Agilent 6000 Series LC/MS System - UNT Chemistry

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Agilent 6000 SeriesLC/MS SystemMaintenance Guide

Notices Agilent Technologies, Inc. 2014WarrantyNo part of this manual may be reproducedin any form or by any means (includingelectronic storage and retrieval or translation into a foreign language) without prioragreement and written consent from Agilent Technologies, Inc. as governed byUnited States and international copyrightlaws.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 applicablelaw, Agilent disclaims all warranties,either express or implied, with regardto this manual and any informationcontained herein, including but notlimited to the implied warranties ofmerchantability and fitness for a particular purpose. Agilent shall not beliable for errors or for incidental orconsequential damages in connectionwith the furnishing, use, or performance of this document or of anyinformation contained herein. ShouldAgilent and the user have a separatewritten agreement with warrantyterms covering the material in thisdocument that conflict with theseterms, the warranty terms in the separate agreement shall control.Manual Part NumberG2581-90017EditionRevision A, May 2014Agilent Technologies, Inc.5301 Stevens Creek Blvd.Santa Clara, CA 95051PatentsSome technology described in this guide iscovered by U.S. patents 6,107,628 and6,803,565 licensed from Battelle MemorialInstitute.Some Ion Mobility technology is covered bypatents US6,818,890; US6,967,325;US7,888,635.Note to CustomerThis product may be used as a componentof an in vitro diagnostic system if the system is registered with the appropriateauthorities and complies with the relevantregulations. Otherwise, it is intended onlyfor general laboratory use.Technology LicensesThe hardware and/or software described inthis document are furnished under alicense and may be used or copied only inaccordance with the terms of such license.Restricted Rights LegendU.S. Government Restricted Rights. Software and technical data rights granted tothe federal government include only thoserights customarily provided to end user customers. Agilent provides this customarycommercial license in Software and technical data pursuant to FAR 12.211 (TechnicalData) and 12.212 (Computer Software) and,for the Department of Defense, DFARS252.227-7015 (Technical Data - CommercialItems) and DFARS 227.7202-3 (Rights inCommercial Computer Software or Computer Software Documentation).Safety NoticesCAUTIONA CAUTION notice denotes a hazard. It calls attention to an operating procedure, practice, or the likethat, if not correctly performed oradhered to, could result in damageto the product or loss of importantdata. Do not proceed beyond aCAUTION notice until the indicated conditions are fully understood and met.WAR NINGA WARNING notice denotes ahazard. It calls attention to anoperating procedure, practice, orthe like that, if not correctly performed or adhered to, could resultin personal injury or death. Do notproceed beyond a WARNINGnotice until the indicated conditions are fully understood andmet.

In This Guide This book contains procedures to clean and maintain yourAgilent 6000 Series LC/MS instrument. This book applies to all6100 Series, 6200 Series, 6400 Series and 6500 Series LC/MSinstruments.1Startup and ShutdownThis chapter describes how to start up and shut down yourLC/MS System.2Calibrant Delivery System and Divert ValveThis chapter describes maintenance tasks for the calibrantdelivery system (CDS) and divert valve.3SourcesThis chapter describes maintenance procedures for thecomponents that make up the source.4Ion Transfer CapillaryThis chapter describes the procedures to remove, clean andreinstall the ion transfer capillary. These procedures apply toboth single- and multi-bore capillaries.5High Pressure Ion FunnelWith time and with heavy usage, the high pressure ion funnelneeds to be cleaned to maintain its performance on the LC/MSinstrument.6Desolvation Assembly and Vacuum ManifoldThis chapter describes the steps to maintain the assemblies thatare inside of the vacuum manifold. For most procedures, thedesolvation assembly needs to be removed to get to the vacuummanifold.6000 Series LC/MS Maintenance Guide3

7Vacuum SystemThis chapter includes procedures to maintain the vacuumsystem of the instrument. Do these steps according to themaintenance schedule or as indicated by instrument symptoms.8ReferenceThis chapter contains safety information, parts lists, and otherreference information for your Agilent 6000 Series LC/MS.46000 Series LC/MS Maintenance Guide

Content1Startup and Shutdown9To start the system in Standby modeTo change between Standby and OnTo shut down the instrument 15Instrument Overview 16Service Area2221214Calibrant Delivery System and Divert Valve25To prepare tuning mix30To prepare the reference mass solution 35To check calibrant levels 39To fill a calibrant bottle (6100 Series)40To fill a calibrant bottle (6200 Series, 6400 Series, and 6500 SeriesLC/MS)42To flush the calibrant delivery system 43To check for leaks 45To replace the inlet filter assembly 46To replace the MS selection valve rotor seal 483Sources51Changing Ion Sources 53To remove an electrospray or Agilent Jet Stream source53To remove a multimode source 54To remove an APCI or APPI source 54To install an electrospray or Agilent Jet Stream source 55To install an APCI source57To install an APPI source 58To install the HPLC-Chip/MS interface 59Source Maintenance 60To flush the nebulizer 606000 Series LC/MS Maintenance Guide5

ContentsTo clean the spray chamber daily61To clean the spray chamber weekly65To remove the nebulizer69To inspect the nebulizer70To adjust or replace the nebulizer needleTo install the nebulizer 79To clean the corona needle 80To replace the corona needle82To change HPLC-Chip capillaries844Ion Transfer Capillary7389To remove the capillary 90To clean the capillary 92To install the capillary 945High Pressure Ion Funnel97To remove the high pressure ion funnel 98To clean the high pressure ion funnel 100To install the high pressure ion funnel1036Desolvation Assembly and Vacuum Manifold105Desolvation Assembly 106To remove the desolvation assembly 106To install the desolvation assembly 109Vacuum Manifold Cover 110To open the vacuum manifoldTo close the vacuum manifold110111Ion Optics Assembly 112To clean skimmer 1112To remove the ion optics assembly (6200 Series) 114To clean the ion optics assembly (6200 Series) 11766000 Series LC/MS Maintenance Guide

ContentsTo remove the ion optics assembly (6100 Series, 6400 Series, and 6500Series) 125To clean the ion optics assembly (6100 Series, 6400 Series and 6500Series) 127Beam-shaping assembly137To remove and clean the complete beam shaping assemblyTo clean the beam-shaping slicer parts 148137Electron Multiplier152To replace the electron multiplier horn 152To clean the high energy dynode 1547Vacuum System157To check the rough pump fluid level (Agilent MS40 ) 158To add rough pump fluid (Agilent MS40 ) 159To replace the rough pump fluid (Agilent MS40 ) 162To replace the fuses 164To bake out the LC/MS 1668Reference167Safety 168Symbols on instruments168General instrument safety 170Physical hazard safety171General chemical safety 174Chemical waste safety175Conformity and Standards 176Safety and Regulatory Certifications176Electromagnetic Compatibility 177Sound Emission Declaration178Environmental Conditions178Tools and PartsTools 1796000 Series LC/MS Maintenance Guide1797

ContentsParts and Supplies81816000 Series LC/MS Maintenance Guide

Agilent 6000 Series LC/MS SystemMaintenance Guide1Startup and ShutdownTo start the system in Standby mode 12To change between Standby and On 14To shut down the instrument 15Instrument Overview 16Service Area 22This chapter describes how to start up and shut down your LC/MS System.For more details, see the site preparation guide that is sent to customersbefore installation. If you move the instrument, you must follow and repeat thesteps detailed in the site preparation guide.WARN I NGAlways wear appropriate protection, including eye protection, lab coat, and gloves,when working with solvents and chemicals or when working with unassembledparts.9

1Startup and ShutdownThe LC/MS System instruments have three standard modes of operation thatyou can select from the software.On ModeOn is the fully operational status of the system. The instrument and the sourceare on. The LC/MS instrument icon indicates the state of the instrument:Table 1Instrument icon color indicationColorStategreenidlebluerunning, injectingrederroryellownot readypurplepre-run, post-rundark grayofflinelight graystandbyRefer to the online Help to learn how to put the instrument in On mode.Standby ModeIn Standby, the source interface is on, the drying gas remains heated, andnebulizer flows are maintained. The source and ion optics voltages are turnedoff, and the mass spectrometer is not sending spectra to the computer.However, the LC/MS high voltage electronics are on.For APCI and multimode sources: The vaporizer gas heaters are reduced.For an instrument with Agilent Jet Stream source: The sheath gastemperature, drying gas flow, and drying gas temperatures are reduced.This mode lets the instrument remain idle for periods lasting from minutes todays. You should place the instrument in Standby mode when it is not in useor when you want to change the ion source.Refer to the online Help to learn how to put the instrument in Standby mode.Powered OffState10When the system is in the powered off state, the system is vented and theinstrument is turned off to allow maintenance or to prepare for long periodswhen the instrument is not used.6000 Series LC/MS Maintenance Guide

Startup and Shutdown1Note that the only way to completely remove electrical power from the systemis to unplug all power cords from the instrument.NOTEBefore you move the instrument to another location, maintain it, or expect it to be idle forlong periods of time, turn off both the front switch and the main power breaker switchbehind the service panel.CA U T I O NIf the LC/MS System is planned to be shut down for longer than one day, unplug theinstrument from the wall outlet to prevent overheating of the turbo pump powersupplies.6000 Series LC/MS Maintenance Guide11

1Startup and ShutdownTo start the system in Standby modeTo start the system in Standby modeThis procedure brings the system from the powered off state to Standby mode.1 Check that nitrogen gas for the drying gas is turned on. If equipped with acollision cell, check that nitrogen gas for the collision cell is turned on.When you use an Agilent Jet Stream source (single or dual nebulizer), thenitrogen gas requirements are greater than when operating withelectrospray, APCI, APPI, or multimode sources. The supply line must havetwo gas filters (part number BHT-4 or RMSN-4) plumbed in parallel toachieve these flows without triggering errors at the instrument. Refer to theInstallation Guide for more details.2 Check that the rough pump is properly connected to the LC/MS instrument.a Check that rough pump power cable is connected to the Foreline Pumppower receptacle.For instruments without a pump expander box: The Foreline Pumppower receptacle is behind the service panel.b For instruments with an ion funnel: Check that the ion funnel pump isconnected to the Auxiliary Pump power receptacle in the pumpexpander box.c Check that the LC/MS mainframe pump has the correct voltage rating foryour AC power (200 to 240 VAC).d Check that the rough vacuum hose is connected to the inlet port of therough pump.e For instruments with an ion funnel: Check that the ion funnel roughvacuum hose is connected to the ion funnel rough pump inlet.f Check that the switch on the rough pump (or pumps) is in the Onposition.3 Check that all foreline and ion funnel pumps and the spray chamberexhaust are vented outside the laboratory.WARN I NG12Vent all exhausts external to the building where they cannot be recirculated byenvironmental control systems. Do not vent exhaust into your laboratory. Theexhaust fumes from the vacuum pumps and spray chamber contains trace amountsof the chemicals you analyze. Health hazards include chemical toxicity fromsolvents, buffers, samples and pump fluid vapor, as well as potentially biohazardousaerosols of biological samples.6000 Series LC/MS Maintenance Guide

Startup and ShutdownTo start the system in Standby modeCA U T I O N1Do not connect the spray chamber exhaust bottle to the rough pump exhaust tubing orthe rough pump exhaust tubing to the spray chamber exhaust tubing. Doing so cancontaminate the instrument with rough pump fluid.4 Turn on the power for the computer and monitor.5 Check that the instrument is plugged into a power outlet.6 For instruments with a pump expander box only: Check that the powerswitch on the pump expander box is connected to the wall outlet and isturned on. The switch is illuminated green when the power is on.7 Turn on the front power switch of the LC/MS System.This starts the pumping system and the electronics.8 For the 6200 Series and 6500 Series LC/MS instruments only: In theTOF/Q-TOF Diagnostics program, connect to the system. Select the PumpDown and HV Condition options.The system monitors the vacuum pressure. Once the vacuum pressurereaches 3 10-6 Torr, the system begins to condition the high voltageelectronics.When high voltage conditioning is complete, close the Diagnostics program.9 Start the data acquisition program.The system comes up in Standby mode.NOTEFor the 6200 Series and 6500 Series LC/MS instruments only: You will not be able to setthe flows while the LC/MS system is in a “Not Ready” state. The system will remain inthe Not Ready state while the high vacuum pressure is above 3.5 10-6 Torr.10 For the 6200 Series and 6500 Series LC/MS instruments only: Let theinstrument continue to pump down.The Rough Vac (rough pump) pressure should be about 1.75 to 3.5 Torr,depending on the instrument type. The TOF Vac (flight assembly region)pressure reaches approximately 3 10-6 Torr within two to three hours. TheTOF Vac reading reaches the 10-7 Torr range after pumping overnight toseveral days.Leave the instrument in Standby.6000 Series LC/MS Maintenance Guide13

1Startup and ShutdownTo change between Standby and OnTo change between Standby and OnUse this procedure when: The LC/MS System is in Standby mode and you need to bring it into theOn mode. Sample analysis is complete and you want to put the LC/MS instrumentin Standby mode.Before you change the state from On to Standby: Check that you have completed tuning and data acquisition and you havesaved all data as needed (described in later chapters). In the data acquisition program, right-click the instrument icon, and thenchange the instrument state to Standby or On.Refer to the online Help.You can only activate the Standby mode or On mode if the ion source ismounted and closed. You can now select parameters for your measurement.In Standby mode: The drying gas flow, drying gas temperature, nebulizer pressure,vaporizer temperature, and sheath gas temperature are reduced. The spray chamber high voltages are turned off. For 6200 Series and6500 Series LC/MS instruments, voltages in the flight tube remain On tomaintain stable operating voltages. The mass spectrometer stops generating spectra.146000 Series LC/MS Maintenance Guide

Startup and ShutdownTo shut down the instrument1To shut down the instrumentYou can turn off the LC/MS System when the instrument will be idle for anextended time or when you must do maintenance.Before you begin, check that you have completed tuning and acquiring data,and that you have saved all data as needed.CA U T I O NWhen you vent the system from the data acquisition program, the LC/MS instrumentdoes not turn off. You must follow the entire shutdown procedure.WARN I NGThe spray shield and related spray chamber components are likely to be hot. Do nottouch them!1 Turn off the solvent flow.If you have analyte in any of the components in the sample delivery system,flush the delivery system with pure solvent before you continue.2 If equipped with a ballast valve, check that the ballast valve on the roughpump is closed.3 From the data acquisition program, vent the system.When you vent the system, these parts are turned off: spray chamber highvoltages, the drying gas heater, the nebulization flow, the detector, andother lens voltages. The drying gas flow is set to 3.5 L/minute. If the APCIsource is installed, the vaporizer heater is also turned off. If the installedsource is an Agilent Jet Stream source, the sheath gas heater is also turnedoff. The Rough Pump turns off when the turbo speed is below 20 percent.4 Wait until the instrument completely vents (reaching 760 Torr).For 6200 Series and 6500 Series LC/MS instruments: This step ensuresthat the flight tube is filled with nitrogen to protect the detector frommoisture damage.5 Turn off the front switch located in the lower left front corner of theinstrument.6 Unplug the main power cable behind the service panel. If the instrument isequipped with a pump expander box, also unplug the pump expander cablebehind the service panel.6000 Series LC/MS Maintenance Guide15

1Startup and ShutdownInstrument OverviewDo this to completely remove power from the instrument and to prevent thepower supplies within the instrument from overheating.You can also shut down the data acquisition program and computer.The system is now shut down.Instrument OverviewThese figures show you where the various switches, covers, and external partsare located.6100 SeriesCDS coverright sidecoverion sourceleft side cover (notshown)front coverpower switchFigure 116Standard 6100 Series cover design.6000 Series LC/MS Maintenance Guide

Startup and ShutdownInstrument Overview16200 Seriesflight assemblyservice panelion sourcefront coverCDS coverpower switchFigure 2Standard 6200 Series LC/MS cover design. The main power switch is locatedon the front lower left.6000 Series LC/MS Maintenance Guide17

1Startup and ShutdownInstrument Overview6400 Series and 6500 SeriesThese figures show the 6400 Series and 6500 Series LC/MS instruments. 6400Series share the same base unit design as the 6500 Series, except for theinclusion of a flight assembly.flightassemblyservice panelion sourcefront coverCDS coverpower switchFigure 3186400 Series (inset) and 6500 Series LC/MS system. The main power switch is behind the servicepanel.6000 Series LC/MS Maintenance Guide

Startup and ShutdownInstrument Overview1flightassemblyion sourceservice panelfront coverCDS coverpower switchFigure 46400 Series (inset) and 6500 Series LC/MS system.6000 Series LC/MS Maintenance Guide19

1Startup and ShutdownInstrument Overviewflight assemblyion sourcefront coverservice panelCDS bottlespower switchFigure 5206400 Series (inset) and 6500 Series LC/MS with an iFunnel ion funnel6000 Series LC/MS Maintenance Guide

Startup and ShutdownInstrument Overview1flightassemblyIM chassision sourceservice panelfrontcoversCDS bottlespower switchFigure 6Ion Mobility Q-TOF LC/MS6000 Series LC/MS Maintenance Guide21

1Startup and ShutdownService AreaService AreaThese pictures show you where various connectors are located.LAN connectionFigure 722Gas, LAN, and power connections behind service panel for the 6400 Seriesand 6500 Series instruments without a pump expander box,6000 Series LC/MS Maintenance Guide

Startup and ShutdownService Area1pump expander box powerswitchFigure 8Power connections and pump expander box behind service panel for 6400 Series and 6500 Series instruments with a pump expander box,6000 Series LC/MS Maintenance Guide23

opened service panelLAN connectionFigure 9Connections behind service panel for 6200 Series LC/MSThis page intentionally left blank.246000 Series LC/MS Maintenance Guide

Agilent 6000 Series LC/MS SystemM

6000 Series LC/MS Maintenance Guide 3 In This Guide This book contains procedures to clean and maintain your Agilent 6000 Series LC/MS instrument. This book applies to all 6100 Series, 6200 Series, 6400 Series and 6500 Series LC/MS instruments. 1 Startup and Shutdown This chapter describes how to start up and shut down your LC/MS System.

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