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〕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
This article describes the CL-TBP extraction chromatography, ICP / MS U3O8 trace elements trace elements Zr, Nb, Ta and Ru. After the U3O8 was dissolved in nitric acid and a little hydrofluoric acid, the mixed solution of nitric acid and oxalic acid was used as the mobile phase with the CL-TBP extraction resin as the stationary phase. The chromatographic separation was carried out to separate the impurity elements from the uranium matrix. Lotions were measured by ICP / MS. When the amount of sample is 0.5g, the lower limit of determination of impurity elements Zr, Nb, Ta and Ru is 1 × 10-8g / g, and the recoveries of the method are between 93% and 112%. The results of eight parallel sampling The relative standard deviation is less than 17%. This method is applied to the determination of Zr, Nb, Ta and Ru in U3O8 standard materials. The measured results agree well with the experimental data