电感耦合等离子体质谱法测定有机相中镎

Determination of Neptunium in Organic Phase by ICP-MS

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238 U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(3 s,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。

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(3 s,n=10)of the method is no greater than 1×10^-8 g/L,the relative standard derivations(s r)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.