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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.).