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本文采用萃取色层法分离—电感耦合高频等离子体光源光谱法测定UF_6水解液中Zn、Cd、Ru、Sn、Pb、Nb和Bi微量杂质元素。先将UF_?水解液转化成UO_2(NO_3)_2蒸发至将结晶,溶于含有0.06 N HF的5 N HNO_3溶液中,通过以Kel—F粉为支持剂,TBP为萃取剂的萃取色层柱后,以5 NHNO_3溶液淋洗杂质,然后以等离子体光源激发进行光谱测定。取样0.3g时,测定下限:Cd、Ru、Nb、Bi为1ppm,Pb、Sn为2 ppm,Zn为5 ppm。当Cd、Ru、Nb、Bi的含量为1ppm和5 ppm,Pb、Sn为5 ppm,Zn为10 ppm时,方法回收率为87—113%,相对标准偏差≤±14%。
In this paper, trace impurity elements of Zn, Cd, Ru, Sn, Pb, Nb and Bi in UF_6 hydrolyzate were determined by extraction chromatography coupled with inductively coupled plasma-atomic fluorescence spectrometry. First UF_? Hydrolyzed liquid into UO_2 (NO_3) _2 evaporated to be crystallized, dissolved in 5 N HNO_3 solution containing 0.06 N HF, through the Kel-F powder as a support agent, TBP extractant extraction chromatography column After the 5 NHNO_3 solution was rinsed with impurities and then excited with a plasma light source for spectrometry. When 0.3 g was sampled, the lower limit of determination was 1 ppm for Cd, Ru, Nb and Bi, 2 ppm for Pb and Sn, and 5 ppm for Zn. The method recovery was 87-113% with relative standard deviation ≤ ± 14% when the contents of Cd, Ru, Nb and Bi were 1 ppm and 5 ppm, Pb and Sn were 5 ppm, and Zn was 10 ppm.