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Ionization techniques and source probes

March 14, 2014, 715004387 Rev. B

Ionization techniques and source probes

Note:

Available source options can vary depending on the software used to

operate the Xevo TQD. Refer to the MassLynx or UNIFI online Help for more

information about supported sources.

Electrospray ionization (ESI)

In electrospray ionization (ESI), a strong electrical charge is applied to the

eluent as it emerges from a nebulizer. The droplets that compose the resultant

aerosol undergo a reduction in size (solvent evaporation). As solvent continues

to evaporate, the charge density increases until the droplet surfaces eject ions

(ion evaporation). The ions can be singly or multiply charged.
The standard ESI probe accommodates eluent flow rates as high as 2 mL/min,

making it suitable for LC applications in the range 100 µL/min to 2 mL/min.
See

page 58

for further details.

Combined ESI and APCI (ESCi)

Combined electrospray ionization and atmospheric pressure chemical

ionization (ESCi) is supplied as standard equipment on the mass

spectrometer. In ESCi, the standard ESI probe is used in conjunction with a

corona pin to allow alternating acquisition of ESI and APCI ionization data,

facilitating high throughput and wider compound coverage.
See

page 62

for further details.

Atmospheric pressure chemical ionization (APCI)

A dedicated high-performance APCI interface is offered as an option. APCI

produces singly charged protonated or deprotonated molecules for a broad

range of nonvolatile analytes.
The APCI interface consists of the ESI/APCI/ESCi enclosure fitted with a

corona pin and an IonSABRE II probe.
See

page 62

for further details.

Содержание Xevo TQD

Страница 2: ...ii March 14 2014 715004387 Rev B...

Страница 3: ...document consult the Waters Web site waters com Trademarks ACQUITY ACQUITY UltraPerformance LC ACQUITY UPLC Alliance Connections INSIGHT ESCi MassLynx nanoACQUITY nanoACQUITY UPLC nanoTile THE SCIENC...

Страница 4: ...emoval or disposal of any Waters product You can reach us via the Internet telephone or conventional mail Safety considerations Some reagents and samples used with Waters instruments and devices can p...

Страница 5: ...nalysis assuming a maximum leak into the laboratory atmosphere of 10 LC eluate Warning To avoid electric shock use the SVT type power cord in the United States and HAR type or better in Europe The mai...

Страница 6: ...ge caused by spilled solvent do not place reservoir bottles on top of the instrument or on its front ledge unless in the bottle tray provided Warning To prevent ignition of flammable solvent vapors in...

Страница 7: ...exposure to toxic or biohazardous substances never place containers on top of the instrument or on its front covers Warning To avoid burn injuries ensure the source heater is turned off and the ion bl...

Страница 8: ...of decontamination to be used and the appropriate protection for personnel undertaking the decontamination process You must handle items such as syringes fused silica lines and borosilicate tips used...

Страница 9: ...ice may not cause harmful interference and 2 this device must accept any interference received including interference that may cause undesired operation Electrical power safety notice Do not position...

Страница 10: ...Symbol Definition Manufacturer Date of manufacture Part number catalog number Serial number Supply ratings Authorized representative of the European Community Confirms that a manufactured product com...

Страница 11: ...pment with this symbol may contain hazardous substances and should not be disposed of as general waste For compliance with the Waste Electrical and Electronic Equipment Directive WEEE 2012 19 EU conta...

Страница 12: ...follow acceptable calibration methods using at least five standards to generate a standard curve The concentration range for standards should include the entire range of QC samples typical specimens a...

Страница 13: ...1 ISM Classification ISM Group 1 Class A This classification has been assigned in accordance with CISPR 11 Industrial Scientific and Medical ISM instrument requirements Group 1 products apply to inten...

Страница 14: ...h 14 2014 715004387 Rev B EC authorized representative Waters Corporation Stamford Avenue Altrincham Road Wilmslow SK9 4AX United Kingdom Telephone 44 161 946 2400 Fax 44 161 946 2480 Contact Quality...

Страница 15: ...ty advisories ix Operating this instrument x Applicable symbols x Audience and purpose xii Intended use of the Xevo TQD xii Calibrating xii Quality control xii EMC considerations xiii Canada spectrum...

Страница 16: ...System operation 35 Ion optics 36 MS operating modes 37 MS MS operating modes 38 Product daughter ion mode 39 Precursor parent ion mode 40 Multiple reaction monitoring mode 40 Constant neutral loss m...

Страница 17: ...62 APCI mode 62 Installing the IonSABRE II probe 63 Removing the IonSABRE II probe 65 Combined APPI APCI source 66 APPI operation 66 APCI operation 67 Dual mode operation 68 The combined APPI APCI so...

Страница 18: ...n from the source 95 Operating the source isolation valve 96 Removing O rings and seals 99 Cleaning the instrument case 100 Emptying the exhaust trap bottle 100 Gas ballasting the roughing pump 102 Ga...

Страница 19: ...bly 137 Cleaning the ion guide assembly 140 Removing the differential aperture from the ion guide 142 Fitting the differential aperture to the ion guide assembly 144 Fitting the ion guide assembly to...

Страница 20: ...189 APPI APCI source replacing the APPI lamp drive seals 191 Removing the APPI lamp drive assembly seals 191 Fitting the new APPI lamp drive assembly O rings 197 Replacing the instrument s fuses 199...

Страница 21: ...g the liquid waste line 233 Connecting the workstation 235 Connecting Ethernet cables 236 I O signal connectors 237 Signal connections 238 Connecting to the power supply 241 C Materials of Constructio...

Страница 22: ...xxii March 14 2014 715004387 Rev B...

Страница 23: ...uding its controls and connections for gas and plumbing Contents Topic Page Uses and compatibility 24 Ionization techniques and source probes 31 IntelliStart Fluidics system 34 Ion optics 36 MS operat...

Страница 24: ...ation ESI APCI ESCi source Requirement Dedicated APCI operation requires an additional probe IonSABRE II Optional dual mode APPI APCI source Optional NanoFlow ESI source Optional TRIZAIC UPLC source O...

Страница 25: ...tart technology monitors LC MS MS performance and reports when the instrument is ready for use The software automatically tunes and mass calibrates the instrument displays performance readbacks and en...

Страница 26: ...e ACQUITY Xevo TQD UPLC MS system includes an ACQUITY UPLC ACQUITY UPLC H Class or ACQUITY UPLC I Class system and the Waters Xevo TQD fitted with the ESI APCI ESCi source The nanoACQUITY Xevo TQD UPL...

Страница 27: ...ocuments on http www waters com click Services and Support Support Library System Core components ACQUITY UPLC Binary solvent manager Sample manager Column heater UPLC detectors Solvent tray ACQUITY U...

Страница 28: ...tween 0 20 and 5 00 L min With open loop control and nanoACQUITY UPLC columns of internal diameters ranging from 75 m to 1 mm the flow rates can extend to 100 L min The column hardware and the matched...

Страница 29: ...2777 autosampler Spark Holland Symbiosis system Software and data system MassLynx v4 1 or UNIFI software can control the mass spectrometer See page 30 for more information about those applications Bot...

Страница 30: ...rmation about using MassLynx software You configure settings monitor performance run diagnostic tests and maintain the system and its modules via the MassLynx Instrument Console application The Instru...

Страница 31: ...accommodates eluent flow rates as high as 2 mL min making it suitable for LC applications in the range 100 L min to 2 mL min See page 58 for further details Combined ESI and APCI ESCi Combined electr...

Страница 32: ...e concentration the ion currents observed approximate those seen in normal flow rate electrospray However for similar experiments NanoFlow s significant reduction in sample consumption accompanies sig...

Страница 33: ...hromatography APGC The Waters APGC couples an Agilent GC with the Xevo TQD making it possible to perform LC and GC analyses in the same system without compromising performance The APGC provides comple...

Страница 34: ...se smaller volumes see page 52 The reservoirs can also deliver sample through direct or combined infusion to enable optimization at analytical flow rates From a wash reservoir that contains solvent fo...

Страница 35: ...tions between the fluidics components to carry out the operations processed by the software You can set IntelliStart fluidics configuration requirements in the system console You can edit the paramete...

Страница 36: ...an be filtered according to their mass to charge ratios 4 The mass separated ions pass into the T Wave collision cell where they either undergo collision induced dissociation CID or pass to the second...

Страница 37: ...ed ion recording SIR mode for quantitation when you cannot find a suitable fragment ion to perform a more specific multiple reaction monitoring MRM analysis see page 38 In SIR and MRM modes neither qu...

Страница 38: ...tatic at precursor mass Fragment precursor ions and pass all masses Scanning Precursor parent ion spectrum Scanning Static at product mass MRM Static at precursor mass Static at product mass PICS Prod...

Страница 39: ...t ion mode Typical applications Product ion mode is typically used for the following applications Method development for MRM screening studies Identifying product ions for use in MRM transitions Optim...

Страница 40: ...MS MS equivalent of SIR Because both MS1 and MS2 are static greater dwell time on the ions of interest is possible so the sensitivity achieved is better compared with scanning mode MS MS This mode is...

Страница 41: ...de the background for all other components This enables fast characterization of potential matrix effects providing a platform for more robust method development Typical application You typically use...

Страница 42: ...s If it does the loss registers at the detector In constant neutral loss mode the spectrum shows the masses of all precursors that actually lost a fragment of a certain mass Constant neutral loss mode...

Страница 43: ...he ACQUITY UPLC Console or UNIFI software displays an error message alerting you that a leak has developed See Waters ACQUITY UPLC Leak Sensor Maintenance Instructions for complete details Vacuum syst...

Страница 44: ...following figure shows the rear panel locations of the connectors used to operate the instrument with external devices Instrument rear panel Power Source vent Turbo vacuum Nitrogen inlet Collision cel...

Страница 45: ...ration This chapter describes how to start and shut down the instrument Contents Topic Page Starting the mass spectrometer 46 Preparing the IntelliStart Fluidics system 52 Rebooting the instrument 54...

Страница 46: ...e rear panel ensure the nitrogen supply is connected to the instrument s nitrogen inlet connection see the figure on page 44 Requirement The nitrogen must be dry and oil free with a purity of at least...

Страница 47: ...to initialize and to sound an alert indicating that the PC is ready Tip The power and status LEDs change as follows Each system instrument s power LED shows green During initialization the binary or...

Страница 48: ...which the turbopump is starting the roughing pump starts IntelliStart displays Instrument in standby and the Operate LED remains off c Wait a minimum of 2 hours for the instrument to be fully pumped d...

Страница 49: ...mode and the Operate LED remains off c Wait a minimum of 2 hours for the instrument to be fully pumped down evacuated Tip In the Instrument Summary pane the Status indicator shows green when the instr...

Страница 50: ...tatus Power LED The power LED to the top right hand side of the mass spectrometer s front panel indicates when the instrument is powered on or powered off Operate LED The Operate LED on the right hand...

Страница 51: ...e according to the following table If you are using an APCI interface IntelliStart software automatically sets the parameters according to the following table Flow rate versus temperature and gas flow...

Страница 52: ...ndard reservoir bottles 15 mL for instrument setup and calibration Use the Low volume Adaptor Kit sold separately to infuse smaller volumes The low volume vials have a volume of 1 5 mL Required materi...

Страница 53: ...o the manifold and tighten it 3 Screw the low volume vial into the adaptor 4 For each low volume vial ensure that the end of the solvent delivery tube is positioned so that it is close to but does not...

Страница 54: ...strument s solvent delivery system can require more than one purge cycle to minimize carryover Rebooting the instrument The reset button causes the mass spectrometer to reboot Reboot the instrument wh...

Страница 55: ...ource When leaving the mass spectrometer unused for a long period In these instances put the mass spectrometer in Standby mode See the online Help for details Emergency shutdown of the mass spectromet...

Страница 56: ...2 Preparing for Operation 56 March 14 2014 715004387 Rev B...

Страница 57: ...chemical ionization Combined Atmospheric Pressure Photoionization APPI APCI NanoFlow For details about other Waters and third party source options refer to the documentation supplied with the source...

Страница 58: ...inside its source 2 Remove the protective sleeve if fitted from the ESI probe tip Warning To avoid personal contamination with biohazards or toxic materials and to avoid spreading contamination to unc...

Страница 59: ...assembly 4 Tighten the probe locking ring to secure the probe in place Requirement Fully tighten the probe locking ring Doing so ensures a successful result on the automatic pressure test which runs...

Страница 60: ...low rates 1 2 mL min Requirements If you are replacing the tubing between the selector valve and the probe minimize the length to reduce peak broadening When cutting the tubing to length cut it square...

Страница 61: ...probe from the probe adjuster assembly 6 If available fit the protective sleeve to the ESI probe tip Warning To avoid personal contamination with biohazards or toxic materials and to avoid spreading c...

Страница 62: ...mode an option for the mass spectrometer produces singly charged protonated or deprotonated molecules for a broad range of nonvolatile analytes The APCI interface consists of the ESI APCI ESCi enclos...

Страница 63: ...instrument for working on the source see page 88 2 With the probe label facing toward you carefully slide the IonSABRE II probe into the hole in the probe adjuster assembly ensuring that the probe loc...

Страница 64: ...flow rates 1 2 mL min use 0 005 inch ID tubing for sample flow rates 1 2 mL min Requirements If you are replacing the tubing between the selector valve and the probe minimize the length to reduce peak...

Страница 65: ...g ring 5 Carefully remove the probe from the probe adjuster assembly Warning To avoid personal contamination with biohazards or toxic materials and to avoid spreading contamination to uncontaminated s...

Страница 66: ...advanced into the source APPI mode The IonSABRE II probe introduces vaporized sample into the source where photons generated by an ultraviolet UV lamp mounted in the APPI lamp drive assembly produce s...

Страница 67: ...introduces vaporized sample into the source The sample passes between the sample cone and the corona pin which typically operates with a discharge current of 5 A The corona discharge generates ions th...

Страница 68: ...for dual operation When the source is configured for dual operation in APCI mode current is applied to the corona pin but the repeller electrode is inactive Dual operation in APCI mode When the source...

Страница 69: ...comprises the standard IonSABRE II probe and a source enclosure with an APPI lamp drive incorporated The combined APPI APCI source enclosure Notice To prevent damage to the corona pin and lamp assemb...

Страница 70: ...ne window provides a constant photon output You vary the intensity of incident radiation upon the sample molecules by adjusting the distance between the UV lamp and probe tip APPI lamp drive assembly...

Страница 71: ...ce enclosure see page 92 5 Install the corona pin see page 93 6 Connect the APPI drive cable to the instrument s front panel connector Warning To avoid personal contamination with biohazards or toxic...

Страница 72: ...front panel 4 Disconnect the APPI drive cable from the instrument s front panel 5 Remove the source enclosure see page 90 Notice To prevent damage to the corona pin and lamp assembly ensure that the l...

Страница 73: ...comprises the NanoFlow stage for x axis y axis and z axis adjustment the sprayer enclosure and a microscope camera NanoFlow source stage and microscope camera A sprayer is mounted on an X Y Z stage th...

Страница 74: ...e page 61 If you are removing an IonSABRE II probe see page 65 3 Remove the existing source enclosure see page 90 Warning To avoid personal contamination with biohazards or toxic materials and to avoi...

Страница 75: ...unted beneath the stage on the front of the NanoFlow source and your sprayer Tip For details regarding how to fit each sprayer see the corresponding reference Waters Universal NanoFlow Sprayer Install...

Страница 76: ...age cable to the instrument s HV connection Tip The NanoFlow stage contains a high voltage interlock so the capillary voltage the voltage applied to the sprayer assembly and the sampling cone voltage...

Страница 77: ...tage out of the NanoFlow source enclosure and remove the magnetic cover 4 Unscrew the retaining screw and lift the sprayer from the stage Warning To avoid lacerations puncture injuries and possible co...

Страница 78: ...capillary from the sprayer 7 Carefully remove the new borosilicate glass capillary from its case by lifting vertically while pressing on the foam with two fingers 8 Load sample into the capillary usin...

Страница 79: ...the capillary 10 Fit the capillary into the holder probe 11 Finger tighten the nut so that 5 mm of glass capillary protrude from its end Tip Measure the protrusion from the end of the nut to the shoul...

Страница 80: ...n For tuning instructions see the instrument s online help Restarting a stalled borosilicate glass capillary electrospray Should the spray stop you can restart it To do so in the MassLynx Tune window...

Страница 81: ...n or inside its source 88 Removing and refitting the source enclosure 90 Installing and removing the corona pin 93 Operating the source isolation valve 96 Removing O rings and seals 99 Cleaning the in...

Страница 82: ...e heater 167 Replacing the ion block source heater 170 Replacing the source assembly seals 174 Replacing the air filter 178 Replacing the roughing pump oil 180 Replacing the roughing pump s oil demist...

Страница 83: ...equired See page 100 Replace the oil free scroll pump s seals Annually See Edwards document XDS35i Instruction Manual A730 01 880 Gas ballast the roughing pump ESI weekly See page 102 Inspect and adju...

Страница 84: ...ona pin APCI and ESCi modes When the corona pin is corroded or black or the sensitivity decreases to unacceptable levels See page 166 Replace the IonSABRE II probe heater Options using the IonSABRE II...

Страница 85: ...Annually Tip Applications that contaminate the roughing pump oil reduce this period which must be determined from experience See page 183 Clean the APPI APCI source UV lamp window When the window bec...

Страница 86: ...collaboration option that controls the two way connection with the ACQUITY UPLC system by enabling the Connections INSIGHT iAssist service level Consult these sources for more information about Connec...

Страница 87: ...ging tubing or operating the instrument Know the physical and chemical properties of the solvents used see the Material Safety Data Sheets for the solvents in use Warning To avoid electric shock do no...

Страница 88: ...ent for operations on or inside its source 1 In the Instrument Console click Stop Flow to stop the LC flow or if column flow is required divert the LC flow to waste as follows a In the Instrument Cons...

Страница 89: ...C flow to waste as follows a On the Setup pane click Fluidics b On the Sample Fluidics page from the Flow Path menu select Waste 2 Click Instrument Standby Mode and confirm that the Operate indicator...

Страница 90: ...the source If you are removing an ESI probe see page 61 If you are removing an IonSABRE II probe see page 65 3 Disconnect the probe adjuster and options cables from the instrument s connectors 4 Pull...

Страница 91: ...ands grasp the source enclosure and lift it vertically off the two supporting studs on the source adaptor housing 6 Store the cables neatly by plugging them into the cable storage positions on the rea...

Страница 92: ...nt s connectors Warning To avoid personal contamination with biologically hazardous or toxic materials and to avoid spreading contamination to uncontaminated surfaces wear clean chemical resistant pow...

Страница 93: ...re Warning To avoid personal contamination with biologically hazardous or toxic materials and to avoid spreading contamination to uncontaminated surfaces wear clean chemical resistant powder free glov...

Страница 94: ...Store the blanking plug in a safe location Corona pin mounting contact 4 Fit the corona pin to the mounting contact ensuring that the corona pin is securely mounted Corona pin Warning To avoid punctur...

Страница 95: ...page 95 Tip Store the corona pin in a safe location 4 Fit the blanking plug to the corona pin mounting contact see the figure on page 94 5 Close the source enclosure Warning To avoid personal contamin...

Страница 96: ...he enclosure Warning To avoid personal contamination with biohazards or toxic materials and to avoid spreading contamination to uncontaminated surfaces wear clean chemical resistant powder free gloves...

Страница 97: ...horizontal position Warning To avoid personal contamination with biohazards or toxic materials and to avoid spreading contamination to uncontaminated surfaces wear clean chemical resistant powder fre...

Страница 98: ...4 Maintenance Procedures 98 March 14 2014 715004387 Rev B 2 Close the source enclosure TP03130 Isolation valve handle in open position...

Страница 99: ...O ring 1 Use the forked end of tool 1 to impale the O ring or seal 2 Pull the O ring or seal from its groove if necessary use tool 2 as an aid 3 Dispose of the O ring or seal in accordance with local...

Страница 100: ...Emptying the exhaust trap bottle Inspect the exhaust trap bottle in the instrument s exhaust line daily and empty it before it is more than 10 full Nitrogen exhaust trap bottle Notice To avoid damagin...

Страница 101: ...rap bottle to the cap 6 Secure the nitrogen exhaust trap bottle in the upright position 7 Close the source enclosure Tip A leak test runs automatically If the test results in a failure ensure that the...

Страница 102: ...ors tend to condense in the pump oil diminishing pumping efficiency Gas ballasting purges condensed contaminants from the oil Note This procedure is not required for an oil free roughing pump Roughing...

Страница 103: ...103 A handle operated gas ballast valve See page 105 Gas ballasting a pump fitted with a screwdriver operated gas ballast valve Required material Flat blade screwdriver Notice To avoid shortening the...

Страница 104: ...er turn to the open position 2 Run the pump for 30 to 60 minutes Tip It is normal for the roughing pump temperature to increase during ballasting To maintain an ambient temperature of less than 40 C i...

Страница 105: ...To maintain an ambient temperature of less than 40 C in the space where the pump is located ensure the space is adequately ventilated 3 Move the gas ballast valve handle on the pump clockwise from th...

Страница 106: ...the oil level in the sight glass is lower when the pump is running than when it is stopped When the pump is running the oil level is typically at 30 to 60 of the maximum level Adding oil to the rough...

Страница 107: ...r plug is tightened the plug seals by means of an O ring Compression is controlled by the O ring groove depth in the plug Overtightening does not improve the plug seal it merely makes the plug difficu...

Страница 108: ...related causes for decreased signal intensity See page 109 If cleaning the sample cone and cone gas nozzles fails to increase signal sensitivity also clean the extraction cone See page 119 If cleanin...

Страница 109: ...nation to uncontaminated surfaces wear clean chemical resistant powder free gloves when working with the source components Warning To avoid electric shock before beginning this procedure prepare the i...

Страница 110: ...sampling cone assembly 90 degrees moving the handle from the vertical to the horizontal position 3 Slide the sampling cone assembly out of the ion block assembly Notice To avoid damaging the instrume...

Страница 111: ...nd cone extraction tool To disassemble the sampling cone assembly 1 Slide the collar to the end of the combined 2 5 mm Allen wrench and cone extraction tool Warning To avoid personal contamination wit...

Страница 112: ...ert the collar in the sample cone 3 Rotate the tool and collar counter clockwise and then lift them to remove the sample cone from the cone gas nozzle Notice To avoid damaging the fragile sample cone...

Страница 113: ...of deterioration or damage dispose of it in accordance with local environmental regulations 6 Unscrew and remove the PEEK cone gas nozzle handle from the cone gas nozzle Warning To avoid spreading co...

Страница 114: ...1 If the sample cone contains debris place a drop of formic acid on its aperture 2 Immerse the sample cone cone gas nozzle and cone gas nozzle handle in separate glass vessels containing 1 1 methanol...

Страница 115: ...in the ultrasonic bath for 10 minutes 5 Carefully remove the components from the vessels and blow dry them with inert oil free gas 6 Inspect each component for persisting contamination If contaminatio...

Страница 116: ...2 Carefully fit the sample cone into the cone gas nozzle 3 Fit the O ring into the groove created between the sample cone and cone gas nozzle Fit a new O ring if the old one has been disposed of Notic...

Страница 117: ...aminated surfaces wear clean chemical resistant powder free gloves when working with the source components Warning To avoid puncture wounds take great care while working with the source enclosure open...

Страница 118: ...the cone gas nozzle handle is oriented horizontally and at the top and then slide the sampling cone assembly into the ion block assembly 3 Grasp the cone gas nozzle handle and use it to rotate the sam...

Страница 119: ...Vent and shut down the mass spectrometer see the mass spectrometer s online Help for details 2 Close the source isolation valve see page 96 Warning To avoid personal contamination with biohazards or...

Страница 120: ...mbined 2 5 mm Allen wrench and cone extraction tool to unscrew the 4 captive screws that secure the ion block assembly 4 Remove the ion block assembly from the PEEK ion block support TP03130 Screws se...

Страница 121: ...llen wrench and cone extraction tool to loosen the captive screws securing the 2 PEEK extraction cone retainer clips and then rotate the retainer clips clear of the extraction cone Warning To avoid pe...

Страница 122: ...ve the extraction cone handle insulator from the extraction cone handle Notice To avoid damaging the extraction cone aperture take great care when removing it from the ion block To avoid damaging the...

Страница 123: ...gas for example nitrogen for drying air drying optional Wash bottle containing HPLC grade or better 1 1 methanol water Large beaker Warning To avoid personal contamination with biohazards or toxic mat...

Страница 124: ...nd then placing the vessels in the ultrasonic bath for 10 minutes 4 Carefully remove the extraction cone from the vessel and blow dry it using inert oil free gas 5 Inspect the extraction cone for pers...

Страница 125: ...to the source assembly Required materials Chemical resistant powder free gloves Combined 2 5 mm Allen wrench and cone extraction tool Warning To avoid personal contamination with biohazards or toxic...

Страница 126: ...nozzle and extraction cone fails to increase signal sensitivity Disassembling the source ion block assembly Required materials Chemical resistant powder free gloves Combined 2 5 mm Allen wrench and co...

Страница 127: ...s 4 Slide the sampling cone assembly out of the ion block assembly Notice To ensure correct operation of the ion block assembly after reassembly follow these guidelines Do not remove the sampling cone...

Страница 128: ...mm Allen wrench and cone extraction tool to loosen the 2 ion block cover plate captive securing screws 6 Remove the ion block cover plate 7 Grasp the isolation valve and pull it out of the ion block...

Страница 129: ...d 2 5 mm Allen wrench and cone extraction tool to loosen the captive PEEK terminal block securing screw 11 Use the needle nose pliers to grasp the PEEK terminal block and partially lift it out of the...

Страница 130: ...ly grasp the heat shrink tubing on the heater cartridge assembly and carefully slide it and the PEEK terminal block out of the ion block 13 Use the O ring removal kit to carefully remove the cover sea...

Страница 131: ...hole in the ion block blanking plug and then unscrew and remove the ion block blanking plug and associated seal 17 If the blanking plug seal shows signs of deterioration or damage dispose of it in ac...

Страница 132: ...ction cone retainer clips 19 Remove the extraction cone from the ion block Notice To avoid damaging the extraction cone aperture take great care when removing the extraction cone from the ion block To...

Страница 133: ...Chemical resistant powder free gloves Appropriately sized glass vessels in which to completely immerse components when cleaning Use only glassware not previously cleaned with surfactants HPLC grade o...

Страница 134: ...ltrasonic bath for 10 minutes 4 Carefully remove the components from the vessels and blow dry them using inert oil free gas Inspect each component for persisting contamination Requirement If contamina...

Страница 135: ...extraction cone seal to the ion block 2 Fit the extraction cone handle s insulator onto the extraction cone handle 3 Fit the extraction cone onto the ion block 4 Fit the 2 PEEK extraction cone retaine...

Страница 136: ...extraction tool to tighten the captive PEEK terminal block securing screw 11 Ensure that the grooves for the cover seal cone gas O ring and isolation valve O ring are free of dirt and debris Tip If c...

Страница 137: ...and use it to rotate the sampling cone assembly through 90 degrees 21 Fit the ion block assembly to the source assembly see page 125 Cleaning the ion guide assembly Clean the ion guide assembly if cle...

Страница 138: ...the adaptor housing and remove the ion block support 4 If any of the O rings show signs of deterioration or damage dispose of them in accordance with local environmental regulations Warning To avoid s...

Страница 139: ...of the ion guide and remove the guide from the adaptor housing Notice To avoid damaging the ion guide assembly when removing it from the source assembly do not grasp the ion guide by its metal lens p...

Страница 140: ...inert gas for example nitrogen for drying air drying optional HPLC grade or better 1 1 methanol water Wash bottle containing HPLC grade or better 1 1 methanol water Large beaker To clean the ion guide...

Страница 141: ...ow dry it using inert oil free gas 7 Inspect the ion guide assembly for persisting contamination Requirement If contamination is present do as follows a Use the wash bottle containing methanol to rins...

Страница 142: ...secure the differential aperture to the 3 supporting rods 2 Remove the differential aperture from the ion guide Notice To avoid a reduction in sensitivity remove and clean the differential aperture on...

Страница 143: ...ol water formic acid 4 Place the vessel in the ultrasonic bath for 30 minutes 5 If you used formic acid in the cleaning solution rinse the differential aperture by immersing it in a glass vessel conta...

Страница 144: ...ligns correctly with the ion guide assembly sight along the central axis of the ion guide from the ion entry side and confirm that the hole at the centre of the differential aperture is concentric wit...

Страница 145: ...n block support onto the source 1 Ensure that the grooves for the PEEK ion block support O rings are free from dirt and debris Warning To avoid personal contamination with biohazards or toxic material...

Страница 146: ...p To fit an O ring in its groove start fitting the O ring at the notch in the groove and then progressively work the ring into the groove in either direction from the notch 3 Fit the PEEK ion block su...

Страница 147: ...e gloves 7 mm wrench 10 mm wrench To remove the ESI probe tip and gasket 1 Remove the ESI probe from the source see page 61 Warning To avoid personal contamination with biohazards or toxic materials a...

Страница 148: ...ch 14 2014 715004387 Rev B 2 Use the 10 mm wrench to remove the probe tip Tip If the probe tip is difficult to remove use the 7 mm wrench in conjunction with the 10 mm wrench Probe tip 10 mm wrench Pr...

Страница 149: ...accordance with local environmental regulations 5 If the probe tip is damaged dispose of it in accordance with local environmental regulations Warning To avoid spreading contamination dispose of the...

Страница 150: ...mm wrench to tighten the probe tip 4 Use the nebulizer adjuster knob to adjust the capillary so that it protrudes by approximately 0 5 mm from the end of the probe 5 Fit the ESI probe onto the source...

Страница 151: ...ose pliers To remove the existing capillary 1 Remove the probe from the source see page 61 2 Retrieve the combined 2 5 mm Allen wrench and cone extraction tool from its storage location on the source...

Страница 152: ...ined 2 5 mm Allen wrench and cone extraction tool to remove the 3 screws retaining probe end cover 4 Remove the end cover and gasket from the probe assembly 5 Unscrew and remove the nebulizer adjuster...

Страница 153: ...March 14 2014 715004387 Rev B 153 6 Use the 10 mm wrench to remove the probe tip Tip If the probe tip is difficult to remove use the 7 mm wrench in conjunction with the 10 mm wrench Probe tip 10 mm w...

Страница 154: ...e 9 Unscrew and remove the knurled collar from the UNF coupling 10 Remove the knurled collar and conductive sleeve from the capillary 11 Use the 7 mm wrench to loosen the locknut Tip Use the 8 mm wren...

Страница 155: ...uired materials Chemical resistant powder free gloves Combined 2 5 mm Allen wrench and cone extraction tool 10 mm wrench Needle nose pliers LC pump HPLC grade or better 1 1 acetonitrile water Ferrule...

Страница 156: ...screw the connector into the PEEK union so that it is finger tight Rationale Doing so ensures a minimum dead volume when fitting the capillary 3 Fit the UNF coupling to the new capillary Warning To a...

Страница 157: ...e capillary 10 Tighten the knurled collar onto the UNF coupling 11 Perform a leak test by attaching the free end of the PEEK tubing to an LC pump and pumping 50 50 acetonitrile water through it at 1 m...

Страница 158: ...m Allen wrench and cone extraction tool to fit and tighten the 3 screws retaining the probe end cover 20 Return the combined 2 5 mm Allen wrench and cone extraction tool to its storage location on the...

Страница 159: ...further details To clean the IonSABRE II probe tip 1 On the Instrument Console system tree click Xevo TQD Manual optimization 2 On the Manual Optimization page click to stop the liquid flow 3 Click G...

Страница 160: ...ve the probe from the source see page 65 2 Retrieve the combined 2 5 mm Allen wrench and cone extraction tool from its storage location on the source adaptor housing 3 Use the combined 2 5 mm Allen wr...

Страница 161: ...e PEEK union UNF coupling assembly and capillary from the probe Tip The PEEK union used with the IonSABRE II probe is notched on one of its flats a feature that distinguishes it from the PEEK union us...

Страница 162: ...l regulations Installing the new capillary Required materials Chemical resistant powder free gloves Needle nose pliers 7 mm wrench Combined 2 5 mm Allen wrench and cone extraction tool Red PEEK tubing...

Страница 163: ...t connector and screw the connector finger tight into the PEEK union Rationale Doing so ensures a minimum dead volume when fitting the capillary 3 Fit the UNF coupling to the new capillary Requirement...

Страница 164: ...50 acetonitrile water through it at 1 mL min If leakage occurs disassemble and remake the connection and repeat the leak test If the backpressure on the LC pump is high replace the capillary and repea...

Страница 165: ...ch and cone extraction tool to fit and tighten the 3 screws retaining the probe end cover 20 Return the combined 2 5 mm Allen wrench and cone extraction tool in its storage location on the source adap...

Страница 166: ...g film and a methanol saturated tissue 3 Install the corona pin in the source see page 93 Warning To avoid personal contamination with biohazards or toxic materials and to avoid spreading contaminatio...

Страница 167: ...robe heater Required material Chemical resistant powder free gloves To remove the IonSABRE II probe heater 1 Remove the probe from the source see page 65 Warning To avoid personal contamination with b...

Страница 168: ...ce with local environmental regulations Notice To avoid damaging the probe heater s electrical connections do not twist the heater when removing it from the probe assembly Warning To avoid spreading c...

Страница 169: ...llary sleeve on the probe assembly 3 Fit the probe heater to the probe assembly ensuring that the heater is fully seated on the probe assembly 4 Fit the probe to the instrument see page 63 5 In the In...

Страница 170: ...5 mm Allen wrench and cone extraction tool Ion block source heater To replace the ion block source heater 1 Remove the ion block assembly from the instrument see page 119 2 Ensure that the isolation v...

Страница 171: ...014 715004387 Rev B 171 3 Use the combined 2 5 mm Allen wrench and cone extraction tool to loosen the 2 captive screws securing the ion block cover plate 4 Remove the ion block cover plate Ion block c...

Страница 172: ...llen wrench and cone extraction tool to remove the 2 screws securing the heater wires to the PEEK terminal block 6 Use the needle nose pliers to carefully swing the ring terminal tags out of the termi...

Страница 173: ...he combined 2 5 mm Allen wrench and cone extraction tool to fit and tighten the 2 screws securing the heater wires to the PEEK terminal block 12 Fit the ion block cover plate onto the ion block assemb...

Страница 174: ...nclosure seal Nebulizer gas seal Desolvation gas seal Removing the probe adjuster assembly probe and source enclosure seals Required materials Chemical resistant powder free gloves O ring removal kit...

Страница 175: ...mbly see page 99 Probe seal Nebulizer gas seal 3 Use the O ring removal kit to carefully remove the following seals from the source enclosure Source enclosure seal Nebulizer gas seal Desolvation gas s...

Страница 176: ...embly seals Required materials Chemical resistant powder free gloves Wash bottle containing HPLC grade or better 1 1 methanol water New seals Warning To avoid spreading contamination dispose of the se...

Страница 177: ...nclosure Tip Start by feeding the seal into the groove at the bottom right hand corner and then working around the seal in a counterclockwise direction 3 Fit the following new seals to the source encl...

Страница 178: ...material New air filter To replace the air filter 1 Lift the instrument s visor so that the source probe is fully exposed 2 Fully open the source enclosure 3 Disconnect the probe cable from the high...

Страница 179: ...rd you 5 Remove and dispose of the old filter 6 Place the new filter flat on the inside part of the grill with its edges beneath the metal lip 7 Close the air filter grill 8 Connect the probe cable to...

Страница 180: ...le Gas ballasting helps to circulate and mix the oil through the pump before draining 2 Vent and shut down the instrument see the mass spectrometer s online Help for details 3 Allow the roughing pump...

Страница 181: ...drain plug is clean and properly seated 10 Use the 8 mm Allen wrench to fit and tighten the roughing pump s oil drain plug Warning To avoid spreading contamination dispose of the roughing pump oil in...

Страница 182: ...se the 8 mm Allen wrench to refit the oil filler plug 15 Gas ballast the roughing pump see page 102 Tip After you add oil to the pump the following situations can occur The oil level drops slightly du...

Страница 183: ...e mass spectrometer s online Help for details 2 Allow the roughing pump to cool 3 Use the 6 mm Allen wrench to remove the 4 bolts securing the exhaust flange to the roughing pump Warning To avoid pers...

Страница 184: ...7 Rev B 4 Carefully remove the exhaust flange and oil demister element from the roughing pump 5 Use the 10 mm wrench to remove the nut that secures the oil demister element to the exhaust flange TP026...

Страница 185: ...lange from the oil demister element 7 Remove the spring from the oil demister element 8 Dispose of the oil demister element in accordance with local environmental regulations Warning To avoid spreadin...

Страница 186: ...of the spring fit the exhaust flange to the oil demister element Warning To avoid personal contamination with biohazards or toxic materials and to avoid spreading contamination to uncontaminated surf...

Страница 187: ...st flange to the roughing pump Requirement The bolts securing the source exhaust flange to the roughing pump must each be sequentially and incrementally tightened until they are all fully tight 5 Use...

Страница 188: ...om its storage location on the source adaptor housing 4 Hook the short end of the Allen wrench through the ring on the back of the bulb extraction plug and tug to remove it Warning To avoid personal c...

Страница 189: ...urce enclosure 11 Slide closed the instrument s source interface door APPI APCI source cleaning the lamp window The transmission of the high energy photons responsible for APPI relies on the cleanline...

Страница 190: ...on the source see page 88 2 Pull the source enclosure release located at the bottom right hand side outward and swing open the enclosure 3 Use methanol or isopropyl alcohol applied to the lint free cl...

Страница 191: ...ly seals Required materials Chemical resistant powder free gloves Combined 2 5 mm Allen wrench and cone extraction tool 3 mm Allen wrench Small Phillips cross head screwdriver Small Pozidriv screwdriv...

Страница 192: ...bulb extraction plug aperture 5 Clear an area lay out the soft cloth or mat and lay the source enclosure on its face Warning To avoid personal contamination with biohazards or toxic materials and to a...

Страница 193: ...action tool to remove the remaining 2 lamp drive cover screws which were hidden by the release handle 8 Slide the cover off the lamp drive 9 Use the 3 mm Allen wrench to remove the 4 source enclosure...

Страница 194: ...2 Slide the lamp assembly shaft and flange out of the APPI source enclosure Tip The cables remain attached to the shaft which you fully withdraw and lay on the bench beside the source enclosure TP0320...

Страница 195: ...r screws 15 Remove the PEEK insulator from the end of the mounting shaft 16 Slide the shaft mounting flange off the shaft and note the correct orientation for its reassembly 17 Use the O ring removal...

Страница 196: ...g from the APPI source enclosure side 20 Dispose of the O rings in accordance with local environmental regulations Warning To avoid spreading contamination dispose of the O rings in accordance with lo...

Страница 197: ...ring in the small radius at the bottom of the groove Then use a suitable tool one with a circular cross section to roll the remainder of the O ring into the groove 2 Fit the lamp bulb sealing O ring...

Страница 198: ...nge is uniformly seated on the APPI source enclosure side plate 8 Use the combined 2 5 mm Allen wrench and cone extraction tool to tighten the four mounting flange securing screws 9 Remove the mountin...

Страница 199: ...e enclosure to the machine refit the corona pin and probe Refer to page 71 for instructions Replacing the instrument s fuses If one or both of the mass spectrometer s fuses blow the instrument will sh...

Страница 200: ...4 Maintenance Procedures 200 March 14 2014 715004387 Rev B...

Страница 201: ...uct manuals where they accompany statements describing the hazards and advising how to avoid them This appendix presents the safety symbols and statements that apply to all of the products that Waters...

Страница 202: ...r a component of an instrument or device When one of these symbols appear in a manual s narrative sections or procedures an accompanying statement identifies the applicable risk and explains how to av...

Страница 203: ...rning Risk of tipping Warning Risk of explosion Warning Risk of eye injury Warning To avoid injury from bursting nonmetallic tubing heed these precautions when working in the vicinity of such tubing w...

Страница 204: ...tective panels The components they cover are not user serviceable Warning To avoid nonlethal electric shock ensure the mass spectrometer is in Standby mode before you touch any of its external surface...

Страница 205: ...es of Health NIH publication Biosafety in Microbiological and Biomedical Laboratories BMBL Observe Good Laboratory Practice GLP at all times particularly when working with hazardous materials and cons...

Страница 206: ...Bottles Prohibited symbol The Bottles Prohibited symbol alerts you to the risk of instrument damage caused by solvent spills Notice To avoid damaging the instrument s case do not clean it with abrasi...

Страница 207: ...la conformit la r glementation peut annuler le droit de l utilisateur exploiter l quipement Achtung Jedwede nderungen oder Modifikationen an dem Ger t ohne die ausdr ckliche Genehmigung der f r die o...

Страница 208: ...se trouvant proximit de l instrument Evitez d utiliser des tubes s v rement d form s ou endommag s Evitez d utiliser des tubes non m talliques avec du t trahydrofurane THF ou de l acide sulfurique ou...

Страница 209: ...dimetilsolfossido provocano rigonfiamenti nei tubi non metallici riducendo notevolmente la pressione di rottura dei tubi stessi Advertencia se recomienda precauci n cuando se trabaje con tubos de pol...

Страница 210: ...A Safety Advisories 210 March 14 2014 715004387 Rev B Nonmetallic Tetrahydrofuran THF Methylene chloride Dimethyl sulfoxide THF...

Страница 211: ...par le mat riel risque d tre d fectueuses Vorsicht Der Benutzer wird darauf aufmerksam gemacht dass bei unsachgem er Verwenddung des Ger tes die eingebauten Sicherheitseinrichtungen unter Umst nden n...

Страница 212: ...type et de la puissance indiqu s sur le panneau proximit du couvercle de la boite fusible de l instrument Vorsicht Zum Schutz gegen Feuer die Sicherungen nur mit Sicherungen ersetzen deren Typ und Ne...

Страница 213: ...la rubrique Remplacement des fusibles du chapitre traitant des proc dures de maintenance Vorsicht Zum Schutz gegen Feuer die Sicherungen nur mit Sicherungen ersetzen deren Typ und Nennwert im Abschni...

Страница 214: ...symbols The following electrical symbols and their associated statements can appear in instrument manuals and on an instrument s front or rear panels Electrical power on Electrical power off Standby...

Страница 215: ...5004387 Rev B 215 Handling symbols The following handling symbols and their associated statements can appear on labels affixed to the packaging in which instruments devices and component parts are shi...

Страница 216: ...A Safety Advisories 216 March 14 2014 715004387 Rev B...

Страница 217: ...nt or remove it from service contact Waters Technical Service for recommended cleaning flushing and packaging procedures See page 87 Contents Topic Page External wiring and vacuum connections 218 Conn...

Страница 218: ...panel connections appear in the figure below Note that the connectors and controls not identified are for use by Waters engineers only Rear panel Power Source vent Turbo vacuum Nitrogen inlet Collisio...

Страница 219: ...tallation kit NW25 center rings included in the installation kit NW25 clamps included in the installation kit 10 mm reducer fitting included in the installation kit 10 mm ID nylon tube included in the...

Страница 220: ...ct the roughing pump 1 Place the PTFE drip tray on the floor within 5 feet of the instrument 2 Place the pump on the PTFE drip tray Warning To avoid personal contamination with biohazards or toxic mat...

Страница 221: ...osite end of the 10 mm nylon tube to the 10 mm source vent port on the instrument s rear panel 7 Using 1 hose clamp connect a length of 12 7 mm clear PVC exhaust tubing to the roughing pump exhaust po...

Страница 222: ...ck the oil level in the pump see Checking the roughing pump oil level on page 106 and if needed Adding oil to the roughing pump on page 106 Requirement To ensure correct operation of the roughing pump...

Страница 223: ...rical connections To make the electrical connections to the roughing pump 1 Connect the relay cable from the roughing pump d c connector to the pump connector on the instrument s rear panel 2 Connect...

Страница 224: ...fe NW25 tee included in the installation kit NW25 center rings included in the installation kit NW25 clamps included in the installation kit NW40 center rings included in the installation kit Warning...

Страница 225: ...ed in the Waters Rotary Pump Kit Bear in mind these requirements when connecting the roughing pump The pump must be horizontal or within one degree of horizontal The ambient temperature of area in whi...

Страница 226: ...1 inch vacuum hose in step 4 to the 1 inch OD straight vacuum port on the instrument s rear panel 6 Connect the opposite end of the 10 mm nylon tube to the 10 mm source vent port on the instrument s...

Страница 227: ...9 Connect electric cables to the roughing pump see page 227 Connecting electric cables to the Edwards oil free roughing pump Roughing pump connections To connect cables 1 Connect the relay cable from...

Страница 228: ...as supply 1 Use the sharp knife to cut a 3 8 cm to 5 0 cm 1 5 inch to 2 inch length of 6 mm PTFE tubing Requirement Cut the tubing squarely that is perpendicularly to its horizontal axis 2 Connect one...

Страница 229: ...ust connections 5 Attach the nitrogen regulator to the nitrogen supply 6 Install the 6 mm stud into the regulator outlet 7 Connect the free end of the long piece of 6 mm PTFE tubing to the 6 mm stud S...

Страница 230: ...e 1 8 inch Swagelok nut and ferrule to connect the 1 8 inch stainless steel tube to the collision cell gas inlet on the rear of the instrument see the figure on page 229 2 Use the wrench to tighten th...

Страница 231: ...nitrogen exhaust ensure that the nitrogen exhaust is vented via the nitrogen exhaust trap bottle and laboratory exhaust system The laboratory exhaust system must provide a minimum vacuum of 0 20 kPa...

Страница 232: ...in the source exhaust system confirm the integrity of the system by performing the following leak test Leaks can result in the release of biohazardous or toxic materials Notice To avoid damage to the...

Страница 233: ...ver the barbed fitting of the drain located at the bottom of the instrument Warning To prevent personal contamination with biohazards or toxic materials always wear chemical resistant powder free glov...

Страница 234: ...t its end is above the surface of the waste solvent Positioning of drain tube Warning To prevent leakage of biohazards or toxic materials ensure that the drain line does not crimp or bend impeding flo...

Страница 235: ...ort on the rear panel of the instrument 3 Connect the other end of the shielded network cable to the port labeled Instrument LAN on the workstation rear panel To connect the instrument to the power so...

Страница 236: ...net connections 1 Connect one end of one shielded Ethernet cable to the network switch and then connect the other end to the Ethernet card on the preconfigured ACQUITY workstation Tip On preconfigured...

Страница 237: ...are typically SELV include contact closure inputs and outputs for autosamplers and UV RI and fluorescence detector signal outputs for LC MS systems The electrical connections on the rear panel of this...

Страница 238: ...ctions Description Analog Out Used for analog chart output functionality The output voltage range is 0 to 1 V The resolution of the voltage output is 12 bits Stop Flow Out Used to stop the solvent flo...

Страница 239: ...tive leads of the signal cable to the connector 3 Slide the clamp with the bend facing down into the protective shield 4 Insert the clamp and shield with the bend facing down into the connection cover...

Страница 240: ...signal cable into the connection cover and position the clamp over the cable leads Tighten the clamp into place with the second self tapping screw 6 Place the second connection cover over the first c...

Страница 241: ...panel of the instrument 2 Connect the male end of the instrument power cord to the 200 to 240 V AC wall outlet prepared as described in the instrument Site Preparation Guide 3 Connect the power cord...

Страница 242: ...B External Connections 242 March 14 2014 715004387 Rev B...

Страница 243: ...aused by personal exposure to biohazards or toxic materials you must confirm the integrity of the source exhaust system and address any safety issues raised by the contents of this Appendix Contents T...

Страница 244: ...r details about the most common ingredients used to prepare mobile phases Items exposed to solvent Item Material Autotune reservoirs High density polyethylene Corona discharge pin mounting contact PEE...

Страница 245: ...er Methanol Acetonitrile Formic acid 0 1 Acetic acid 0 1 Trifluoroacetic acid 0 1 Ammonium acetate 10 mM Ammonium formate 10 mM These solvents are not expected to cause any problems with the materials...

Страница 246: ...C Materials of Construction and Compliant Solvents 246 March 14 2014 715004387 Rev B...

Страница 247: ...tubing or stainless steel finger tight screws to connect the selector valve to the source probes use the PEEK tubing and natural beige colored PEEK finger tight screws specified on page 250 Warning To...

Страница 248: ...nt behind the visor The letters etched on the front of the valve represent the components to which the associated port is connected Etched letters with a light background indicate inputs while letters...

Страница 249: ...15004387 Rev B 249 Plumbing schematic Requirement Ensure that the end of the tubing is fully submerged in the solvent in the wash reservoir P W R B A S LC LC column Xevo TQD probe Pump Reservoir A Res...

Страница 250: ...visit Notice To avoid leaks when plumbing the IntelliStart Fluidics system use only the tubes nuts and ferrules shown in the following tables to ensure over pressure protection The use of parts not re...

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