SEPARATIONOFTHESILTANDCLAYFRACTIONSFORX

RAYPOWDERDIFFRACTIONBYCENTRIFUGATION
Centrifugationisanimportantresearchtechniquewithwideapplicationsinthebasicsciences.Examplesof
geologicalusesincludetheseparationofsiltandclayforXraypowderdiffractionanalysesandrecaptureof
theentiresampleaftertreatmentwithacidsoroxidizingagents.Decantationmaynotbeanacceptable
alternativetocentrifugationbecausenormalgravitationalmethodsofparticlesedimentationtakean
inordinateamountoftime,andforparticlesfinerthan0.5micrometersBrownianmotioninterfereswith
settling(Folk,1974).
WehavewrittenaprogrambasedonStoke'sLawthatcalculatescentrifugeruntimesand
speedsforparticlesofvariousdiameteranddensityinmediaofdifferenttemperature,
specificgravity,andviscosity(Poppeandothers,1988).Theprogram,whichwaswritten
inUnisoftCandimplementedonUNIXsystemV,isfast,interactive,allowstheuserto
selectallparticleandmediumrelatedparameters,andisnotspecifictoanyonepieceof
centrifugationequipment.
Theprogrampromptstheuserfortheparticleradiusinmicrometersandtheangular
velocityinrevolutionsperminuteandthenconvertsthesevaluesintotheproperunitsrequiredbythe
formula.Itisimportanttonotethatwhenanalyzingnonsphericalparticlessuchasphyllosilicates,thevalue
fortheradiusdoesnotrepresenttheactualradius,buttheequivalentradiusofasphericalparticleofthesame
materialwhichwouldsettleatthesamerateastheactualparticle.Toobtainthe
correctresults,theusermustexercisecaretoensurethetheothervaluesarein
theproperunitsrequiredbytheprogramandwhendeterminingtheinitial(R1)
andfinal(R2)distancesfromtheaxisofrotation.Becauseofmechanical
differencesinthedesignsofindividualcentrifuges,theusermustmeasure
thesedistancesonthespecificpieceofequipmentbeingused.TheunitsofR1
andR2areunimportantbecausetheycanceloutintheequation.
Programdocumentationcanbeviewedineitheratext,MicrosoftWordorHTMLversion.Programsource
codeandincludeheaderfile,programdocumentation,andahelpfulREADMEfilearestoredinthedirectory
labeledsoftwarelocatedatthetoplevelofthisCDROM.

PROCEDUREFORSEPARATIONOFSILTANDCLAY
BYCENTRIFUGATION
MaterialsRequiredforCentrifugation:
markingpencil
labelingtape
plasticcentrifugetubes(~50ml)with
caps
centrifugetuberack
squeezebottlewithdistilledwater
plasticbeakers
dispersant(sodiumhexametaphosphate)
spatula
ultrasonicprobe
labtissues
thermometer
timer

Ifthesuppliedcentrifugationprogramistobeused,

theoperatorshouldfirstdeterminethenecessary
information(initialandfinaldistancesfromtheaxisof
rotation,andtheaccelerationanddecelerationtimes
ofthecentrifugeforvariousspeeds(rev./min.)and
constructatableofruntimesforcommon
temperatures.

Applylabelingtapetothetopedgeofthecentrifuge
tubeandlabelthetapewiththemarkingpencil.Note:
thebottomedgeofthetapecanactasaguide
facilitatingequalfillingofthetubesthatwillkeepthe
centrifugeinbalance.Applylabelingtapetoand
labeltheplasticbeakers.

Pourenoughsampleintothecentrifugetubestofill
theroundedpartofthebottomofthecentrifuge
tubes.Note:Thepowderfromtherandomlyoriented
aggregatemountscanbeused.

Addasmallamount(about0.25g)ofdispersantto
thecentrifugetubes.Thedispersantwillcoverthetip
ofanarrowspatulaasshown.

Adddistilledwatertothebottomedgeofthelabeling
tape.Placeacaponthecentrifugetubeandshake
thetubetohomogenizethesuspension.

Dispersethesamplefor1520secondswiththe
ultrasonicprobe.Rinsethetipoftheultrasonicprobe
withdistilledwaterandwipeitdrywithlabtissue
betweensonifications.

Checkthewatertemperatureandfindcentrifugation
timesinminutesandsecondsfromtheprepared
table.

TurnonthepowerswitchandpressStop/Open.This
releasesthesafetylatchandallowsthecoverofthe
centrifugetobeopened.Placethetubesinthe
centrifuge.Besurethatthecentrifugeisbalancedby
havingoppositetubesfilledequally2,4,6,or8
tubesmaybeused.Closecover.

Adjustthespeedcontrol,setthemachine'stimerto
hold,adjustthebrake,pressstartonthecentrifuge,
andstartthetimer.Note:thetimersonmost
commercialcentrifugesarenotaccurateenoughto
useforsiltandclayfractionseparations.Whenthe
totalruntimeminusthedecelerationtime(Ttd)has
expiredonthetimer,pressstop.Thespeedshould
readnearzerowhenthecalculatedtotaltimeis
reached.
Removetubesfromthecentrifuge,pryoffcaps,and
pourthesupernatantliquidintotheplasticbeakers.
Becarefulthatthesedimentonthebottomofthe
tubesisnotpouredoff.Ifthesiltandclayfractions
aretobecompletelyseparated,repeatthe
centrifugationprocedureuntilthesupernatantis
reasonablyclear(45times).