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1、XRFXRF中的樣品制備卓尚軍中國科學院上海硅酸鹽研究所無機材料分析測試中心2012-12-26S.ZhuoSICCASSampleFormsSampleForms?BulkSolids:alloys,glasses,plastics,ceramics?PressedPowder:ParticlesSizeEffectMineralogicalEffect?FusedDisk:—heatingamixtureofsample&fluxathighT(℃)—melts,dissolve,agitation—pouringthemeltintomouldandcooling—addnon
2、-wettingagentifnecessary(NHI,NHBr)44?Liquid:homogeneous,easytopreparingstandards….2012-12-26S.ZhuoSICCASSampleSurfaceSampleSurfaceR(R(kcpskcps)=f(1/d)=f(1/d2))?Nonflatsamples–Concave(Distance,Shadoweffect)–Convex(Distance,Shadoweffect)?Surfacefinish(Shadoweffect)2012-12-26S.ZhuoSICCASEffectofSu
3、rfacefinishEffectofSurfacefinish?Thelongerthewavelengthoftheanalyteline,thefinerthesurfacefinishmustbe?30-50μmfinishisadequatefortheKlinesdowntoatomicnumber13(Al)2012-12-26S.ZhuoSICCASParticlesizeeffectParticlesizeeffect(SiO2)(Al2O3)RSiO2=f(NpSiO2)VolumeRAl2O3=f(NpAl2O3)Volume2012-12-26S.ZhuoSI
4、CCASMineralogical/metallurgicaleffectMineralogical/metallurgicaleffect(SiO2)(SixAlyOz)ISiO2=f((NpSiO2)+(NpSixAlyOz))VolumeSSiO2(kcps/%)<>SSixAlyOzIAl2O3=f(NpSixAlyOz)Volume2012-12-26S.ZhuoSICCASInhomogeneityInhomogeneity:solvingproblems:solvingproblems?Theeliminationofparticlesizeeffectandminer
5、alogicaleffectGrainsizeeffectMineralogicalsolvedeffectsolvedGrainsizereductionYesNoFusionYesYes(solidsolution)2012-12-26S.ZhuoSICCASMetalSampleMetalSample?MetalDisc:—grinding,turning,polishing?SmallMetalPiecesorPowders:—Re-meltinginHF-furnace—Pressingat100tons—Dissolveinacid—Loosepiecesinliquid
6、-cup—Pre-oxidationandfusion2012-12-26S.ZhuoSICCASPowders(non-metallic)Powders(non-metallic)?Oxide:—minerals,ores,glass,cement,refractories,ceramics,slags,sinters,flyash?Sulphides:—sulfideores,e.g.PbS,ZnS,CuS,FeS2?Miscellaneous:—plants,coal,airbornedust2012-12-26S.ZhuoSICCASGrindingandPressingGr
7、indingandPressing?Typeofgrinder:e.g.vibrationballmillwithgrindingsetofWC?Amountofsample?Grindingtime?Wet/drygrinding?Pressure/time?Bindingagent?backing2012-12-26S.ZhuoSICCASBindingAgentBindingAgentBinderBinder/sampleCellulose1+5Te