XRF表征课C.pptVIP

S. Zhuo SICCAS XRF 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 Sample Forms Bulk Solids : alloys, glasses, plastics, ceramics Pressed Powder : Particles Size Effect Mineralogical Effect Fused Disk : — heating a mixture of sample flux at high T(℃) — melts, dissolve, agitation — pouring the melt into mould and cooling — add non-wetting agent if necessary (NH4I, NH4Br) Liquid : homogeneous, easy to preparing standards…. Sample Surface R(kcps) = f (1/d2) Non flat samples Concave (Distance, Shadow effect) Convex (Distance, Shadow effect) Surface finish (Shadow effect) Effect of Surface finish Particle size effect Mineralogical/metallurgical effect Inhomogeneity : solving problems The elimination of particle size effect and mineralogical effect Metal Sample Metal Disc : — grinding, turning, polishing Small Metal Pieces or Powders : — Re-melting in HF-furnace — Pressing at 100 tons — Dissolve in acid — Loose pieces in liquid-cup — Pre-oxidation and fusion Powders (non-metallic) Oxide : — minerals, ores, glass, cement, refractories, ceramics, slags, sinters, fly ash Sulphides : — sulfide ores, e.g. PbS, ZnS, CuS, FeS2 Miscellaneous : — plants, coal, airborne dust Grinding and Pressing Type of grinder : e.g. vibration ball mill with grinding set of WC Amount of sample Grinding time Wet/dry grinding Pressure/time Binding agent backing Binding Agent Fusion Type of flux: Li2B4O7, LiBO2….. Sample/flux ratio: 1:3, 1:6, 1:10….. Temperature time: 1000o, 1200o…… Crucible materials: 5%Au-95%Pt Furnace or fusion device: 高频炉，马沸炉，气体 Oxidizing agent: LiNO3, NH4NO3 Heavy absorber: La2O3 ……. Non-wetting agent: NH4I, NH4Br Casting dish : 5%Au-95%Pt Plastics Hot pressing Note: Mind for infinite thickness Loose granulates in liquid cup Plants Dry, (Grinding) and pressing Ash and measurement of residue : Note: Volatile substances will disappear Water (Low concentrations) Pre-concentrati