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1、XRFXRF中的样品制备卓尚军中国科学院上海硅酸盐研究所无机材料分析测试中心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
