Step by step GCMS operating manualWord文档下载推荐.docx
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loadthelatestcalibrationfile.
Block2.
Createandsavesamplelist.
Block3.
Runtheanalysis.
Block4.
SwitchthemachineintoStandbymode;
switchoffMStunewindow.
Block5
Analysisofchromatogramsanddatacollecting.
Block6.
Don’tdo.
Block1–Open/createproject.
Whenyoustart–youcanopenyourexistingprojectorcreateanewone.ToopenexistingprojectdotoFile–Open.Projectislikeafolderwhereyourinformationwillbestored.
WhencreatingnewonegotoFile-ProjectWizard.
FornewprojectfillintheProjectnameandpressNext.
Confirm–CreatenewprojectandpressFinish.
Block1–Inletmethod
OnethemainwindowthebottomShortcutshouldbepressed.Youshouldseethefollowingviewwithblueiconsontheleft.
PressfirsticonInletmethod.ItmanageswithchromatographypartinGC-MS.
Pressontheiconwithbottle(Inletparameters).
Youobtainthefollowingwindow.
Pressthetab“Oventemperatureramp”
Setupnecessaryparametersforchromatography(forcapillarycolumn).Maximumtemperatureshouldnotexcide280-300Candbehigherthanboilingpointofyouranalyte.Ifboilingpointofyouranalyteishigherthanmaximumofcapillarycolumn–youranalytewontcomeupfromthecolumnandmayevenblockthecapillar.Userumpfunctionwhennecessary.Maximumoventemperatureis325C.
Recommendedstartingtemperatureis40-60Ctocutoffyoursolvent.Goodsolventforthecolumnare:
hexane,benzene,THF,chloroform,DCM.Notacceptablesolventsarewater,acidsandalkalis(completedamageofthecolumn),DMF,DMSO.
ThenpressthetabBackInjector.
ConfirmGassaver–Enabled;
Flow–15mL/min;
time6min;
InjectorOn.Setuptemperatureofinjector(shouldbeenoughtoevaporateyouranalyte–shouldbehigherthanboilingpointofanalyte)andshouldnotbehighenoughtodestroytheanalyte.Maximumpossibleinjectortemperatureis230-250C.
ThengotoFileandSaveas.Savethemethodwithextension.h68.InletmethodshouldbesavedinthefolderACQUDBinyourprojectfolder.Allfoldersintoyourprojectfolderarecreatedautomaticallywhenyoucreateanewproject.Youcanadd“Inletmethod”wordsinthenameofInletmethodsavedfileforconvenience.
Block1-MSmethod
PressblueiconMSmethod.MSmethodmanageswiththeworkofmassdetector(massspectrometrypartinGC-MS.
Ifthereisablueline–clickbluelinetwice.YoucanseeMSwindow.Ifthereisnoblueline–clicktypeofmethodofmassdetector–MSscan.
Inthedropupwindowyoushouldsetup:
startandendofmassscanning(recommendedfrom50upto600Da.Timemin:
Startmeanstimewhenyourdetectorstartsscanning.Itstartsnotfrom0minbutfrom3.5-4minbecauseweneedtoavoidworkofdetectorwhensolventcomesout.Highconcentrationofsolventcandamagedetector.Thereforeitstartafter4minwhenallsolventalreadycameoutfromthecolumn.EndanalysisshouldcorrespondtoyourRuntime.Youtakethisvalue(endofyouranalysis)fromthetabofInletmethod–Oventemprump(seeabove).ToseetheendtimeyourneedclickthebottomRuntime.
InletMethodwindowcanbeclosedaftersavingtheInletfile.
Inourcasethelengthofanalysisis19min.
IonizationmodeisE+;
dataprocessing–Centroid;
Scantimeis0.6secs;
Inter-Scandelayis0.07secs.AfterthatpressOKbottom(seebelow).
Asaresultyoushouldseethewindowasshownbelow.
ThengotoOption–Solventdelay.
Reconfirmthedelaytimewhenyoursolventcomeoutfromthecolumn.Itshouldcorrespondtothestartoftheanalysis(seetwopicturesbelow).Inourcaseitis4min.PressOK.
ThengotoFileandSaveastheMSmethodwiththeextension.expinthefolderACQUDBinyourprojectfolder(seebelow).YoucanaddMSmethodwordsinthenameofMSmethodsavedfileforconvenience.
Block1–MSTunewindow
NextpressMStuneblueiconattheleftsideofthemainwindow.Thewindowsasbelowisappeared.
MSmethodwindowcanbeclosedaftersavingthefile.
NowthemachineisonStandbymode.PressthebottomPresstoOperate(rightbottomcorner).Redcolorshouldbechangedintogreenone(seebelow)
CheckFilamentCurrent(A).Ifitisclosetozero–pressReinitializeFilamentbottom.
Thevalueoffilamentcurrentshouldbeabout5Ainnormalcondition(below).
Checkwhethercomputercanseethemachine.GototheOption–Communicationstatus.
Ifthemachineis“Notpresent”–gotoOptionandclickReinitialize.
Thenloadthelatestcalibrationfile.GotoFile–Open–andchoosethehighlightedbelowfilefromdropupwindow220711_MS1.ipr.(ShouldbeinyoursubfolderACQUDBinyourprojectfolder).
MStunewindowshouldbealltimeopenwhendoinganalysis!
!
Block2.Samplelistinthemainwindow.
YouneedtofillinFileName.SampleIDandFiletextcells–uptoyou(maybeempty).
ClickonthecellunderMSmethod.ChoosetheMSfilefromdropupwindow.
HighlightandconfirmpressingOpenbottom(Orjustclicktwiceonfilename).ThecellofMSmethodinthelineofyoursampleshouldbefilledinlikeshownbelow.
DothesamewithInletmethod.ClicktwiceontheemptycellunderInletmethodandchoosethecorrectfilefromdropupwindow.
ThecellofInletmethodinthelineofyoursampleshouldbefilledinlikeshownbelow.
FillinthevialnumberinBottlecell(numberofyoursampleinthecarouselautosampler),andput10forInjectvolumecell.Thisisallinformationthatisneededforanalysis.
YoumayinsertnecessaryamountoflinesclickingontheexistinglineandtochooseInsertorAdd.
OryoucangotoSampletabandchoosenecessarycommandaswell.
Whenfinishingsamplelistyouneedtosaveit.GotoFile–Saveas.
Block3.Runtheanalysis.
Checkwhethereverythingisready.
Highlightthelinesofsampleswhichyouwanttoanalyze(justclickingonitorclickinganddraggingifmany).
ThenpressiconStartup(Bluetriangle).
Machinewillasktoreconfirmorchangetheamountofsampleindropupwindow.
CheckthethickshouldbeinAcquireSampleData,andpressOK.
Machinewillstartanalysis.Greencolorshouldappearonrunningsampleline.
Block4.SwitchthemachineintoStandbymode;
switchoffMStunewindow.
Whenthemachineisfinishanalysespress“PresstoStandby”bottom.GreencolorshouldturnintoredandPresstoStandbyshouldbechangedintoPresstooperate.
Whenyouseethefollowingpicture(below)–youcanclosetheMStunewindow.Itwilltakesometime(upto10-20seconds).
Block5.Dataanalysis.
Highlightthelineofnecessarysample(clickonitonce).–Seebelow.
ClickonChromatogrambottomandwindowwithchromatogramofyoursampleisappeared.
Rightmouseclickonthepeakyouwanttoanalyze.Verticallineisappearedandyoucanseemass-spectrumwindow.
Clickonthelibraryicononthemassspectrumwindowtoidentifyyourchemicalusinglibraryofmassspectra.
Thefollowingwindowisappearedautomatically.Youcanseealistofchemicalsthatfittoyousamplemassspectrum.Thefirstonefromthetopinthelisthasalltimethehighestprobabilityoffitting.
Block6.Don’tdo.
Notabene!
NeverclosethemainwindowofGC-MS(below)!
AnyotherwindowsmaybeclosedwithoutinterruptingGC-MSactivity.OnlyMSTunewindowcannotbeclosedwhenanalysisisrunning.AndMSTunewindowcanbeclosedonlyaftertransferringintoStandbymode(redcolorwindowattherightbottomcornerandnofilamentcurrentorclosetozerocurrentvalue).