radiators 5977B Series MSD Troubleshooting and Maintenance Manual 197 Analyzer Heaters and Radiators The ion source and mass filter are housed in cylindrical aluminum tubes called radiators (See Figure 49 on page 198) or (See Figure 50 on page 199). The radiators control the distribution of heat in the analyzer. They also provide electrical shielding for analyzer components. The source heater and temperature sensor are mounted in the source heater block. The mass filter (quad) heater and temperature sensor are mounted on the mass filter radiator. Analyzer temperatures can be set and monitored from the MSD Data Acquisition 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 fragmentation and, therefore, lower high-mass sensitivity. After pumpdown, it takes at least 2 hours for the analyzer to reach thermal equilibrium. Data acquired sooner may not be reproducible. Recommended settings (for EI operation): • Ion source 230 °C • Quadrupole 150 °C The GC/MSD interface, ion source, and mass filter (quad) heated zones interact. The analyzer heaters may not be able to accurately control temperatures if the setpoint for one zone is much lower than that of an adjacent zone. CAUTION Do not exceed 200 °C on the quadrupole, or 350 °C on the ion source. 7 Analyzer Analyzer Heaters and Radiators 198 5977B Series MSD Troubleshooting and Maintenance Manual Figure 49. Heaters and radiators with an XTR source Mass filter radiator Mass filter heater assembly Ion source radiator Ion source heater assembly 7 Analyzer Analyzer Heaters and Radiators 5977B Series MSD Troubleshooting and Maintenance Manual 199 Figure 50. Heaters and radiators with an HES Mass filter radiator Mass filter heater assembly Ion source radiator Ion source heater/sensor wires (gray and purple) 7 Analyzer Analyzer Heaters and Radiators 200 5977B Series MSD Troubleshooting and Maintenance Manual 5977B Series MSD Troubleshooting and Maintenance Manual 201 8 Electronics GC Control Panel, Power Switch, and Front Panel LED 202 Side Board 204 Electronics Module 205 LAN/MS Control Card 209 Power Supplies 210 Back Panel and Connectors 211 Interfacing to External Devices 214 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. WARNING Dangerous voltages are present under the safety covers. Do not remove safety covers. Refer servicing to your Agilent Technologies service representative. 8 Electronics GC Control Panel, Power Switch, and Front Panel LED 202 5977B Series MSD Troubleshooting and Maintenance Manual GC Control Panel, Power Switch, and Front Panel LED GC Control Panel (LCP) You can view MSD system status and perform some control functions from the control panel on a connected 8890 GC (touchscreen) or 7890 GC (keypad). There is no control panel on the MSD. Functions available through the GC control panel include: • Configure network settings of the MSD • Change the MSD temperatures • View analyzer vacuum or turbo pump speed • View foreline pump vacuum • Vent or pumpdown the MSD • View the firmware version and serial number of the MSD • Enable LVDS on the MSD • Reboot the MSD • Enable BOOTP on the MSD Power switch The power switch is part of the electronics module, and is located on the lower left of the front of the MSD. It is used to turn the MSD and foreline pump on and off. Front Panel LED The front panel LED shows the current instrument status through a color code, as shown in Table 16 on page 203. CAUTION Do not switch the MSD off unless it has completed the vent program. Incorrect shutdown can seriously damage the MSD. 8 Electronics GC Control Panel, Power Switch, and Front Panel LED 5977B Series MSD Troubleshooting and Maintenance Manual 203 Table 16 Front panel Instrument Status LED codes Instrument status LED code Ready Solid green Acquiring data Blinking green Not ready Solid yellow JetClean Acquire & Clean operation Blinking magenta JetClean Clean Only operation Solid magenta Not connected to DS (system idle) Solid blue Ready and not connected to DS Solid yellow for 3 sec, quick double blink Start up (prior to FW load) Blinking red Fault Solid red 8 Electronics Side Board 204 5977B Series MSD Troubleshooting and Maintenance Manual Side Board The side board is mounted on the side plate. It performs these functions: • Provides the 1 MHz reference clock for the RF amplifier. • Generates the RF component of the voltage applied to the quadrupole mass filter according to a signal from the main board. The amplitude of this voltage is proportional 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 by the main board. • Switches the filament power from one filament to the other. • Monitors for RF faults and shuts down the analyzer if one is detected. 8 Electronics Electronics Module 5977B Series MSD Troubleshooting and Maintenance Manual 205 Electronics Module Most of the electronics in the MSD are contained in the electronics module. The whole electronics module can be replaced, if necessary, by your Agilent Technologies service representative. The electronics module contains: • Main board • Signal amplifier board • LAN/MS control card • AC board (power distribution/vacuum control board) • Low voltage (AC-DC) power supply • High voltage (HED) power supply • Toroid transformer assembly • Lens driver board for HES Main board The main board is mounted on the outer side of the electronics module. The main board performs these functions: • Receives and decodes digital instructions from the LAN/MS control card. • Sends digital information to the LAN/MS control card. • Generates voltages for the ion source lenses. • Generates control signals for filament selection, filament emission current, and electron energy. Generates control signals for quadrupole RF drive, quad frequency adjustment, DC polarity selection, and all detector voltages. • Performs analog-to-digital conversion for the Direct 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 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 signals (on and off) used by the AC board for the high vacuum pump and calibration valve. • Generates ±280 VDC (nominal) power for main board lens amplifiers and side board DC amplifiers. 8 Electronics Electronics Module 206 5977B Series MSD Troubleshooting and Maintenance Manual • Supplies and controls the power for the ion source and quadrupole (mass filter) heaters. • Provides 24 VDC power for the cooling fans. Signal amplifier board The signal amplifier board amplifies the output of the detector. It produces an output voltage of 0 to 10 V DC, proportional to the logarithm of the input current of 3 picoamps to 50 microamps. An analog-to-digital converter converts the amplifier output voltage to digital information. The LAN/MSD control card converts the data into abundance counts proportional to the detector signal current. Lens driver board for HES The lens driver board provides the lens voltages for the extractor, post extractor 1, and post extractor 2 lenses. AC board The AC board is mounted on the opposite side of the electronics panel from the LAN/MSD control card. The AC board is also sometimes called the power distribution/vacuum control board. It performs these functions: • Provides input voltage transparency for the MSD. • Distributes AC line power to the AC/DC power supply, the foreline pump, and the turbo pump controller. • Turns the calibration valve on or off as directed by the main board. • Provides the voltage for the calibration valve. • Provides a logic interface to turbo controller. • Controls the diffusion pump: • Controls the foreline gauge. • Turns on the diffusion pump once the foreline pressure is low enough, as directed by the main board. • Regulates the AC power to the diffusion pump heater. • Turns off the diffusion pump if the foreline pressure is too high or if the diffusion pump is too hot. 8 Electronics Electronics Module 5977B Series MSD Troubleshooting and Maintenance Manual 207 • Passes the foreline pressure signal from the foreline gauge or turbo pump speed and other vacuum status information to the main board. • Turns off the foreline pump in case of a problem with pumpdown. Diffusion pump control The power regulator ensures that the diffusion pump heater receives constant power, even if there are fluctuations in the AC line voltage. It measures the voltage across the heater and the current through it, multiplies them together, and compares the result with a standard value. Any discrepancy is applied as an error signal to adjust the power. If the power distribution board senses a malfunction in the diffusion pump power regulator, it shuts off power to the diffusion pump. See Figure 51. Turbo pump control Your MSD is equipped with a turbo pump with an integrated controller. The AC board sends control signals to, and receives turbo pump status information from, the turbo pump controller. The turbo pump controller provides power to the turbo pump and regulates pump speed. If the pump fails to reach 80% speed within 7 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. Figure 51. Diffusion pump control Hi vac power cable Diffusion pump harness Diffusion pump heater cable Fan Diffusion pump Heater Sensors HI VAC Power Harnes CAL valve MSD electronics module (AC board) Foreline gauge 8 Electronics Electronics Module 208 5977B Series MSD Troubleshooting and Maintenance Manual Pumpdown failure shutdown The AC board will shut down both the high vacuum and the foreline pump if the system fails to pump down correctly. Other conditions that trigger shutdown are turbo pump speed below 80% after 7 minutes, or foreline pressure above 300 mTorr after 7 minutes. This is usually because of a large air leak: either the sideplate has 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. To correct the problem, power cycle the MSD and troubleshoot. You have 7 minutes to find and correct the air leak before the system shuts down again. Press on the side plate when turning on the MSD power to ensure a good seal. 8 Electronics LAN/MS Control Card 5977B Series MSD Troubleshooting and Maintenance Manual 209 LAN/MS Control Card The LAN/MS control card is located to the left of the main board on the electronics panel. The LAN/MS control card 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 LAN/MS control card include: • Instrument controller • Data processor • Main processor • Serial communication processor • Network communication controller • Remote start processor • Random access memory (RAM) • Status LEDs • Local Control panel firmware • Mini display module LEDs on the LAN/MS control card are visible on the rear panel. The upper two LEDs indicate network communication. The two bottom LEDs are the power (On, digital 5 V) and the heartbeat indicator. The flashing heartbeat LED indicates that the operating system of the MSD is functioning. In case of catastrophic loss of flash memory, the heartbeat flashes in an SOS (•••– – – •••) pattern. 8 Electronics Power Supplies 210 5977B Series MSD Troubleshooting and Maintenance Manual Power Supplies Low voltage (AC-DC) power supply The low voltage power supply is mounted next to the toroid transformer in the electronics module. A universal input power supply, it converts AC line voltage into the DC voltages used by the 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 V DC for the high energy dynode (HED) in the detector for the EI MSD. The EI/PCI/NCI MSD requires a bipolar power supply that can also provide +10,000 V for NCI operation. The HED power supply also provides 600 VDC for the detector focus lens. Due to the high impedance of this circuit, measuring the detector focus voltage with a handheld voltmeter will give a typical reading of 90 to 100 V where the polarity matches that of the HED voltage. Toroid transformer The toroid transformer is mounted next to the AC board. It provides 24 VAC for the mass filter and source heater circuits. The input wires take 120 VAC or 200 to 260 VAC from the AC board. The AC board samples the line voltage and uses a relay to appropriately strap the toroid primary. The output wires connect to the main board. 8 Electronics Back Panel and Connectors 5977B Series MSD Troubleshooting and Maintenance Manual 211 Back Panel and Connectors The back panel (See Figure 52 on page 213) contains several connectors, the primary fuses, and several status LEDs. Most of these components are part of the AC board or the LAN/MS control card, and extend through the back panel. HI-VAC SIGNAL The high vacuum signal connector is on the AC board. See “Turbo pump control” on page 207 and “Diffusion pump control” on page 207. HI-VAC POWER The high vacuum power connector carries power for the diffusion pump heater or the turbo controller from the AC board. Primary fuses The primary fuses limit current into the MSD in case of a short circuit in the foreline pump. The primary fuses are on the AC board. Power cord receptacle The AC power cord brings in all electrical power for the MSD. The power cord can be detached from the MSD. FORELINE PUMP The foreline pump power cord receptacle provides AC power for the foreline pump. If the power switch is off, no power is supplied to the foreline pump. REMOTE The remote start connector is the external connector for the remote start circuitry on the LAN/MS control card. It receives remote start signals from the GC. 8 Electronics Back Panel and Connectors 212 5977B Series MSD Troubleshooting and Maintenance Manual High vacuum gauge connector This powers the high vacuum gauge and connects its signal to the controlling electronics. SERIAL A This RS-232 connector is not currently used. CI COMM This RS-232 connector goes to the CI flow module if it is installed on the MSD. It handles data communication between the GC and the MSD. LAN The LAN cable from the data system is connected to this LAN connector. This cable carries all data communication between the PC and the MSD. LAN/MSD control card LEDs The two upper LEDs indicate network communication. The two bottom LEDs are the power and the heartbeat indicator. GC COMM This RS-232 cable connector is used for LVDS communication with a supported GC. 8 Electronics Back Panel and Connectors 5977B Series MSD Troubleshooting and Maintenance Manual 213 Figure 52. Back panel connections Remote start Primary fuses Power cord LAN High vacuum control High vacuum power Foreline pump RS-232 Serial B power cord RS-232 Serial A GC communication High vacuum gauge connector 8 Electronics Interfacing to External Devices 214 5977B Series MSD Troubleshooting and Maintenance Manual Interfacing to External Devices Remote control processor The remote control processor on the LAN/MS control card synchronizes start-run signals with GCs and other devices. The functions of the remote control processor are extended to the remote start (Remote) connector (Figure 53) 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. They also include: • Receive a start run signal from an external device • Program the timing of events during a run System ready When interfacing to an external device, it is often desirable to send a system-ready signal to the device. In the case of a multisample Tekmar purge-and-trap, each sample is purged onto a trap where it waits for a ready signal. On receipt of the ready signal, the desorbtion cycle begins. When a specific temperature is reached, the purge-and-trap closes a contact to indicate the run has started. Figure 53 Remote start connector Start Ground Ready 8 Electronics Interfacing to External Devices 5977B Series MSD Troubleshooting and Maintenance Manual 215 The ready pin on the remote start connector on the GC is held low at all times except when the GC, MSD, and data system are all ready. On system ready, a logic high of 5 VDC 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 general-purpose remote start cable (05890-61080), that terminates in spade lugs, is also available. Ensure that the system is actually ready before the start run signal is sent. If necessary, the remote start connector on the back of the MSD 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. 8 Electronics Interfacing to External Devices 216 5977B Series MSD Troubleshooting and Maintenance Manual 5977B Series MSD Troubleshooting and Maintenance Manual 217 9 Parts To Order Parts 218 Electronics 219 Fuses 219 Vacuum System 219 O-rings and seals 219 Standard foreline pump and related parts 220 MVP-070 foreline pump and related parts 222 IDP3 Dry foreline pump and related parts 223 Turbo pump and related parts 225 Turbo pump and related parts 225 Analyzer 226 Extractor ion source 228 CI ion source 230 HES ion source 232 EI GC/MSD Interface 234 CI GC/MSD Interface 235 Consumables and Maintenance Supplies 236 This chapter lists parts that can be ordered for use in maintaining your 5977B Series MSD. It includes most of the parts or assemblies in the MSDs. This chapter is organized so that related parts are grouped together. Some of the parts listed are not user-replaceable. They are listed here for use by Agilent Technologies service representatives. 9 Parts To Order Parts 218 5977B Series MSD Troubleshooting and Maintenance Manual To Order Parts To order parts for your MSD, contact your local Agilent Technologies office. Supply them with the following information: Model and serial number of your MSD, located on a label on the lower left side near the front of the instrument. • 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 specifications 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 assemblies are available on an exchange-only basis. When you return the original part to Agilent Technologies (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 on-line catalogue on the worldwide web at http://www.agilent.com/chem. If you still cannot find it, contact your Agilent Technologies service representative or your Agilent Technologies office. 9 Parts Electronics 5977B Series MSD Troubleshooting and Maintenance Manual 219 Electronics The printed circuit boards in the MSD are available only as complete assemblies. Individual electronic components are not available. This section contains the following parts: fuses (Table 17). Fuses Vacuum System This section lists replacement parts available for the vacuum system. It includes, O-rings and seals (Table 18), standard foreline pump and related components (Table 19 on page 220 and Figure 54 on page 221), dry foreline pump and related components (Table 20 on page 222, Table 21 on page 223, Figure 55 on page 222, and Figure 56 on page 223), diffusion pump and related components (Table 22 on page 224 and Figure 57 on page 224), and turbo pump vacuum system components (Table 23 on page 225 and Figure 58 on page 225). O-rings and seals Table 17 Fuses Description Part number Fuse T12.5A, 250 V 2110-1398 Table 18 O-rings and seals Description Part number Calibration valve O-ring (1/4-inch) 5180-4182 KF10/16 seal (foreline pump inlet), Micro-Ion vacuum gauge KC16AV KF10/16 seal (foreline pump inlet and diffusion pump outlet), Micro-Ion vacuum gauge KC16AV KF50 seal (diffusion pump inlet) 0100-1884 Side plate O-ring 0905-1442 Vent valve O-ring (1/4-inch) 5180-4182 9 Parts Vacuum System 220 5977B Series MSD Troubleshooting and Maintenance Manual Standard foreline pump and related parts Table 19 Standard foreline pump and related parts (Figure 54 on page 221) Description Part number Pfeiffer RVP – 115 V G3870-80055 Pfeiffer RVP – 230 V G3870-80056 Pfeiffer RVP – 200 V G6870-80054 Pfeiffer RVP – 115 V – Rebuilt G3870-89055 Pfeiffer RVP – 230 V – Rebuilt G3870-89056 Pfeiffer RVP – 200 V – Rebuilt G6870-89054 Foreline hose assembly (hose and internal spring) 05971-60119 Hose Clamp* used with 05971-60119 * Hose clamps are interchangeable, but give an optimum fit if they are matched 1400-3241 Foreline pump inlet seal (KF10/16) KC16AV KF10/16 Clamp (foreline inlet), Micro-Ion vacuum gauge KC160000AB Oil drip tray G3170-00012 Drain plug for foreline pump 0100-2452 O-ring for foreline pump drain plug 0905-1619 Fill plug 0100-2451 O-ring for foreline fill plug 0905-1620 Oil mist filter (blue) G1099-80039 Hose barb adapter (exhaust fitting) G3170-80006 O-ring for oil mist filter and hose barb adapter 0905-1193 Foreline pump oil 6040-0621 5 mm hex key 8710-1838 9 Parts Vacuum System 5977B Series MSD Troubleshooting and Maintenance Manual 221 Figure 54. Pfeiffer DUO pump 9 Parts Vacuum System 222 5977B Series MSD Troubleshooting and Maintenance Manual MVP-070 foreline pump and related parts Table 20 Dry foreline pump and related parts (Figure 55) Description Part number Dry pump, MVP 070-3 G3870-80051 Dry pump, MVP 070-3C G3870-80061 Dry pump, MVP 070-3 – Rebuilt G3870-80052 Dry pump, MVP 070-3C – Rebuilt G3870-89052 Figure 55. MVP-070 foreline pump 9 Parts Vacuum System 5977B Series MSD Troubleshooting and Maintenance Manual 223 IDP3 Dry foreline pump and related parts Table 21 IDP3 foreline pump and related parts (Figure 56) Description Part number Foreline hose assembly (hose and internal spring) 05971-60119 Hose Clamp* used with 05971-60119 * Hose clamps are interchangeable, but give an optimum fit if they are matched 1400-3241 Dry foreline pump G3870-60600 Replace tip seal set, non-ammonia IDP3TS Solid tip seal kit, inert G3870-67000 KF10/16 Clamp (foreline inlet), Micro-Ion vacuum gauge 0100-1397 KF16 Hose adapter G1099-20531 Vibration Isolation kit IDP3VIBISOKIT Exhaust hose G3170-60100 Exhaust adapter G3170-80029 Barbed fitting G3170-80006 Exhaust filter cartridge REPLSLRFILTER2 Figure 56. IDP3 Dry foreline pump CAUTION Agilent does not recommend using hydrogen as a carrier gas on systems equipped with an IDP3 foreline pump. 9 Parts Vacuum System 224 5977B Series MSD Troubleshooting and Maintenance Manual Diffusion pump and related parts Table 22 Diffusion pump MSD vacuum system components (Figure 57) Item Description Part number 1 Diffusion pump 120 V G1099-80500 220/240 V G1099-80501 2 Fan (for high vacuum pump) G7005-60564 3 Foreline gauge assembly G1099-60545 KF50 clamp 0100-1395 Figure 57. Diffusion pump removed from analyzer chamber connection and related parts Diffusion pump Foreline gauge assembly High vacuum fan 9 Parts Vacuum System 5977B Series MSD Troubleshooting and Maintenance Manual 225 Turbo pump and related parts Table 23 Turbo pump MSD vacuum system components (Figure 58) Description Part number Turbomolecular pump G3170-80162 Pfeiffer HiPace 300 turbo pump- Rebuilt G3170-89162 Turbo power assembly G3170-60600 Centering ring seal with screen 0905-1613 Figure 58. Turbo pump and related parts Turbo Pump Ion gauge assembly 9 Parts Analyzer 226 5977B Series MSD Troubleshooting and Maintenance Manual Analyzer Table 24 and Figure 59 show the analyzer chamber and associated parts. Table 25 and Figure 60 on page 227 (non-HES version) or Figure 61 on page 227 (HES version) show the replacement parts for the analyzer. Analyzer screws are listed in the tables that follow. Table 24 Analyzer chamber and related parts Description Part number Calibration vial G3170-80002 Vent valve knob G7077-20554 Figure 59. Analyzer chamber and related parts Calibration vial Vent valve knob Table 25 Analyzer parts Description Part number TAD assembly (Detector, HED, bracket) G7002-80105 Detector (Electron multiplier horn) G7002-80103 EI 350 ion source, new Turbo – inert Diffusion – stainless steel G3870-67700 G3870-67750 EI 350 extractor ion source G3870-67720 HES ion source G7002-67055 CI ion source G7077-67404 Interface tip seal G3870-20542 9 Parts Analyzer 5977B Series MSD Troubleshooting and Maintenance Manual 227 Figure 60. Analyzer parts (non-HES version) Figure 61. Analyzer parts (HES version) Ion source Electron multiplier horn (under clips) Detector Detector Electron multiplier horn (under clips) Ion source 9 Parts Analyzer 228 5977B Series MSD Troubleshooting and Maintenance Manual Extractor ion source Table 26 Analyzer screws Description Part number Ion source thumbscrew G1099-20138 Table 27 Parts list for extractor ion source (Figure 62 on page 229) Item Description Part number 1 Setscrews G3870-20446 2 Screws G3870-20021 3 Source body G3870-20440 4 Extractor lens G3870-20444 5 Extractor lens insulator G3870-20445 6 Filament G7005-60061 7 Spring washer 3050-1301 7 Flat washer 3050-0982 8 Lens insulator G3870-20530 9 Entrance lens assembly, Extended G7000-20026 10 Ion focus lens 05971-20143 11 Repeller insulator G1099-20133 12 Repeller G3870-60171 13 Flat washer 3050-0891 14 Belleville spring washer 3050-1301 15 Repeller nut 0535-0071 16 Source heater block assembly G3870-60177 17 Insert, Repeller block G3870-20135 9 Parts Analyzer 5977B Series MSD Troubleshooting and Maintenance Manual 229 Figure 62. Extractor EI ion source 9 Parts Analyzer 230 5977B Series MSD Troubleshooting and Maintenance Manual CI ion source Table 28 Parts list for the CI ion source (Figure 63 on page 231) Item Description Part number 1 Setscrew G1999-20022 2 Filament screw G1999-20021 Not shown CI interface tip seal G3870-20542 4 CI repeller insulator G1999-20433 5 CI lens insulator G3170-20540 6 CI drawout cylinder G1999-20444 7 CI drawout plate G1999-20446 8 CI ion source heater block assembly G3870-60415 9 Entrance lens G3170-20126 10 CI ion source body G3170-20430 11 CI ion focus lens G1999-20443 12 CI repeller G7077-20432 13 CI filament G7005-60072 14 Dummy filament G1999-60454 15 Curved washer 3050-1374 16 Flat washer 3050-9082 9 Parts Analyzer 5977B Series MSD Troubleshooting and Maintenance Manual 231 Figure 63. The CI ion source 15 16 9 Parts Analyzer 232 5977B Series MSD Troubleshooting and Maintenance Manual HES ion source Table 29 Parts list for the HES EI ion source (Figure 64 on page 233) Item Description Part number 1 Source finger grip G7002-20008 2 Filament block G7002-20019 3 Extractor lens (5)* , with 3 mm opening * The number in parenthesis is the number engraved on the lens G7004-20061 4 Ceramic insulator for extractor G7002-20064 5 Entrance lens assembly, Extended, HES (1)* G7004-20065 6 Ion focus lens (2)* G7004-20068 7 Lens insulator/holder G7002-20074 8 M2 x 0.4 screw x 12 mm long gold plated screw G7002-20083 9 Source body G7002-20084 10 Post extractor lens 2 (3)* G7004-20090 11 Post extractor lens 1 (4)* G7004-20004 12 M2 x 6 mm gold plated screw G7002-20109 13 Locking ring lens insulator G7002-20126 14 High efficiency dual filament G7002-60001 15 Ring heater/sensor assembly G7002-60043 16 Source mount 1.5 mm G7002-60053 17 Repeller assembly G7002-67057 9 Parts Analyzer 5977B Series MSD Troubleshooting and Maintenance Manual 233 Figure 64. HES ion source 1 2 8 16 17 15 9 4 3 11 10 6 5 7 13 12 14 8 12 9 Parts Analyzer 234 5977B Series MSD Troubleshooting and Maintenance Manual EI GC/MSD Interface Table 30 lists the replacement parts related to the EI GC/MSD interface. Figure 65 illustrates the parts. Table 30 EI GC/MSD interface Item Description Part number Not shown EI Transferline Assembly G7077-67300 1 Transferline tip cap, threaded G3870-20547 2 1/16 Ferrule no hole (qty 10) 5181-3308 3 M3 set screw 0515-0236 4 Transferline tip base, threaded G3870-20548 5 Transfer tip G3870-20542 6 Column nut 05988-20066 7 M3 screw G1999-20022 8 M4 X 0.7 16MM-LG 0515-0383 9 Heater clamp G7077-20210 10 Transfer line spring G1999-20023 11 Welded interface assembly G3870-60301 12 Heater/sensor assembly G1099-60109 Figure 65. EI GC/MSD interface 9 Parts Analyzer 5977B Series MSD Troubleshooting and Maintenance Manual 235 CI GC/MSD Interface Table 31 lists the replacement parts related to the CI GC/MSD interface. Figure 66 illustrates the parts. Table 31 CI GC/MSD interface Item Description Part number Not shown CI Transferline Assembly, untested G7077-67400 1 Transferline tip cap, threaded G3870-20547 2 1/16 Ferrule no hole (qty 10) 5181-3308 3 M3 set screw 0515-0236 4 Transferline tip base, threaded G3870-20548 5 Transfer tip G3870-20542 6 Column nut 05988-20066 7 M3x3L screw-set, gold plated G1999-20022 8 M4 X 0.7 16MM-LG screws for heater clamp 0515-0383 9 Heater clamp G7077-20410 10 Transfer line spring G1999-20023 11 Welded interface assembly G3870-67401 12 Heater/sensor assembly G1099-60107 Figure 66. CI GC/MSD interface 9 Parts Consumables and Maintenance Supplies 236 5977B Series MSD Troubleshooting and Maintenance Manual Consumables and Maintenance Supplies This section (Tables 32 through 36) lists parts available for cleaning and maintaining your MSD. Table 32 EI maintenance supplies Description Part number Abrasive paper, 30 µm 5061-5896 Alumina powder, 100 g 3937-6201 Cloths, clean (qty 300) 05980-60051 Cloths, cleaning (qty 300) 9310-4828 Cotton swabs (qty 100) 5080-5400 Diffusion pump fluid (2 required) 6040-0809 Foreline pump oil, D545, 0.5 L 6040-0621 IDP-3 foreline pump replacement tip seal kit IDP3TS IDP-3 foreline pump 24V Power Supply G3870-60600 Gloves, clean – Large 8650-0030 Gloves, clean – Small 8650-0029 Grease, Apiezon L, high vacuum 6040-0289 9 Parts Consumables and Maintenance Supplies 5977B Series MSD Troubleshooting and Maintenance Manual 237 Table 33 Tools Description Part number Column installation tool G1099-20030 Funnel 9301-6461 Hex key, 5 mm 8710-1838 Tool Kit G1099-60566 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) 8710-1094 Screwdrivers Flat-blade, large 8730-0002 Screwdrivers Torx, T-6 8710-2548 Screwdrivers Torx, T-10 8710-1623 Screwdrivers Torx. T-20 8710-1615 Tweezers, nonmagnetic 8710-0907 Wrenches, open-end 1/4-inch x 5/16-inch 8710-0510 Wrenches, open-end 10-mm 8710-2353 9 Parts Consumables and Maintenance Supplies 238 5977B Series MSD Troubleshooting and Maintenance Manual Table 34 Ferrules Description Part number For the GC/MSD interface using a standard column nut • Blank, graphite-vespel 5181-3308 • 0.3-mm id, 85%/15% for 0.10-mm id columns 5062-3507 • 0.4-mm 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/MSD interface using a self-tightening column nut • Blank, graphite-vespel 5181-3308 • 0.3-mm id, 85%/15% for 0.10-mm id columns 5062-3507 • 0.4-mm id, 85%/15% for 0.0 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 5062-3512 Figure 67. GC/MSD interface with a self-tightening column nut GC/MSD interface with self-tightening nut 9 Parts Consumables and Maintenance Supplies 5977B Series MSD Troubleshooting and Maintenance Manual 239 Table 35 Ferrules for the GC inlet, using standard or self-tightening column nuts Description Part number • 0.27-mm id, 90%/10%, for 0.10-mm id columns 5062-3518 • 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 Figure 68. GC inlet with self-tightening column nut GC inlet with selftightening nut 9 Parts Consumables and Maintenance Supplies 240 5977B Series MSD Troubleshooting and Maintenance Manual Table 36 Miscellaneous EI and CI parts and samples Description Part number Benzophenone, 100 pg/µL 8500-5400 Octafluoronaphthalene, OFN, 1 pg/µL 5188-5348 Octafluoronaphthalene, OFN, 100 fg/µL 5188-5347 OFN, 10 fg/µL 5190-0585 PFHT, 100 pg/µL 5188-5357 PFTBA, 10 g 8500-0656 PFTBA sample kit 05971-60571 PFDTD calibrant 8500-8510 Foreline pump tray (Pfeiffer pump) G1099-00015 Duo 2.5s and DS-42 foreline pump oil pan G3870-00015 Eval A, hydrocarbons 05971-60045 Ion gauge electronics G3870-80030 Methane/isobutane gas purifier G1999-80410 www.agilent.com Agilent Technologies, Inc. 2019 First edition, January 2019 *G7077-90035* G7077-90035
