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本文采用火花源质谱同时分析UF_6中Ta、Nb、Sb、W、Mo、V、Sr、Pb、Bi、Zn、Th十一个微量元素。UF_6样品水解后,加入内标Y、Lu,同位素稀释剂和浓硫酸。溶液蒸乾后,残渣在马弗炉中850℃下灼烧20 min,使转化成U_3O_8。用高纯银粉与U_3O_8混合(重量比为1:1)。压成电极后,用火花源双聚焦质谱仪进行分析。采用内标法和同位素稀释法达到了定量分析目的。内标法的相对标准偏差为±13—40%。同位素稀释法的相对标准偏差为≤±13%。分析结果与其它分析方法测定值相符。测定灵敏度除Th(5ppm)外均达1ppm以下。
In this paper, eleven trace elements Ta, Nb, Sb, W, Mo, V, Sr, Pb, Bi, Zn and Th in UF_6 were simultaneously analyzed by spark source mass spectrometry. After hydrolysis of UF_6 sample, internal standard Y, Lu, isotope diluent and concentrated sulfuric acid were added. After the solution was evaporated to dryness, the residue was burned in a muffle furnace at 850 ° C for 20 min to convert to U_3O_8. Mixed with high-purity silver powder U_3O_8 (weight ratio of 1: 1). After being pressed into electrodes, the spark source dual-focusing mass spectrometer was used for analysis. The internal standard method and isotope dilution method were used to achieve the purpose of quantitative analysis. The relative standard deviation of the internal standard method is ± 13-40%. The relative standard deviation of isotope dilution is ≤ ± 13%. The results of the analysis are consistent with those of other analytical methods. Measurement sensitivity except for Th (5ppm) up to 1ppm or less.