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氧化镧标准样品的研制

Development of lanthanum oxide certified reference materials

  • 摘要: 为研制氧化镧标准样品,补充和完善稀土类标准样品体系,以氧化镧原料为基体,采用溶液掺杂法制备标准样品。将氧化镧原料分散于有机溶剂中,按成分设计要求加入标准溶液,经恒温水浴搅拌挥发、电热板近干蒸发、850 ℃马弗炉灼烧2 h、球磨、混料、均匀性初检、包装、稳定性检验、均匀性检验、数理统计及定值等工序,完成标准样品的研制。所研制的氧化镧标准样品设计定值指标共38项,包括14个稀土元素氧化物及ThO2、Sc2O3、TiO2、V2O5、Co2O3、NiO、CuO、Rb2O、SrO、CdO、PbO、As、BaO、ZnO、P2O5、SiO2、Al2O3、Cr2O3、MnO2、MgO、Fe2O3、CaO、SO42-、Cl-等非稀土杂质。邀请8家稀土检测领域具有较强技术能力的实验室,采用可靠分析方法确定了标准样品的标准值与不确定度。结果表明,该标准样品可有效完善和丰富国内外有色金属领域稀土类标准样品系列,已报请国家质量监督检验检疫总局和国家标准化管理委员会批准为国家级标准样品。

     

    Abstract: To develop lanthanum oxide certified reference materials and supplement and improve the system of rare earth reference materials.The samples are prepared by the solution doping method using lanthanum oxide as the raw material.Disperse lanthanum oxide raw materials in an organic solvent and add standard solutions in accordance with the composition design requirements.The development of the reference material was completed through a series of processes, including stirring volatilization in a constant-temperature water bath, evaporation, calcination at 850 ℃ for 2 hours, ball milling, mixing, preliminary homogeneity inspection, packaging, stability testing, homogeneity verification, mathematical statistics and value assignment.The standard value of certified reference materials is 38 elements,including 14 kinds of rare earth oxide,ThO2,Sc2O3,TiO2,V2O5,Co2O3,NiO,CuO,Rb2O,SrO,CdO,PbO,As,BaO,ZnO,P2O5,SiO2,Al2O3,Cr2O3,MnO2,MgO,Fe2O3,CaO,SO42-,Cl-.Eight laboratories with rich experience and strong technical ability in the field of rare earth detection were invited to use reliable analytical methods to determine the certified values and expanded uncertainties of lanthanum oxide certified reference materials.The certified reference materials has further improved and enriched the rare earth standard sample series in the field of nonferrous metals at home and abroad, and has been submitted to the State Administration for Market Regulation, National Standardization Administration for approval as a national standard sample.

     

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