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HowtoprepareIRsamples?

1.Materialsforsamplepreparation

ThefollowingtableliststhetypicalIRmaterialsforvariousapplications.TheseIRmaterialsare
usedforIRwindowordiluents.Itisworthynotingthathygroscopicmaterialsaresuitablefor
organicsampleswhilenonhygroscopicmaterialsareusedforwatercontainingsamples.

2.Samplepreparationfortransmissionanalysis

2.1Solidsamples
(2.1.1)Thinplatesamples
Youcanusestandardmagneticplatesampleholder.

(2.1.2)Powdersamples
Youcanpresspowderintoapellet.Inthismethod,youcanselectdifferentdiluents(matrixes)
forvariousapplications.FormidIRfrequencyrange,KBr,KClordiamonddustcanbeused.For
farinfraredtesting,highdensitypolyethylene(HDPE)ordiamonddustissuitable.Fornear
infraredanalysis,CsIorKBrcanbeselected.YoucanprepareaKBrPelletasfollows:

(a)ThepowdersampleandKBrmustbegroundtoreducetheparticlesizetolessthan5mmin
diameter.Otherwise,largeparticlesscattertheinfraredbeamandcauseaslopebaselineof
spectrum.
(b)AddaspatulafullofKBrintoanagatemortarandgrindittofinepowderuntilcrystallites
cannolongerbeseenanditbecomessomewhatpastyandstickstothemortar.

(c)Takeasmallamountofpowdersample(aboutof0.12%oftheKBramount,orjustenough
tocoverthetipofspatula)mixwiththeKBrpowder.Subsequentlygrindthemixturefor35
minutes.
(d)Assemblethediesetasshowninthedrawing.Whenassemblingthedie,pleaseaddthe
powdertothe7mmcollar.PutthedietogetherwiththepowderintotheQwikHandiPress.
Pressthepowderfor2minutestoformapellet.AgoodKBrpelletisthinandtransparent.
Opaquepelletsgivepoorspectra,becauselittleinfraredbeampassesthroughthem.White
spotsinapelletindicatethatthepowderisnotgroundwellenough,orisnotdispersed
properlyinthepellets.
(e)Disassemblethediesetandtakeoutthe7mmcollar.Putthecollartogetherwiththepellet
ontothesampleholder.
(f)Pleasecleanthedieafteryoufinishyourexperiment.

ItisworthynotingthatBrfromtheKBrcanoftenreplaceligandsinthecompoundwhose
spectrumisdesired.

2.2.Liquidsamples
(2.2.1)Makingasandwich
TopreparealiquidsampletoIRanalysis,firstlyplaceadropoftheliquidonthefaceofahighly
polishedsaltplate(suchasNaCl,AgClorKBr),thenplaceasecondplateontopofthefirstplate
soastospreadtheliquidinathinlayerbetweentheplates,andclampstheplatestogether.
Finallywipeofftheliquidoutoftheedgeofplate.Youcanmountthesandwichplateontothe
sampleholder.Afterfinishingyourexperiment,cleantheplateswithisopropanol(Nowater!)
andreturnthemtothedesiccators.

Precaution:Volatileliquidcantbepreparedwiththismethod,becauseitwillevaporatewhile
itsspectrumisbeingobtained.Iftheliquidsampleistoxicorsmelly,pleasedontusethis
method.Inaddition,NaClandKBraredissolvedintowater,andthustheycantbeusedfor
aqueoussamples.

(2.2.2)Usingaliquidcell
ThethermoNicoletdemountablepathlengthcellisdesignedforliquidsample.Assemblethe
cellasshowninthedrawing.Thenuseasyringetofilltheliquidintothecell.Finallysealthe
cell.

3.SamplepreparationforATRanalysis
Thestronglyinfraredadsorbingmaterialssuchasrubbers,polymerfilmsandaqueoussolutions
canbeanalyzedbytheattenuatedtotalreflection(ATR)technique.Minimumornosample
preparationisrequiredforATRanalysis.Therearetwokindsofcrystalsavailableatour
laboratory,i.e.,45ZnSeand45Ge.

3.1Solidsamples
Forsolidsamples,pleaseusetheflatcrystal.Toobtainthebestresults,therecommended
sampledimensionis7590mmlong1625mmwide<4mmthick.Thesamplesurfacemustbe
flat,otherwiseintimatecontactbetweenthesampleandtheATRcrystalcannotbeobtained.

Firstlyplaceasampleontopsurfaceofthecrystal.Thenplacethegripperplateonthesample.
Adjustthepressureappliedtothegripperplatetoensuretheconsistentcontactisachieved
betweenthecrystalandthesample.Precaution:ifyoufindaconsiderableforceisnecessaryto
overcometheresistance,STOP!Excessivepressurecancrackandpermanentdamagethe
crystal.Also,thecrystalmustbekeepcleanandscratchfree.Scratchesaffectthe
sample/crystalcontactandthushavesignificantinfluenceonthedepthofpenetration.

3.2Liquidsamples
Forliquidsamples,pleaseusethetroughcrystal.Fillthetroughplatewithyourliquidsample.
Thenplacethecoveroverthetroughplate.
Precaution:Ensuretheliquidsampledoesnotattackthecrystal.

Afteryouhavefinishedyourexperiment,cleanupthecrystalusingpropersolvents(Acetoneor
watercanbeusedforZnSeandGe).

4.SamplepreparationforPMIRRASmeasurement
Typically,youcandepositametalfilmontheregularglassslide(orsiliconwafer).The
metal/glasscombinationcanbeactedasthereferencesample.Inaddition,youwilldeposita
monolayer(ororganicfilm)overthemetalfilm.Hence,youwillhavetwosamples,i.e.,the
metal/glasscombinationandthemonolayer/metal/glasscomposite.Therecommended
dimensionofsampleis55~75mmx17~25mm.

References:
Samplingcatalogue,ThermoNicolet.