FTIRTroubleshooting

SomecommondifficultiesencounteredwhentakingFTIRspectraarelistedbelow.Pleasecontactthe
toolmanagerforfurtherhelp.

Nosignal:
Problem:Cannotseepeaksatallrelativetobaselinenoise.
Causes:SamplenotincontactwithsurfaceORbeammisaligned.
Solutions:
VerifysampleisfaceDOWN.
GotoCheckSignaltabintheDataCollectionwindow,andverifythatsignalisconsistentwithlisted
values.Ifnot,contactNBTCstaffforassistance.
Putthesampleinfirmcontactwiththesurface,ifusingATRmakesurethesampleisclampedfinger
tight.
Verysmallparticlescanimpedesignaltry1)cleaningATRcrystalwithIPAandacottonswab
orlenspaper(noKimwipes!)and2)puttingapieceoflenspaper(notaKimwipe)betweenthe
sampleandATRandpullingthelenspaperout.

Lowsignal:
Problem:Peaksverysmallcomparedtobaselinenoise.
Causes:Insufficientsignal
Solutions:
UseliquidnitrogencooledMCTdetector.
Increasenumberofrunspermeasurement(shouldntneedmorethan256evenformonolayers).
Increasesamplethickness,ifpossible.
Uselargersamplemask(forVeeMAX)
Verysmallparticlescanimpedesignaltry1)cleaningATRcrystalwithIPAandacottonswaborlens
paper(noKimwipes!),then2)puttingapieceoflenspaper(notaKimwipe)betweenthesampleand
ATRandpullingthelenspaperout.

Noisybaseline:
Problem:Sharppeaksaround40003500and20001300cm1,ascanbeseeninthelightbluetrace
below(Darkblueisofthesameblanksample):

Othernotes:Primarilyaproblemforsampleswithlowsignalmonolayersetc.Samesamplewillchange
overtimeIntheexamplebelow(absorbance):Bluetraceisimmediatelyafterpumpingdown,pinkafter
severalminutes,andbrownisseveralminutesafterthat.Notethatthepeaksaround14001600cm1
areobscuringimportantspectroscopicdatathatcanbeseeninthepinktrace.

Cause:Atmosphericwatereithermoreorlessofitcomparedtobackground.
Solutions:
Pumpdownthechamberforaboutthesameamountoftimeaswasdoneforthebackground
spectrum.
Takemultiplespectraoverseveralminutesandselecttheonewheretheatmosphericwaterpeaksare
smallest.
Tominimizetheamountofwaterinthesystem,pumpdown,ventwithoutusingtheairbypass,and
pumpdownagain(thiswillpurgethechamberwithnitrogen).
Ifyourestillhavingdifficulties,retakingthebackgroundspectrummaybehelpful.

TriangularPeak
Problem:Largetriangleshapedpeakaround2200cm1,whenusingdiamondATRsetup.
Othernotes:Maynotoccuronallsamples.Seespectrabelowforanexample:

Causes:Refractiveindexmismatch(SiliconondiamondATR).
Solutions:UsegermaniumATRcrystalwithVeeMAXsampleholdercontactNBTCstaffforassistance.

ErrantPeak
Problem:Doubletpeakaround2350cm1,ascanbeseeninthelightbluetracebelow(Darkblueisof
thesameblanksample):


Othernotes:Morefrequentlyseenatatmosphericpressure.Samesamplewillchangeovertime.
Causes:Atmosphericcarbondioxide
Solutions:
Ifworkingwithanonvolatilesample,pumpingdownthechamberforthebackgroundandsample
spectrashouldremovethispeak.
Ifworkingwithliquidsorothervacuumsensitivesamples,letthesamplesitinthecoveredchamberfor
severalminutesbeforetakingameasurement,asthechamberisnitrogenpurged.
Takemultiplespectraoverseveralminutesandselecttheonewherethedoubletpeaksaresmallest.

Ringing:
Problem:Spectrathatlookliketheonebelow,withcontinuouswavyfeaturesthatobscuresample
peaks.


Othernotes:Theringingmaynotoccuronallsamples.Itmayhappenonyourbackgroundsampleifyou
rerunit.Theexactwavelengthatwhichthepeaksappearmayvary.Youmayseesamplepeaks
transposedovertheringingsection(asseenhereataround1650cm1).
Causes:MostfrequentlycausedbytheIRbeamreflectingofftheundersideoftheVeeMAXsample
holder.
Solutions:
Preparealargersampletousewiththelargersamplemask(5/8diameterrecommended).
UsetheVMaxatanongrazingangle(<60).
RecoatingtheundersideofthemaskcontactNBTCstaffforassistance.
AdjustaperturesizecontactNBTCstaffforassistance.