摘要
采用TBP萃淋树脂萃取色层分离,ICP–MS法测定U_3O_8中痕量杂质元素Th和Zr。U_3O_8样品先经硝酸溶解,再用盐酸转化成氯化铀酰,以TBP萃淋树脂作为固定相,6 mol/L盐酸作为流动相,使铀与待测杂质元素Th和Zr进行分离,用ICP–MS测定淋洗液中杂质元素Th和Zr的含量。Th和Zr的检出限分别为0.008 5μg/L和0.068μg/L,线性方程分别为y=55.789x–0.001 2和y=23.889x–0.001 7,线性相关系数r2=1。测定结果的相对标准偏差均小于5%(n=5),加标回收率在96%~103%之间。用该法测定U_3O_8标准物质,测定结果与标准值一致。该法操作简便,分离快速,测定结果准确、可靠。
A method for the determination of Th and Zr in triurannium octoxide(U_3O_8) by ICP–MS with TBP chromatography was established. The sample was dissolved in the solution of HNO_3 and than converted to uranyl-chloride with HCl. The uranium was separated by using TBP levextrel resin chromatography as fixed phase and 6 mol/L HCl as mobile phase. The trace elements of Th and Zr retained in aqueous phase were detected by ICP–MS. The detection limits of Th and Zr were 0.008 5 μg/L and 0.068 μg/L, respectively. The work curve linear equation of Th and Zr were y=55.789x–0.001 2 and y=23.889x–0.001 7, respectively, the correlative coefficient r^2=1. The relative standard deviation were less than 5%(n=5). The recovery rate was 96%–103%. The determination value of standard reference material by this method was consistent with the standard values. This method is simple and fast in separation, it is accurate and reliable.
出处
《化学分析计量》
CAS
2016年第3期16-19,共4页
Chemical Analysis And Meterage
基金
国家重大仪器设备开发专项(2011YQ14015008)
长江学者和创新团队发展计划项目(IRT13054)
