Agilent 1290-6500 Q-TOF操作规程

1290 - G6500-© , 20102011 5Rev. B.04.00TOF Q-TOF MassHunter B.04.00800 820 3278400 820 3278 ( )800 820 1172lsca-china_800@Agilent /chem/library/chem/education/chem/eseminars/chem/techsupport/chem/supplies/chem/techsupp (2) (3)1 (6)1.1 (6)1.2Q UAD (7)1.3TOF (8)1.4Q-TOF (9)1.4 (10)1.4.1 ESI — (10)1.4.2 APCI — (10)1.4.3 ESI with Agilent Jet Steam Technology— ESI (11)1.4 (11)2 (12)2.1 (12)2.2 (12)3 (13)3.1 (13)3.2 (17)4 (18)5 (22)5.1 (22)5.2 (24)5.3 (26)5.4DAD (27)5.5Q-TOF (27)6 (28)6.1 (28)6.2 (29)6.3 (29)6.4 (30)6.4.1 Manual Tune (30)6.4.2 Diagnostics (30)6.4.3Instrument State (31)6.4.4 Preferences (31)6.5I NITIAL T UNE (32)6.6S TANDARD T UNE (33)6.7Q UICK T UNE (33)6.8C HECK T UNE (34)6.9C ALIBRATION (34)6.10Q UADRUPOLE T UNE (36)6.11 (37)7 (38)7.1 (38)7.2 (39)7.3 (40)7.4 (41)7.5DAD (42)7.6Q-TOF (43)7.6.1 General (44)7.6.2 (45)Dual ESI (45)7 ESI Jet Stream (45)APCI (46)7.6.3 Q-TOF (47)TOF (47)MS/MS (Auto MS/MS) (48)MS/MS (Targeted MS/MS) (52)7.6.4 Ref Mass (54)7.6.5 Chromatogram (55)7.7P ROPERITIES (55)7.8 (55)8 (56)8.1 (56)8.2 W ORKLIST (57)8.2.1 (57)8.2.2 (57)8.2.3 (58)8.2.4 (59)8.2.5 (59)8.2.6 (59)9 (60)9.1 (60)9.2 (61)9.3 (61)9.4 (62)9.5 (63)9.6 (64)9.7 (65)9.8W ALK C HROMATOGRAM S PECTRUM P REVIEW (66)9.9 (67)9.10 (67)9.11 (68)9.12 (69)9.13F ORMULA C ALCULATOR (70)9.14M ASS C ALCULATOR (70)10 (71)10.1MS (71)10.2 N EBULIZER (71)10.3 (72)10.4 (73)10.5 (74)10.6 (75)10.7 (76)10.8 (76)10.9 (77)10.10 (77)11 (78) (79)1 (79)1.1 (ESI) (79)1.2 Agilent ESI (Jet Stream) (79)1.3 APCI (79)2 (80)3 (81)3.1 G1960-80060 (81)3.2 59987-20040 (82)4 (83)51290 (84)6 (85)7 (86) (86) (86) (86)11.1Skimmer 1 Lens 1 Lens 2/Q-TOF Edwards EM28 1.8-2.5 Torr Q-TOFG6510 G6520 G6530 G6538 G6540TOF TOF~ 3.0×10-6 torr ~ 8.0×10-8 torr ~ 3.0×10-6 torr ~ 8.0×10-8 torr ~ 2.0 ×10-5 torr ~ 2.0×10-7 torr ~ 5.0×10-5 torr ~ 2.0×10-7 torr1.2 Quad/ - V dc V rfRF DC RF DC++1.3 TOF=×1.4 Q-TOFQ-TOFTOF(TTI, Total Transmission Ion) TOF Q-TOF TOFMS/MS (Auto MS/MS)SIM TOFQ-TOF TOFMS/MS (Targeted MS/MS) :SIM TOF1.490Standby1.4.1 ESI —ESI ESI1.4.2 APCI —APCI (CI) , ESI APCI-1.4.3 ESI with Agilent Jet Steam Technology— ESIESI ESI ESI MS MS1.422.1LAN Switch2.2HPLC Q-TOF Gxxxx USxxxxxxxx DExxxxxxxx JPxxxxxxxxAgilentHPLC G4220A, DEBAA0078533.10.7 MPa ~110psi0.7 MPa ~110 psiPeak Peak0.15 MPa 0.2 MPa 30psi1. LAN Switch2.3.( )4. Connection > ConnectIP 192.168.254.12 OK5. ParametersTOFQ-TOF Turbo1 Turbo2 95% TOF2.5Torr TOF 1.5×10-6Torr Agilent MassHunter1.5×10-6Torr MassHunter6. TOF 1.5×10-6Torr Instrument ON/OFF Condition HV ConditionHV Condition0.6 Hour Cycle (Quick Vent) Q-TOF Condition2 Hour Cycle (Optics Service) Q-TOF Condition8 Hour Cycle (TOF Service) Q-TOFCondtion Agilent13 Hour Cycle (Installation) Q-TOF CondtionTOF 1.5×10-6Torr Condition System Turn-On Start( Flush CDS) TOF HV Condition( ) HV Condition HV Condition AgilentHV ConditionConditionCondition Condition Condition Completed7. Condition HV File Connection > Disconnect Q-TOF8. MassHunter MassHunter9.Shut Down Stopped Close3.220-30minInstrument ON/Off Vent15-30min Vent Vent Parameters VentVent MassHunter Q-TOF VentQ-TOF LCVent Parameter4MassHunterActuals setup Actuals Setup Background Color TextLC “Not Ready Text Long” Not Ready Logbook “Not Ready Text Long” — AReadyNot Ready Standby By Shut DownQ-TOF55.1ConfigurationTray (Tray) G4226 1-10 54 Agilent 1.5 mL 96 384P1-E5P1 1E E5 5G1330B Thermostat G1330B 4-40G1330B UG1330B110Plate 2 P2-XY X- Y-Plate 1 P1-XYTray Illumination On/Off Reset InjectorMove Home Home Needle Up Valve Bypass/ Valve Main Pass Main Pass BypassMain PassMain Pass BypassLock Door During RunInjector Flush Pump5.2On Off StandbyControl On Off StandbySet Solvents Level “Prevent analysis if level fall below” “Turn pump off if running out of solvent”From PumpTo ColumnFrom PumpTo Column23 45 61 12 5 634ONSeal Wash 5 0.2 Single Wash10%Purge and Prime : 1290 Purge Prime PurgeEnable purge purge PurgeB A B PurgePrime Purgeprime purge5.3ControlColumnsThermostat Controlling On5.4 DADUV Lamp On (UV Lamp) 1290 DADControlCalibration BalanceIntensity Plot Calibration Intensity Plot Holmium Test LC Lab AdvisorLC Instrument Utilities5.5 Q-TOFOn Standby Off TOF(Off)StandbyVent Pump Down Vent MS Pump Down APPI UV Lamp MS APPI APPI Reset Ion Source Type:66.1ESI G6530A G6540A Initial Tune 100mL10 40(G1969-85000) 10 mL 2.5 mL88.5 mL 95.6 mL1.5 mL 1.9 mLHP-0321 5 L 0.1 mM ( G1969-85003 )Initial Tune Calibration Check Tune 650K 100mLG6510A G6520A/B G6538A4(G1969-85000) 25 mL71.25 mL3.75 mLCalibrant BQ-TOF B A1. Quad Tune TOF2. APCI APPI MMI 43. Fragmentor6.2/ Q-TOF On Context Tune Tune Method Editor Agilent MS Acquisition Worklist Pane Yes No6.3Q-TOF TOFTOF Initial Tune Standard Tune Quick Tune Check Tune Set Detector Gain Calibration Initial Tune Standard TOF Tune Quick Tune Check Tune Calibration Set Detector GainQuadrupole( ) Intial Quad Tune, Quad Tune Check Quad Tune Initial Quad Tune Quad Tune Check Quad TuneInitial TuneStandard TuneQuick TuneCalibrationTOF Extended Dynamic Range Initial Tune Standard Tune Quick Tune Check Tune Calibration High Resolution Calibration Quick Tune Check Tune Standard Tune Initial Tune Extended Dynamic RangeCalibration Calibration Check Tune1-2 Quick Tune Check Tune Quick TuneQuick Tune Standard TuneStandard Tune Initial TuneCalibration6.46.4.1 Manual TuneManual Tune6.4.2 DiagnosticsQ-TOF TOF Vent6.4.3Instrument StateHigh Resolution Extended Dynamic Range Minimum Storage Size Q-TOFHigh Resolution Extened Dynamic Range Q-TOF 3200 1700 Minimum Storage Size G6520B 6530A 20000 G6538A G6540A 100006.4.4 Preferences650,000 Fragmentor Fragmentor 650,000 Adjust abundances for optimal calibration, Fragmentor6.5 Initial TuneStandard Tune Initial Tune Initial Tune ExtendedDynamic RangeInstruments State Extended Dynamic Range Extended Dynamic RangeApply Extended Dynamic Range Apply Yes.Autotune Positive Negative Q-TOF G6530A G6540A, Pause Between Autotunes For Calibration Solution Swapping)Initial Tune Yes Start Autotune6.6 Standard TuneQuick Tune Standard Tune Standard Tune Extended Dynamic RangeStandard Tune Initial Tune Autotune Standard Tune, Start Autotune6.7 Quick Tune1-2 Quick Tune Checktune Quick Tune Quick Tune Extended Dynamic Range High ResolutionInitial Tune Standard Tune Autotune Quick Tune, Start Autotune6.8 Check TuneCheck Tune Check TuneCheck Tune Start Autotune6.9 CalibrationCalibration CalibrationTOF Mass Calibration Calibration Bottle B MS TOF (Positive) (Negative) CalibrateCalibrateBCalibration Calibration alt + Print Screen Paint Wordpad Excel Edit Paste6.10 Quadrupole Tune1.2. TOF Calibration InitialQuad Tune Quad Tune Extended Dynamic Range Quadrupole( ) Intial Quad Tune, Quad Tune Check Quad TuneInitial Quad Tune Quad Tune Quad Tune Quad Checktune Check Quad TuneIntial Quad Tune 40TOF Yes6.11Context Acquisition Acquisition Instruments State Confirmation Yes NoCalibrationOKYes MassHunter No7LC MSMassHunter “Context” Acquision HPLC Q-TOF7.1File>New>Method File>Open>Method D:\MassHunter\Methods\ Default.mAgilent “ ”“Ion Source not identical” Ion SourceApply7.2Agilent 3 Standard injectionInjection with Needle WashUse Injection ProgramHigh ThroughputDisable Overlapped injection High ThroughputSetup Wash needle in wash-vessel Wash needle in Flush Port 5-10Options (Draw Position) (vial/Well bottom sensing)- - -- -(As Pump)5mm 5mm10mm1-10Bottom Sensing7.3Setup A B A B A1-B1 A1-B2 A2-B1 A2-B2 A1-A2 B1-B2OptionsTimetable (Insert)(Append) (Cut) (Copy) (Paste)B 0-100%BOptionUse enhanced compressibility calibration SetupUse enhanced compressibility calibration, A B126 104 11512095 150 110 100 100 120 118 87114467.4Time Table OptionsA B Auto7.5 DADSetupSpectrum DADPeak Width 15-20Peak Width (Hz) 0.0012 160 0.0025 80 0.005 40 Hz 0.01 20 Hz 0.03 10 Hz 0.05 5 Hz 0.1 2.5 Hz 0.2 1.25 Hz 0.4 0.625 Hz 0.85 0.3125 HzOptions Required lamps (UV) DAD7.6 Q-TOFQ-TOF Q-TOF (Time Segment) (Experiment) …Q-TOF LC i-button(Time Segments), (experiments#)Fragmentor:MS Q-TOF Time SegmentExperiment # Time=0 minutes Expt=1(Seg) (Expt)- Expt Add-Time Add- - Apply7.6.1 GeneralLC MS (centroid) (profile)Abs. threshold ( ) centroid Rel. threshold (%) ( ) % centroidedcentroided 0 centroid Do not wait for setpoints to equilibrate7.6.2Gas Temp Drying Gas NebulizerFragmentor Skimmer (skimmer) OCT 1 RF Vpp Fragmentor Skimmer OCT1 RF Vpp Dual ESIESI 4000V 3500VESI HPLC 200 L/minHPLC * Nebulizer pressureDrying Gas FlowDrying Gas TempCapillary Voltage1-10 L/min 15-20 psi 4 325 4000V 3500V10-50 L/min 15-20 psi 5 325 50-200 L/min 20-40 psi 8 350 200-500 L/min30-50 psi 8-10 350 500-1000 L/min50-60 psi10-123507 ESI Jet StreamESI ESI (Sheath Gas Temp) (Sheath Gas Flow) (Nozzle Voltage)Jet Steam Standby 125Jet StreamHPLC 250-600 L/min 250C 11 L/min 500 V 45 psi 4000 V (pos) 3500 V (Neg) 5 L/min300HPLC 250-600 L/minAPCIAPCI ESI APCI 500 L/min 200 L/min HPLC APCIHPLCAPCIHPLC L/min Nebulizer pressure Drying Gas Flow Drying Gas Temp Vaporizer Temp Corona Current Capillary Voltage200-1500 60 psi 4-6 L/min 350 300-500 4 uA( )10uA( ) 3500 V7.6.3 Q-TOFQ-TOF TOF , MS/MS MS/MS TOFAcquisition MS (Seg) TOF(TTI) TOFTOF Mass Range experimentMin Range m/z Max Range m/z Acquisition Rate/TimeRate TimeTransients/spectrum ( ) TOFMS/MS (Auto MS/MS)SIM TOFQ-TOF TOFMS/MS TOF Q-TOF TOF MS/MSMS/MS , MS/MS, TOF (Spectral Parameters) MS 1 (Precursor Selection I )Static Exclusion Range List / MS/MS (active exclusion) MS/MSMS/MSSpectral ParametersMS1 MS2 MS/MS MS MS/MS (transient) MS/MSCollisiion Energy Fixed Collision EnergyPrecursor Selection IMax Precursor Per Cycle 10 2 MS/MSPrecursor Threshold % 100% 100 000counts 1% 1000countsStatic Exclusion Range ListActive Exclusion MS/MS “Enabled”4 2Precursor Selection II ActiveActiveActive。