电感耦合等离子体质谱法测定有机相中镎

建立了电感耦合等离子体质谱法(ICP-MS)测定30%(体积分数,下同)磷酸三丁酯(TBP)/煤油和0.5 mol/L 2-噻吩甲酰三氟丙酮(TTA)/二甲苯中镎的分析方法。样品经异丙醇适当稀释或直接进入ICP-MS分析,在有机进样条件下对仪器和操作参数进行优化和选择,研究了有机相和大量²³⁸U在有机基体中引起的基体和质谱干扰,以钍为内标消除基体干扰。研究结果表明:方法的检出限为1×10^-8 g/L(3s,n=10);相对标准偏差(s_r)为0.8%(n=10)(镎质量浓度为2.02μg/L);加标回收率为95.5%～115%。该法适用于动力堆乏燃料后处理流程以及预处理后0.5 mol/L TTA/二甲苯中镎的分析。

Determination of Neptunium in Organic Phase by ICP-MS

A simple, reliable and rapid method was built for determining of neptunium in 30% tributyl phosphate/kerosene and 0.5 mol/L thenoyltrifluoroacetone in xylene by inductively coupled plasma mass spectrometry(ICP-MS) equipped with a sample for organic phase. The instrumental and operating parameters were optimized with the standard solution of organic matrices. The effect of matrix on determination of neptunium was discussed in detail by ICP-MS. The internal standard element of Th was employed to eliminate the signal effect induced by matrix and instrument signal drift. The results suggest that the detection limit(3s, n=10) of the method is no greater than 1×10^-8 g/L, the relative standard derivations(sr) is 0.8%(n=10), and the recoveries vary from 95.5%-115%. This method is applicable for the determination of neptunium in organic phase from the commercial spent fuel reprocessing.