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UserguideforCary5000absorptionspectrometerwithexternalDRA1800attachment.
(lastupdated10/25/2017)
ThisguideisforuseoftheCary5000withtheDRAonly.ForusewithouttheDRAasastandardtransmissionspectrometerseetheUserguideforCary5000inabsorptionmode.
Importantwarnings!• DonotunplugorplugintheexternalDRAattachmentwhentheinstrumentis
on.Thiswillruinthedetectorsoftheintegratingsphere• DonotputwhitelightintotheDRAwiththeDRAelectricallyconnectedtothe
Cary.• Minimizetheamountoftimethattheintegratingsphereisopen.Long-termlight
exposurehurtthedetectorovertime.• Wearcleangloveswhileusingtheinstrument• Donotuseliquidorpowdersamplesintheintegratingsphere.
QuickStartforusingDRA1. Turnoncomputer2. ClickontheCaryScanicononthetaskbar3. Checklensandmirrorarecorrectforyourmeasurement.(Wareglovestochange
themirrorsorlens).a. InstallSmallSampleKitmirror(M3SSK)orregularM3mirrorifneededb. IfusingSSKinstallcorrectlensL2.
4. MakesurecoverfortheDRAisfullyclosedandturnCaryon.5. IfyougetanerrorturngotothesectionbelowonStartupErrors.off6. Wait20minutesforthelampstowarmup.7. Ifyouneedtochangeand/oraligntheopticsseethelocalusermanualbelowand
rememberneverputwhitelightintotheintegratingspherewhentheCaryisturnedon.Toaligntheinstrumentuse550nmlight.
8. SelectSetupa. setwavelengthrange,%Tor%Rb. UnderOptionstab:setslitwidthandheight,SBWto2nm,Detectorand
Gratingchangewavelengthsc. UnderBaselinetab:chosezero/baselined. UnderStoragetab:Setyourfilename
9. Makesurethatallexitsoftheintegratingsphereareblockedwithfullreflectors.Whenusingthesmallspotkityoumusttakecarethatthefullreflectorscompletelycovertheexitportswiththeirwhitereflectormaterial.
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10. ChooseBaselineandrun100%Tscan,thenblockthesamplebeamattheentrancetotheintegratingsphereforthe0%Tscan.Ifusinganapertureholderforreflectionmeasurements,pleaseseethe“Aperturekitforsmallsamples”sectiononpage4.
11. Mountyoursample12. ChooseStarttorunthespectra 13. Whendoneremovesampleandremountreflectors.14. TurnoffCary15. Shutdowncomputer.
IntroductionandHelpForacompleteguidetotheCaryhardwareandopentheCary“Scan”programandclickontheHelptab.
Forthebasictheoryofdiffusereflectancemeasurements,usefuldiagramsofthediffusereflectanceadaptor(DRA),alignmenttipsandprocedures,anddescriptionsofalltheDRAaccessories(VATH,SmallSpotKit,andcentermountholders)gotoHelp>Helptopics>Accessories>Cary4000/5000/6000i>SolidSample>externalDRA
TolearnmoreaboutthesoftwareandtakingmeasurementsintheScanmenu,gotoHelp>Helptopics>SoftwareApplications>Scan
StartupError1. Ifyoureceivetheastartuperror(normallyE9303)whenstartingtheCary.Dothe
following:2. ClickokandlettheCarycontinuetheinitializationprocess.3. AfteritstartsandgotoCommandsandusetheGoTomenuoptiontogoto500nm.4. Checkthatthesmallapertureinthesamplebeamlightpathisallthewayopen.5. Turnthelightsoffintheroom.Checkthatthegreenlightcomesoutofthe
monochromatorwindowandisdirectedintotheintegratingsphere.Youneedtocheckboththesampleandreferencebeams.
6. Ifyoudon’tseeanylightcomingoutofthemonochromator,youneedtogobackandusetheGoTocommandagainandwaituntilitcompletesbeforeopeningtheinstrument.
7. Checkthatthereisnothingblockingthelightfromenteringintegratingsphere.8. Checkthatthereisnosampleonanyoftheportsorinsidetheintegratingsphere.9. ClosethesamplecompartmentontheCaryandmakesureyouheartheinterlock
click.10. TurnofftheCary,wait10s,andthenturntheCarybackon.Itshouldnowstartup
correctly.
Start
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LocalUserGuidefortheCary500withDiffuseReflectanceAccessoryIntegratingSphere.
Turningtheinstrumenton:OpentheCaryScanprogramonthetaskbarorDesktopTheDRAmusttobefullyclosedinorderfortheinstrumenttoinitialize.Turnontheinstrument(0/Iswitchonthelowerleftsideofthefrontoftheinstrument).IntheScanprogram,watchthelowerleftcornertoseethestatusoftheinstrument.Whenthetrafficlightisgreen(topcenterofscreen),thenascancanberun.IfthereisanerrormessageseeStartupErrorsectionabove.
BasicsconfigurationandalignmentTherearefourpositionsinwhichthesamplecanbeplacedforusewiththeintegratingsphere(seeFigure1andFigure2).
1. Theentranceslottotheintegratingsphereisfornormalincidencediffusetransmission
2. Therearslotisfornormalincidencediffusereflection3. Thecentermountholderallowsforvariableanglediffusereflectanceand
transflectancemeasurements
4. Inaddition,theVATH(variableangletransmissionholder)accessorycanbeputinfrontoftheintegratingsphereforvariableanglespeculartransmissionmeasurements.IfyouwouldliketousetheVATHaccessory,pleasetalktooneoftheGLAsfortheinstrumentfirst.
ForthenormalorlargesamplesetuptherearethreepositionsforthelargestandardM3mirror(seeFigure4andFigure3)thatcorrespondtothethreesamplepositions(Transmission,Center,andReflection).Eachofthemirrorpositionswillfocusthelightontothepositionofthesample.ThethreedifferentmirrorpositionsaremarkedT(transmittanceslot),C(centermount),andR(rearreflectanceslot)inFigure4.Thus,themirrorneedstobemovedtotherightpositiondependingontheplacementofyoursample.ThecablefortheDRAcangetinthewayofmovingthismirror.
Figure1Integratingsphereentranceslot.
Figure2Integratingsphereexitslots.
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Wareglovestohandlethemirrorsorlens.TurnofftheCaryfirst,ifyouneedtounplugtheDRAtomovethemirror.
Forthesmallsamplesetup(seesmallsamplediscussionbelow)theM3mirrorisreplacedbythesmallsamplekitmirror(M3SSK)intheTposition.Lens(L2)mountsinfrontofthesample(seeFigure3).TherearethreelensesthatcanbeusedagainforthethreepositonsmarkedasT,CorR.
Eachtimethesampleconfigurationischanged,theopticsneedtoberealigned,suchthatthesampleandreferencebeamsarenotclippedattheentrancetotheintegratingsphereandthatthesamplebeamiscenteredonthesample.
1. Putoncleangloves.2. WiththetopdoortotheDRA
closed,underthecommandsmenuclickonGoto,andthentypein550nm(donotusethe“align”option).Whenyoudarkentheroomlights,youshouldseeagreenbeam,whichyoucanusetoalignthebeamontothesample(Alternatively,ifyouhavetroubleseeingthebeam:
Figure4DiffuseReflectanceAccessorywithbeampath.
Figure3Photoofdiffusereflectanceaccessorywithbeampath.
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Blockthesampleandreferencebeamsfromenteringtheintegratingsphere.UnderthecommandsmenugotoaligntoswitchthegratingstozeroordertosendwhitelightintotheDRA.Thewhitelightshouldnotentertheintegratingsphereoritwilldamageit!!)
3. Mostofthemirrorshavetwoknobs,whichyoucanrotatetoadjusttheverticalandhorizontalpositionsofthebeam.StartwithmirrorM2andadjustsothebeamhitsthecenterofmirrorM3thenuseM3sothebeamhitsthecenterofthesample.Someofthemirrorsaremorecomplicatedtoadjust(althoughthesecanoftenbeleftalone).Forhelpwithalignment,talktooneoftheGLAsandreadthealignmentinstructions,whichcanbefoundunderHelp.
SmallsamplesMosttypicallabsamplesaresmallerinsizethanwhattheinstrumentwasdesignedtomeasure.Forallthreetypesofmeasurements(T,C,andR),itisbesttounderfillthesamplearea.Spotsize-Therearetwowaysofreducingthebeamspotsize:
1)Slitwidth:Thesimplestwayistoreducebeamsizeisbytheslitwidth.ClickontheSetuptheoptionstab.Underslitheight,switchtoReduced.Ittakesaboutaminutefortheslittochange.
2)Smallspotkit:Therearealsoaseriesoflensesthatcanbeputintheopticalpathtofocusthebeamintoasmallerspotonthesample.AgaintherearethreelenseswithdifferentfocallengthsandmarkedT,C,andRforthethreepositionsoftheintegratingsphere.Also,thelargemirror(M3)isswitchedoutforaonewithadifferentcurvature;thismirrorisalwayskeptintheTposition,regardlessofthetypeofmeasurementbeingmade.3)Aperturekitforreflectionmeasurements
Fornormalincidencereflectionmeasurements,theopencircleintherearoftheintegratingsphereisseveralinchesindiameter.Thereareaseriesofapertures,whichhavethewhiteSpectralonmaterial(sameroughenedTeflonthatisinsidetheintegratingsphere),thatcanslideontotheslotonthebackoftheintegratingsphere.Thespring-loadedmountthatholdsthesampleagainsttheintegratingspherefirstneedstobetakenoff.Slideontheappropriateapertureandtheneithertapeyoursampleontothebackoftheaperture,orputbackonthespring-loadedsamplemount.
Ifthebeamspotoverfillstheaperture,youcancorrectforthis“straylight”byperformingaZero/baselineCorrection.Normally,the0%TBaselinescanisrunbyblockingthebeambeforeitenterstheintegratingsphere,whichaccountsforelectronicnoise.Inthiscase,donotblockthebeamsothatthe0%TBaselineaccountsforthelightreflectingontheedgesoftheaperture.
PerformingaZero/BaselineCorrection:Selectthisoptiontoapplya100%Tbaselinecorrection(100%TBaseline)andazero-linecorrection(0%TBaseline)to
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thesamplescan(S).Thiscorrectionisperformedwiththerawtransmissiondataandisthus:
𝑆 − 0%𝑇𝐵𝑎𝑠𝑒𝑙𝑖𝑛𝑒100%𝑇𝐵𝑎𝑠𝑒𝑙𝑖𝑛 − 0%𝑇𝐵𝑎𝑠𝑒𝑙𝑖𝑛𝑒
Withthisoption,theCarywillpromptyoutoperforma100%TBaselinefirst,followedbya0%TBaselinewhenyouperformabaselinecollection.
BasicsofmeasurementacquisitionThewavelengthrangeis1800nmto250nm.Scansnormallygofromlongtoshortwavelengths.Therearetwodetectors,aPMTandanInGaAs.Thewavelengthatwhichthesystemchangesfromonetotheother(accompaniedbyagratingchange)canbeadjusted.Usually750to800nmisagoodvalueforthischangeover.Youcanseethechangeinthespectrumwhenyoutakeabaseline(%TransmissionorReflection).Ifyouseeastepinthespectrum,itmaymeanyourbaselineisbadorthatyoursamplehasapolarizationdependency.
Setup–Thesetupbuttonlocatedintheupperleft-handcornerdefinesthescanparameters.ThefollowingusefultabscanbefoundunderSetup.
CarytabHereyoucansettheWavelengthRange,theunitsofthex-andyaxes(nm,cm-1,etc.andA,%T,%R,etc.),aswellastherangefortheaxes.Underscancontrols,theaveragetimeperdatapointandthedataintervalcanbeset.NotethattheScanRatewillbeautomaticallydeterminedfromthesevalues.
OptionstabHereyoucontroltheBeamMode,SpectralBandWidth(SBW),andSlitHeight(seeAppendixAofthisguideformoreinfo).TheDoublebeammodeneedstobeusedfortheintegratingspheremeasurementsandtheSBWistypicallysetto2nm.
TheSlitHeightcanbeusedtodecreasethebeamspotsizenormallyitissettofull.Typically,theUV-Visbuttonwillbeselected.Ifyoudonotneedtogotoshorterwavelengthsthan400nm,youcanselecttheVisbutton,whichwillturnofftheUVlamp.
Baselinetab
Thistabenablesyoutochoosethetypeofbaseline(s)thatyouwanttouseintheScanrun.ThedifferenttypesofbaselinecorrectionsareparticularlyusefulwithsomeoftheVarianaccessories.Youcancollectabaselineimmediatelybeforescanningasampleoruseastoredbaseline.
Theaccuracyofyourbaselinedeterminestheaccuracyofyourmeasurement.Youshouldperformazero/baselinecorrectionbeforerunningyoursamples
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aftertheinstrumenthaswarmedupfor~20minutesusingthesamescanparametersthatyouwilluseforyoursample.TheCaryWinUVsystemcollectsanewbaselinewhenyouselectanytypeofbaselinecorrectionintheBaselinetaboftheSetupdialogboxandthenclickBaselinebuttonintheapplicationwindow.Dependingonthetypeofcorrectionyouhaveselected,theCarywillpromptyoutoperformeitheroneortwobaselinescans.Thefirstisa100%Tbaseline(fortheDRAwiththe100%referencematerialinthesamplepositions).Thesecond,ifrequired,isa0%Tbaseline(withthesamplebeamblocked).
Oncethebaselineshavebeencollected,theywillbeautomaticallyappliedtoeachcollectedsampledatapointasitisdisplayed(indicatedbythereddisplay).Ifthereisnotacorrespondingdatapointinthecurrentbaseline,thenthefilewillbeinterpolatedtoprovidethecorrection.ThecorrectionappliedtoeachpointisdependentontheselectedbaselinetypeintheBaselinetab.
Abaselinecannotbeappliedtoasamplewherethewavelengthrangeofthesampleexceedsthatofthebaseline.Ifyouchangeyourwavelengthrangetooneoutsidethatofthebaseline,theCarywilldisplayanerrormessage.Alsotheredtextintheordinate(y)display,whichindicatesthatthebaselinecorrectionmodeisactivatedwilldisappear.
Forreflectionmeasurementsusingtheaperturekit,ifthebeamspotoverfillstheaperture,youcancorrectforthis“straylight”byperformingaZero/baselineCorrection.Normally,the0%TBaselinescanisrunbyblockingthebeambeforeitenterstheintegratingsphere,whichaccountsforelectronicnoise.Inthiscase,donotblockthebeam,butinsteadremovethereflectanceportcaptoaccountforthelightreflectingontheedgesoftheaperture(theremainderofthelightshouldpassthroughtheintegratingsphereandnotbedetected).
PerformingaZero/BaselineCorrection:Selectthisoptiontoapplya100%Tbaselinecorrection(100%TBaseline)andazero-linecorrection(0%TBaseline)tothesamplescan(S).Thiscorrectionisperformedwiththerawtransmissiondataandisthus:
(𝑆 − (0%𝑇𝐵𝑎𝑠𝑒𝑙𝑖𝑛𝑒))(100%𝑇𝐵𝑎𝑠𝑒𝑙𝑖𝑛𝑒 − 0%𝑇𝐵𝑎𝑠𝑒𝑙𝑖𝑛𝑒)
Withthisoption,theCarywillpromptyoutoperforma100%TBaselinefirst,followedbya0%TBaselinewhenyouperformabaselinecollection.
Thisbaselineoptioncorrectsforanyinherentvariationsintheelectroniczerolineoftheinstrument.Youshouldusethisbaselineoptionifyoursampleshaveareasofverylowtransmission(highabsorbance)asanyvariationsintheinstrument'szerolinewillaffectyourmeasurementsiftheyyoudonotcorrectforthese.YoushouldrefertoASTMmethodE903forfurtherdetails.
SeeAppendixBformoreinfoontheacquisition,storing,andretrievalofbaselinefiles
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IndependentTab
ThisisnormallynotchangedfromdefaultAutoinMeasurementMode.InthismodetheinstrumentwillcollectdoublespectrausingafixedSBWintheUV-VisregionandafixedenergyordetectorgainintheNIRregion.Youcanexplicitlysethowtheinstrumentcontrolsthedetectorreadingsineachregion.WitheitherAutoorFixedSBWsetastheMeasurementMode,youmustsetaSBWvalueintheUV-Visgroup.Thenormalsettingis2.00nm.YouwillfindthattheEnergylevelwillchangeautomaticallytomaintaintherequiredsignallevel.Ifyouwanttheinstrumenttosaninanothermodei.e.fixeSBEintheNIRorfixedenergy(gain)intheUV-Visregionyoucansetthathere.Storagetab
TheAutoStoretaballowsyoutospecifyifyouwanttobepromptedtostorethecollecteddata.YoucanstorethedatainaBatchorDatafileatthestartorendofacollect.Thereare3differentoptionsforautomaticallystoringyourdata
StorageOff:Selectthisifyoudonotwishtobeautomaticallypromptedtosavecollecteddata.Tomanuallystoreyourunsaveddataaftertheruniscomplete,chooseSaveDataAsfromtheFileMenu.YoucansaveyourdataasaBatchorDatafile.IntheScanapplication,dataisautomaticallystoredasaDatafile.SeetheNotebelow.
StorageOn(PromptAtStart):SelectthistodisplaytheWindowsSaveAsdialogboxatthestartofthecollectwhereyoucanentertheBatchfilenameforyourdata.
StorageOn(PromptAtEnd):SelectthistodisplaytheWindowsSaveAsdialogboxattheendofacollectwhereyoucanentertheBatchfilenameforyourdata.
NoteIntheScanapplication,PromptatStartandPromptatEndsaveinformationasa*.DSWfileunlesstherearemultiorcyclescansbeingperformed.Inthesecases,informationissavedinaBatchfile.
CommandsMenuCommandsinthisapplicationcanbeaccessedbothfromthemenuitemsatthetopofthemainwindowandfromtheapplicationbuttonsontherighthandsideofthescreen.Alternatively,youcanusefunctionkeyshortcutsforsomeofthecommands.TheseappearnexttotheitemintheCommandsmenu.
Start:SelectthistostartaScanrunusingthecurrentlysetupparameters.FunctionkeyisF9.
Stop:SelectthistostopaScanrun.IfyouhaveselectedStorageOnintheAutoStoretaboftheSetupdialogbox,alldatacollectedisautomaticallystoredinthe
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filespecifiedintheBatchnamefieldoftheWindowsSaveAsdialogboxbeforeoraftertheruncommenced.FunctionkeyisF12.Connect:TheConnectcommandbecomesavailablewhenmorethanonesoftwareapplicationisrunningatanyonetime.TheapplicationthatisinusewillbeonlineandwillhavecontroloftheCary.AllotherapplicationswillbeofflineanddisplaytheConnectcommand.Ifyouwishtoswaptoadifferentapplication(andstillkeepotherapplicationsrunning)youwillneedtoselectConnectintheapplicationyouwishtoconnecttotheCary.
Zero:SelectthistozerothecurrentordinatevalueusingtheStartwavelength(orequivalent)valuesetintheCarytaboftheSetupdialogbox.TheCarywillchangetothiswavelengthifcurrentlyidlingatadifferentvalue.FunctionkeyisF5.Donotusethisifyousampleisnotzeroatthiswavelength.Goto:SelectthistodisplaytheGotoWavelengthdialogboxandchangetheinstrumenttoanewwavelength.FunctionkeyisF4.Thisoptionisonlyavailableiftheinstrumentisnotcurrentlycollectingdata.Align:ThismovestheCaryspectrophotometerto0nm(whitelight).Youcanthenusethislightforaligningaccessories.Donotuseunlessyouhaveblockedthesampleandreferenceslotstotheintegratingsphere.LampsOff:Switchesoffalllampsources.
LampsOn:Switchonselectedlamps.
GraphmenuTheGraphmenuallowsyoutoviewdatainvariousgraphicalformatsorinmultiplegraphsintheGraphicsarea.Youcandouble-clickontheGraphicsareatotogglethedisplaythroughgraphandreporttographonly.Thegraphfunctionscanalsobeaccessedby:
• clickingoneoftheToolbarbuttons.
• right-clickinginagraphboxortheGraphicsarea.Notallfunctionsareavailableoneverymenu.
NoteTheredtraceinanygraphboxistheoneforwhichallinformationappearsandtheoneusedforcursortracking.Itiscalledthefocusedtrace.Ifyouholdthecursoroveratrace,bubbletextidentifyingthetraceisshown.
UndertheGraphmenu,youcanchangeboththeTraceandGraphPreferencesTracePreferences:SelecttodisplaytheTracePreferenceswindowtochoosethetrace(s)todisplayintheselectedgraph.GraphPreferences:SelecttodisplaytheGraphPreferencesdialogboxandchangetheappearanceofyourgraph.
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SeeAppendixCformoreoptionundertheGraphmenuaswellastheTracePreferencesandGraphPreferencesmenus
StoringDataUndertheFilemenuyoucansaveyourMethod(theSetupconfigurationusedtoperformthescan),yourData,orthecombinationoftheMethodandDataasaBatchfile.
File,SaveMethodAsSelectthisoptiontodisplaytheSaveAsdialogboxandstorethecurrentmethod.YoucanusetheSaveAsdialogboxtostorethemethod,data,report,orgraphicstemplateseparatelyortogetherasaBatchfile.ThedatacanalsobesavedasaCaryGRAMSfile,acommadelimitedASCIISpreadsheetfileorinformatssuitableforotherCarysoftwaresystems(dependsonwhichapplicationyouarerunning).
File,SaveDataAs
SelectthisoptiontodisplaytheSaveAsdialogboxandstorethecollecteddata.YoucanusetheSaveAsdialogboxtostorethemethod,dataorreportseparatelyortogetherasaBatchfile.ThedatacanalsobesavedasaCaryGRAMSfile,acommadelimitedASCIISpreadsheetfileorinformatssuitableforotherCarysoftwaresystems(dependsonwhichapplicationyouarerunning).Afterabatchfilehasbeensaved,youcanusethisoptiontomanuallysavethefileasamethodfile,abatchfile,acommadelimitedASCIIspreadsheetfileoraRichTextFormatfile.
HowtoExportCollectedDataIfyouwanttoexportdatafromaCaryWinUVapplicationintoathird-partyapplication,thensaveyourdataasanASCII*.CSVfile.Todothis:
1. ClickFilemenuitem.2. ClickSaveDataAs.TheSaveAsdialogboxwillappear.3. ClickthedownarrownexttotheFilesoftypelistbox.4. SelectSpreadsheetASCII(*.CSV).5. TypeyourfilenameintotheFilenamefield.6. ClickSavetoexportyourdata.
HowtoCombineDataFilesintoaBatchFile:
Ifyouhaveanumberofdatafilesthatyouneedtocombineintoabatchfile,thenyouneedto:
1. SelectOpenDatafromFilemenu.2. Alistofpreviouslystoredbatchfileswillappear.Clickthedownarrowat
therightofthe“FilesofType”listboxandselect'Data'tolistallthedatafiles.
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3. ChecktheOverlayDatacheckbox.4. HighlightthedatafilesthatyourequireandclickOpen.Thehighlighted
datafileswillloadintotheapplicationandappearinthesamegraphbox.
5. SelectSaveDataAsfromtheFilemenu.6. Alistofpreviouslystoreddatafileswillappear.Clickthedownarrowat
therightofthe“FilesofType”listboxandselect'Batch'tolistallthebatchfiles.
7. MakesurethattheSaveonlyfocusedtracecheckboxisnotchecked.8. IntheFilenamefield,typeinthefilenameforyournewbatchfile.9. ClickSavetocreatethenewbatchfile.Thecurrentmethodwillbestored
withthebatchfiles.Allthedatafilesarenowcombinedintotheonebatchfile.
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AppendixA
HowtheCary5000/6000iControlsSBWandEnergyInaspectrometertheintensityobservedbythedetectorchangeswithwavelength.Doublebeamspectrometersnormallycontrolthereadingfromthedetectorstomakesurethattheystaywithintheiroptimumregion.Thiscanbedoneintwoways.Youcanopenandclosetheslitstoincreaseordecreasetheamountoflightthatreachesthedetectororyoucanchangethegainonthedetectortomakeithavehighergainwhenthelightenergyislowandvisaversa.NormallyonelikestohavetheSpectralBandWidth(SBW)stayconstant(i.e.constantslitwidth).ThisiseasyintheUV-Visregionwherethedetectorisaphotomultipliertube(PMT)thatallowsaverylargechangeingain.However,intheNIRregionthishistoricallywaslesspossiblesinceyouareusingaPbSdetector.ThuswhatwasdonewastolettheSBWvarytomaintainthedetectoroutput.InourCarywehaveaInGaASdetectorandwhileyoucannotchangethegainonthedetectoritisverylownoiseandyoucanuseaamplifierwithsetablegainafterthedetectortobostthesignal.InDoubleorDoubleReverseBeamModeintheUV-Visregiontheslitwidth(SBW)isnormallykeptconstantandtheEnergylevel(gain)ischanged.IntheNIRregion(InGaAsdetector)thereverseisnormallytruei.etheEnergylevelisconstantandtheSBW(slits)changes.Duetotheinherentdifferencesbetweenthetwotypesofdetector,thedifferentmethodsofcontrolnormallyensurethewidestdynamicrangeandthebestsignaltonoise.
Theinstrumentusestwodetectors(PMTandInGaAsdiode),twolightsources(WbulbandD2lamp),andtwogratingsinthemonochromator.Youcansetthewavelengthatwhichthedetectorsandgratingschange.Bothofthesearetypicallysetat800nm,ifyouhaveanimportantspectroscopicfeatureat800nm,youcanmovethechangeover±50nm.Thelampchangeoverisnormallysetto350nmbutagaincanbemoved±50nm
Notethattheinstrumentusesgratingstodispersethelightandneedsordersortingfilterstoremove2nd(and3rd)orderlightfromtheoutputbeam(i.e.at800nmyouwouldalsoget400and200nmlight).Thefilterschangeareat350,570,800,and1200nm.Youcannotmovetheirchangeoverwavelengths.IfyouarecollectingdataindoublebeammodeintheUV-Visregions,youcansethowtheinstrumentcontrolsthedetectorreadings.InSETUPundertheindependenttabifyouchoosehowthedoublebeamspectraarecollected.WitheitherAutoorFixedSBWsetastheMeasurementMode,yousetaSBWvalueintheUV-Visgroup.Thenormalsettingis2.00nm.YouwillfindthattheEnergylevelwillchangeautomaticallytomaintaintherequiredsignallevel.
IfyouarecollectingdataindoublebeammodeintheNIRregion(λ >thedetectorchangewavelengthsetting,generally800nm),witheitherAutoorFixedEnergysetastheMeasurementMode,theEnergylevelisfixedintheNIRgroup.AnEnergysettingof1.0willprovidethebestsignal-to-noiseratiobutwithalargerSBW.Inmostcases,therecommendedsettingis3.0;thisprovidesasmallerSBWovertheentireregionanda
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bettermatchoftheSBWintheNIRregionandtheVisregion.YouwillfindthattheSBWwillchangeautomaticallytomaintaintherequiredsignallevel.IfyouarecollectingdataindoublebeammodeacrosstheUV-VisandNIRregionswithFixedSBWsetastheMeasurementModethenyouwillneedtoentervaluesintheSBWfieldsinboththeUV-VisandtheNIRgroupboxes.ThevaluescanbethesameifyouwanttousethesameSBWacrossthewholescanoryoucansetdifferentvaluesforeachregion,normallytheSBWintheNIRis>>thentheSBWintheUV-Vis.NotethattheSBWisinnmandforafixedsettingoftheSBWtheresolutioninenergytermswillbemuchbetterintheNIRthenintheUVorVisregions.Aspectrabandwidthof2nmat400nmcorrespondsto124cm-1whileat1200nm124cm-1giveaSBWofabout18nm.ThisisonereasonthatmostabsorptionpeaksintheNIRaremuchbroaderinwavelengththenpeaksintheUV-Visregions.
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AppendixB:Acquiring,storing,andretrievingbaselinefilesTheCaryWinUVsystemcollectsanewbaselinewhenyouselectanytypeofbaselinecorrectionintheBaselinetaboftheSetupdialogboxandthenclicktheBaselinebuttonintheapplicationwindow.Dependingonthetypeofcorrectionyouhaveselected,theCarywillpromptyoutoperformeitheroneortwobaselinescans.Thefirstisalwaysa100%Tbaseline(withnothinginthebeam,orinthecaseofaDiffuseorSpecularReflectancemeasurements,withthe100%referencematerialinposition).Thesecond,ifrequired,isa0%Tbaseline(withthesamplebeamtotallyblockedsothattheinstrumentcanmeasuretheelectroniczerovalues).
Oncethebaselineshavebeencollected,theywillbeautomaticallyappliedtoeachcollectedsampledataaccordingtotheappropriatebaselinecorrectionequation.Ifthereisnotacorrespondingdatapointinthecurrentbaseline,thenthefilewillbeinterpolatedtoprovidethecorrection.ThecorrectionappliedtoeachpointisdependentontheselectedbaselinetypeintheBaselinetab.Abaselinecannotbeappliedtoasamplewheretheabscissarangeofthesampleexceedsthatofthebaseline.Ifyouchangeyourabscissarangetooneoutsidethatofthebaseline,theCarywilldisplayanerrormessage.Alsotheredtextintheordinatedisplaywhichindicatesthatbaselinecorrectionmodeisactivatedwilldisappear.
NotthatallvalueswithintheBaselineabscissarangearecorrected,eventhevaluedisplayedwhiletheCaryisidlingataparticularwavelength.
NoteYoushouldbecarefulapplyingcorrectionstosampleswherethefollowing
parametersaredifferentinthebaselinefileandthesamples.Energy,SBW,BeamMode,SourceChangeover,DetectorChangeoverGratingChangeover,SelectedLampforthecollection,Signal-to-NoiseMode,SlitheightandtheIndependentControl.
Baselinesaresavedasapartofabatchfile.However,ifyouwant,youcanalsostorethebaselinesbythemselvesinabaselinefilewithoutthecollecteddata.TodothisyousimplyselecttheBaseline(*.CSW)astheSaveAsTypeintheSaveAswindowaccessedfromtheFile|SaveDataAsmenuitems.WhenyouwanttousethebaselinesforanotherScanrun,yousimplyopenthefileusingeithertheFile|OpenDatacommandorclicktheBaselinebuttonintheBaselinetaboftheSetupdialogbox.
NoteIfyoudecidethatyoudonotwanttousethatstoredfile,butwanttocollectanewbaselineinstead,thentheCarywillusethenew,collectedbaselineinallcorrections.However,theBaselinetabwillstilldisplaythenameofthebaselineinthebaselinefile.Youneedtosavethecollecteddataasabatchfileifyouwantthenewbaselineincludedinthatfile.
NoteAllcorrectionsareperformedwiththerawtransmissiondatathatcomesdirectly
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fromtheinstrument.ThesetransmissionvaluesarethenconvertedintotheselectedYmodefordisplay.
Abaselinecannotbeappliedtoasamplewheretheabscissarangeofthesampleexceedsthatofthebaseline.IfyouwishtousethatbaselinethenyouwillneedtoreducetherangeofthescanbychangingtheStartandStopfieldsontheCarytaboftheSetupdialogbox.
Typesofbaselinesthatcanbeperformed.ChoosethetypeofbaselinecorrectionundertheBaselinetabintheSetupmenu
BaselineCorrection
Selectthisoptiontoapplyabaselinecorrection(Baseline)tothesamplescan(S)thatiscollectedfromtheinstrumentastransmissionvalues.Thiscorrectionisthus:
𝑆𝐵𝑎𝑠𝑒𝑙𝑖𝑛𝑒
Zero/BaselineCorrectionSelectthisoptiontoapplya100%Tbaselinecorrection(100%TBaseline)andazero-linecorrection(0%TBaseline)tothesamplescan(S).Thiscorrectionisperformedwiththerawtransmissiondataandisthus:
S− 0%TBaseline100%TBaseline− 0%TBaseline
Withthisoption,theCarywillpromptyoutoperforma100%TBaselinefirst,followedbya0%TBaselinewhenyouperformabaselinecollection.
Thisbaselineoptioncorrectsforanyinherentvariationsintheelectroniczerolineoftheinstrument.Youshouldusethisbaselineoptionifyoursampleshaveareasofverylowtransmission(highabsorbance)asanyvariationsintheinstrument'szerolinewillaffectyourmeasurementsiftheyyoudonotcorrectforthese.YoushouldrefertoASTMmethodE903forfurtherdetails.
ZeroSRAcorrectionSelectthisoptiontoapplya100%Tbaselinecorrection(100%TBaseline)andazero-linecorrection(0%TBaseline)toasample(S)measuredwithanAbsoluteVWSpecularReflectanceAccessory(SRA).
NoteTheVNSRAandthesinglebouncerelativeSRAaccessoriesshouldnotusethiscorrection.SelectaBaseline/Zerocorrectioninstead.
Thiscorrectionisperformedwiththerawtransmissiondataand,duetothedoublebounceonthesample,isthus:
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S− 0%TBaseline100%TBaseline− 0%TBaseline
Withthisoption,theCarywillpromptyoutoperforma100%TBaselinefirst,followedbya0%TBaselinewhenyouperformabaselinecollection.YoushouldrefertoASTMmethodE903forfurtherdetails.Zero*Std.Ref.Correction
Selectthisoptiontoapplya100%Tbaseline(100%TBaseline)correctionandazero-linecorrection(0%TBaseline)toasample(S)measuredwithareflectanceaccessorywhichisnotabsolute(e.g.,aDiffuseReflectanceAccessoryortheVariableAngleSpecularReflectanceaccessory).TheCarythenmultipliestheresultbytheappropriatevalueinthe'BaselineStdref'filewhicharethetransmissionvaluesassociatedwiththeStandardReferencematerialyouusedtoestablishthebaseline.RefertothehelpfortheDiffuseRelectanceaccessoriesforfurtherdetailsaboutStandardReferencematerials.
Thiscorrectionisperformedwiththerawtransmissiondataandisthus:S− 0%TBaseline
100%TBaseline− 0%TBaseline Baseline Stdref
Withthisoption,theCarywillpromptyoutoperforma100%TBaselinefirst,followedbya0%TBaselinewhenyouperformabaselinecollection.
NoteIfyouselectthisoptiontheBaselinebuttoninthemainwindowwillnotbeenableduntilyouhaveretrievedaStdReffile.ClickthisbuttontobrowseforandselectaStdReffile.Thisfilemustbeinthecorrectformat.
KnownMirrorSelectthisoptionwhenyouareusingaVWSpecularReflectanceAccessory(SRA)withasmallsampleorasampleoflowreflectance.RefertoyourSRAmanualformoreinformation.KnownMirrorCorrection
Thecorrectionequationisasfollows:S− 0%TBaseline
100%TBaseline− 0%TBaselineKnown mirror corrected
where
Known mirror corrected =known mirror− 0%TBaseline100%TBaseline− 0%TBaseline
TipIfbaselinecorrectionisactivated,thetypeofcorrectionthattheCarywillapplywillappearintheinred.
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However,sometimesyoumaynoticethatthetexthasturnedtograyandisinitalics.ThisindicatesthattheCaryiscurrentlyidlingoutsidetheabscissarangeofthebaselinefile,butthatthecurrentmethodStart/Stopparametersdonotexceedtheabscissarangeofthebaseline.
RetrieveBaselineFile
ThisbuttondisplaystheWindowsOpendialogboxwhereyoucanselectastoredbaselinefile.Thetrace(s)inthisfilewillbeusedfortheselectedbaselinecorrection.ThenameoftheselectedfileappearsnexttotheBaselinebutton.
TipIfyouwanttousethebaselineagainwithothersamples,savethemethodusingFile|SaveMethodAs.Then,whenyoure-openthemethod,thebaselinewillalsoopenandbereadytouse.Itispreferabletosavethebaselinewiththemethod,ratherthanabaselinefile,asthatwayyoucanbesurethatallyourcollectionparametersareexactlythesameforthenewScanruns.However,GoodLaboratoryPracticerecommendsthatyoucollectanewbaselineforeachlaboratorysession.
ViewBaselineFileThisdisplaysthetracesintheselectedbaselinefileintheGraphicsarea.
RetrieveStdRefFile
ThisbuttondisplaystheWindowsOpendialogboxwhereyoucanselectastoredreferencefile.ThetraceinthisfilewillbeusedintheZeroxStdRefCorrection.ThenameoftheselectedfileappearsnexttotheStdRefbutton.
TipTheStdReffilemustbeinthevalidformat.Youcanobtainthesefilesfromthemanufacturerofthestandardthatyouareusing.
• Howtocreateanduseastandardreferencefile
Q.WhyismyRetrieveStdRefbuttonunavailable?A.YouneedtoselecttheCorrectiontypeas'Zero*Std.Ref.Correction'.
ViewStdRefFileThisdisplaysthetracesintheselectedstandardreferencefileintheGraphicsarea.
ShowStatusDisplaySelectthischeckboxtodisplaytheShowStatuswindow.Thiswindowallowsyoutoviewthestatusofvariousparametersduringthedatacollection.
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AppendixCGraphmenu,TracePreferencesandGraphPreferencesoptions
1) GraphmenuoptionsPrintXYpoint:Selectthistoprintthecursor'scurrentXandYcoordinatesinthereportarea.Thisoptionisonlyavailablewhenright-clickinginagraphbox.
TracePreferences:SelectthistodisplaytheTracePreferenceswindowtochoosethetrace(s)todisplayintheselectedgraph(TracePreferencesarelistedbelow).GraphPreferences:SelectthistodisplaytheGraphPreferencesdialogboxandchangetheappearanceofyourgraph.Anychangesyoumaketotheappearanceofthegraphwillapplytoallgraphsuntilthesettingsarechangedagain.(Graphpreferencesoptionsarelistedbelow).
CursorMode:SelectthistodisplaytheCursorModesdialogboxtoenableyoutousedifferentcursorsonthescreen.Youcanselecttouseafreecursorthatcanmoveanywhereinthegraphorexactlytracethefocusedscan(redscan).
AxesScales:SelectthistodisplaytheAxesScalesdialogboxandchangetherangeoftheaxes.
Autoscale[XY]:SelectAutoscale[XY]toautomaticallyscalecollecteddatabyscalingtheordinate(Y)heightandabscissa(X)widthtofullscreen.
Autoscale[X]:SelectAutoscale[X]toautomaticallyscalecollecteddatabyscalingtheabscissa(X)widthtofullscreen.Autoscale[Y]:SelectAutoscale[Y]toautomaticallyscalecollecteddatabyscalingtheordinate(Y)heighttofullscreen.
ZoomOut:SelectZoomOuttoZoombacktotheoriginalXandYaxisscalingsetintheCarySetuptab.Thiswillundoallzooming.
AddLabel:SelectAddLabeltodisplaytheAddLabeldialogboxtoenableyoutoplaceatextlabelonyourgraph.
AddPicture:SelectAddPicturetodisplaytheAddPicturedialogboxtoinsertapicture,bitmaporchemicalstructureintoyourgraph.EditAnnotation:SelectEditAnnotationtoalterthecontentorlookofanannotation(suchasalabelorapicture)intheGraphicsarea.DeleteAnnotation:SelectDeleteAnnotationtoremoveanannotation(suchasalabelorapicture)fromtheGraphicsarea.
Single/MultiGraph:SelectSingle/MultiGraphtotogglebetweendisplayingoneorallgraphs.AutoArrangeGraphs:SelectAutoArrangeGraphstoviewandarrangeallgraphssimultaneously.
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CopyGraph:SelectthistocopytheGraphicsareaontotheWindowsClipboard.
PastetoGraph:SelectthistopastethecontentsoftheWindowsClipboardintotheGraphicsarea.Textispastedasalabel;graphicsarepastedaspictures.
AddGraph:ClickAddGraphtoaddanewgraphboxtotheGraphicsarea.RemoveGraph:ClickRemoveGraphtodeletetheselectedgraphboxfromtheGraphicsarea.
ClearAllTraces:SelectClearAllTracestodeletealltracesfromthegraph/s.UserDataForm:SelectthistodisplaytheUserDataForm.
Maths:SelectthistoenabletheMathswindow.Thisoptionisonlyavailablewhenright-clickinginagraphbox.HistoryList:Thisdisplaysalistofthecurrentgraphs.
2) TracePreferencesAsinglegraphboxcandisplaymanytraces.Thiswindowenablesyoutoselectthetrace(s)todisplay(makevisible)intheselectedgraphboxorcolorspace.TracePreferencesisaccessiblefromtheGraphmenu,byright-clickingonatraceorbyclickingonthetoolbar.
TheTracePreferencesmenuisalsoavailablebyright-clickinganywhereinthetracelisting.
Visible:Thisfieldallowsyoutodeterminewhichtraceswillappearontheselectedgraph.Clickinthiscolumntoplaceaticknexttothetraceyouwanttoappearonthegraph.Clickagaintoremovetheticknexttothetrace.
Ifyouareinsinglegraphview,allselectedtraceswillappearontheonegraph.IfyouareinMultiGraphview,thetraceswillappearonthegraphthatiscurrentlyselected.
Color:Thisshowsthecolorinwhichthetracewillbedisplayedinthegraphbox.Theredtraceinanygraphboxistheoneonwhichallinformationappearsandtheoneusedforthecursortracking.Itiscalledthefocusedtraceanditisalwaysred.
ClickingonatraceintheColorcolumnwillcausethattracetobecomethefocusedtraceintheselectedgraphbox.Youcanalsochangethecolorofanytrace(whenitisnotthefocusedtrace),fromtheTracePreferencesmenu.
WhenyouchangethetracelinewidthintheGraphPreferencedialogbox,italsowillchangethewidthofthecolortracelineinthiswindow.
NameofTrace:Thisfieldcontainsadescriptionofthetracescurrentlyavailablefordisplayintheselectedgraphbox.Ifatraceisnotalreadytickedasvisible,youcanclicktoactivatethisproperty.Right-clickinginthiscolumndisplaystheTracePreferencesmenu.Thismenuallowsyoutochangesomeofthepropertiesofthetraces,aswellashiding,displayingordeletingcertaintraces.
Youcanresizethe“NameofTrace”and“File”namefieldsbyselectinganddragging
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thesplitterbarbetweenthefields.
FileName:Thisfielddisplaysthefilenameandpathofthetrace.Ifthenameistoolongtoappearinthefield,youcanusethearrowkeystoscrolltotheendofthefilenameoryoucanmaximizetheTracePreferenceswindow.Ifthefilepathforatraceshows'notsaved',thetraceisunsaveddataandisonlystoredinmemory.TraceAuditLog:Thisfielddisplaysinformationaboutthetracethatishighlighted.Itincludesinstrumentparametersanddataforminformationrelatingtothetracethathasbeenselected.Whenmorethanonetraceishighlighted,thisdisplaysinformationonthetracethatwaslastselected.
SelectTraces:Thedrop-downarrowrevealsanycolumnsyouhavecreatedintheUserDataForm.Youcanselecttracesbasedonanyofthecolumnsyouhavecreated.
3) GraphPreferencesThisdialogboxallowsyoutochangetheappearanceofyourgraph.GraphPreferencesisaccessiblefromtheGraphmenu,byright-clickingonatraceorbyclickingGraphpreferencesicononthetoolbar.AllgraphswillappearlabeledwiththeXaxislabelbeinghorizontalandtheYaxisvertical.Youcannotchangetheorientationoftheselabels.However,youcanalterthefontandsizeoftheaxesandtheirlabels.Anychangesyoumaketotheappearanceofthegraphwillapplytoallgraphsuntilthesettingsarechangedagain.
StandardTab:Thistaballowsyoualterthewayyourgraphappearsonscreen.YoucanviewthechangesyoumakebeforeacceptingtheminthePreviewbox.PreviewBox:Apreviewofeachoftheaxesvariablesisshowntotherightofthisdialogbox.Tochangetheview,alterthesettingsinthevariablesontheleft.AxesColor:Fromthedrop-downlist,selectthecolorthatyouwanttoassigntotheaxesofthegraph(s).
AxesWidth:Fromthedrop-downlist,selectthewidthoftheaxes.Thewidthisgiveninpixelsandrangesbetweenoneandfivepixels.
GridStyle:Thisdrop-downlistallowsyoutospecifywhetherornotyouwantagridonyourgraph.Youcanalsodefinethetypeofgrid.PlotAreaColor:Thisdrop-downlistenablesyoutospecifywhat(ifany)coloryouwouldlikeasthebackgroundofthegraph.TraceWidth:Fromthisdrop-downlistyoucanselectthewidthofthetrace.Thewidthisgiveninpixelsandrangesbetweenoneandfivepixels.
Font:ThisbuttondisplaystheWindowsFontdialogboxthatallowsyoutodefinethefontstylefortheaxesofthegraph(s).Thestyleandsizeofthefontwillbeappliedtoallgraphsuntilthefontischangedagain.
TraceStyle:Thisfieldallowsyoutodefinethewaythatyourtracewillappearonscreen.
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Points EachindividualdatapointcollectedbytheCaryisshownonthegraph.
Pointsandsolidlines
EachindividualdatapointcollectedbytheCaryisshownonthegraph.Aninterpolatedlineisdrawnconnectingthepoints.
Solidlines TheCarysysteminterpolatesthedatabetweentheactual,collecteddatapointsandshowsthedataasacontinuousline.
Stylecyclesautomatically
TheCarysystemwillgiveeachtraceoneoftheabovestylesmakingiteasiertodifferentiatebetweentraces,especiallyonblack-and-whiteprinters.StylecyclingwillonlyoccurwhentheTraceWidthhasbeenselectedat1pixel.
AdvancedTab:Thistaballowsyoutofurtherrefinethewayyourgraphlooks.ForeachoptionyoucanmakeindividualchangestotheX,Yorbothaxes.
Autotickmarks:Usethesliderbarstoalterthenumberoftickmarks(graduations)thatyouwanttoappearonyourgraph.IfyouhaveselectedtheMajorTickscheckbox,thisoptionisunavailable.Majorticks:Selectthistodeterminehowmanytickmarks(graduations)youwanttoappearoneachaxisofyourgraph.
Decimals:Selectthistodeterminehowmanydecimalplacesyouwanttoassigntoeachtickmark(graduation)onyourgraph.
ShowLegend:Selectthistodisplayalegendontherightsideofeachgraphbox.Asingleclickonasamplenameorexamplelinewithinthelegendwillmakeitthefocusedorredscan.InformationaboutthetracewillbedisplayedbelowtheXaxis.
Double-clickingthelegendwillautomaticallydisplaytheTracePreferenceswindow,allowingyoutoviewmoredetailedinformationaboutyourtrace(e.g.,auditlog,filename,etc.).