萃取色层分离ICP/MS测定U_3O_8中Zr、Nb、Ta和Ru

Determination of Zr,Nb,Ta and Ru in Uranium Oxide by ICP/MS with Chromatography

  • 摘要: 〕本文叙述了CL-TBP萃取色层分离,ICP/MS测定U3O8 中痕量杂质元素Zr、Nb、Ta 和Ru 的方法。U3O8 经硝酸及少许氢氟酸溶解后,用CL-TBP萃淋树脂作固定相,硝酸与草酸的混合酸作流动相,进行萃取色层分离使被测杂质元素与铀基体分离,杂质元素淋洗液用ICP/MS测定。取样量为0.5g 时,杂质元素Zr、Nb、Ta和Ru 的测定下限为1×10- 8g/g,方法的重加回收率在93% -112% 之间,8 次平行取样测量结果的相对标准偏差小于17% ,本方法应用于U3O8 标准物质中Zr、Nb、Ta和Ru 的测量,测量结果与定值数据吻合较好

     

    Abstract: The method of determination of Zr,Nb,Ta and Ru in uranium oxide by ICP/MS with chromatography has been developed in this work.The uranium oxide sample was dissolved with HNO 3 and a little HF.The matrix uranium was separated by a chromatographic proess when the CL-TBP was used as a fixed phase and the mixture of HNO 3 and oxalic acid as eluent.The Zr,Nb,Ta and Ru were determined by ICP/MS.The detection limits of Zr,Nb,TA and Ru are less than 10 -8 g/g.Recoveries of the method are between 93%-103% and precisions of the method for 8 samplings are less than 17%.The method developed in this work is useful for the quantitative analysis of Zr,Nb,Ta and Ru in the reference substance of U 3O 8,and the results for those elements are in agreement with the certified values.

     

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