萃取色层分离ICP／MS测定U3O8中Zr,Nb,Ta和Ru

〕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

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

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.