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How To Prepare Ir Samples

1. There are several methods for preparing IR samples for transmission or ATR analysis depending on whether the sample is a solid, liquid or powder. Common materials used include KBr, NaCl, and various IR transparent crystals. 2. For transmission of solids, thin plates or powders pressed into pellets with diluents can be used. For liquids, a sandwich of liquid between plates or a liquid cell can be employed. 3. For ATR, solids can be placed directly on flat or trough crystals while liquids are placed in a trough. Minimum sample preparation is needed for ATR.

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Huy Pham
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124 views

How To Prepare Ir Samples

1. There are several methods for preparing IR samples for transmission or ATR analysis depending on whether the sample is a solid, liquid or powder. Common materials used include KBr, NaCl, and various IR transparent crystals. 2. For transmission of solids, thin plates or powders pressed into pellets with diluents can be used. For liquids, a sandwich of liquid between plates or a liquid cell can be employed. 3. For ATR, solids can be placed directly on flat or trough crystals while liquids are placed in a trough. Minimum sample preparation is needed for ATR.

Uploaded by

Huy Pham
Copyright
© © All Rights Reserved
Available Formats
Download as PDF, TXT or read online on Scribd
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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.

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