User guide for Cary 5000 absorption spectrometer with ...mmrc.caltech.edu/Cary UV-Vis...
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1 User guide for Cary 5000 absorption spectrometer with external DRA 1800 attachment. (last updated 10/25/2017) This guide is for use of the Cary 5000 with the DRA only. For use without the DRA as a standard transmission spectrometer see the User guide for Cary 5000 in absorption mode. Important warnings! • Do not unplug or plug in the external DRA attachment when the instrument is on. This will ruin the detectors of the integrating sphere • Do not put white light into the DRA with the DRA electrically connected to the Cary. • Minimize the amount of time that the integrating sphere is open. Long-term light exposure hurt the detector over time. • Wear clean gloves while using the instrument • Do not use liquid or powder samples in the integrating sphere. Quick Start for using DRA 1. Turn on computer 2. Click on the Cary Scan icon on the taskbar 3. Check lens and mirror are correct for your measurement. (Ware gloves to change the mirrors or lens). a. Install Small Sample Kit mirror (M3 SSK) or regular M3 mirror if needed b. If using SSK install correct lens L2. 4. Make sure cover for the DRA is fully closed and turn Cary on. 5. If you get an error turn go to the section below on Startup Errors. off 6. Wait 20 minutes for the lamps to warm up. 7. If you need to change and/or align the optics see the local user manual below and remember never put white light into the integrating sphere when the Cary is turned on. To align the instrument use 550 nm light. 8. Select Setup a. set wavelength range, %T or %R b. Under Options tab: set slit width and height, SBW to 2 nm, Detector and Grating change wavelengths c. Under Baseline tab: chose zero/baseline d. Under Storage tab: Set your filename 9. Make sure that all exits of the integrating sphere are blocked with full reflectors. When using the small spot kit you must take care that the full reflectors completely cover the exit ports with their white reflector material.
Transcript of User guide for Cary 5000 absorption spectrometer with ...mmrc.caltech.edu/Cary UV-Vis...
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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.).
