巯基棉分离-电感耦合等离子体质谱法测定铅铋共晶合金中痕量碲  

Determination of trace Te in lead bismuth eutectic by inductively coupled plasma mass spectrometry with thiol cotton fiber separation

作　　者：黄兴德 赵思倩 李勇 吴久伟[1] 葛丁 官国英[1] HUANG Xingde;ZHAO Siqian;LI Yong;WU Jiuwei;GE Ding;GUAN Guoying(Department of Isotope,China Institute of Atomic Energy,Beijing 102413)

机构地区：[1]中国原子能科学研究院同位素研究所,北京102413

出　　处：《分析试验室》2021年第10期1192-1196,共5页Chinese Journal of Analysis Laboratory

基　　金：中核集团集中研发项目(FA18000510)资助。

摘　　要：建立了巯基棉(TCF)分离与电感耦合等离子体质谱ICP-MS结合测定LBE中痕量碲(Te)的分析方法,解决了ICP-MS无法直接测定铅铋共晶合金(LBE)中小于1μg/g痕量Te元素的问题。利用TCF的选择吸附性使溶液中Te与Pb,Bi分离,溶液中Pb,Bi的含量降至0.01 mg/L以下,而Te的损失率小于1%,成功消除了溶液中大量Pb,Bi产生的基体效应。优化了TCF的用量、滤液的流速、洗脱等条件。在优化的分析条件下,信号强度与Te标准工作溶液质量浓度在0.01~100μg/L范围内呈良好的线性关系,线性相关系数R2为0.9999,方法的检出限和定量限为0.04,0.15 ng/g,加标回收率95.5%~106.1%,精密度为1.1%~1.9%。方法可用于LBE样品中痕量Te的分析研究。A method of thiol cotton fiber( TCF) separation combined with inductively coupled plasma mass spectrometry( ICP-MS) was established for determination of trace Te in lead bismuth eutectic( LBE),which solved the problem that the trace element Te( < 1 μg/g) in LBE cannot be directly determined by ICP-MS.Using the selective adsorption characteristics of TCF to separate Te from Pb and Bi in the solution,the content of Pb and Bi was reduced to less than 0. 01 mg/L,while the loss rate of Te was less than 1%,leading to the matrix effect caused by a large amount of Pb and Bi was successfully eliminated. In addition,the amount of TCF,flow rate of filtrate and elution conditions were optimized. Under the optimal conditions,the signal intensity and concentration of Te was in a good linear relationship in the range of 0. 01-100 μg/L,the linear correlation coefficient R2 was 0. 9999,and the detection limit of the method was 0. 04 ng/g,the lower limit of quantification was 0. 15 ng/g,with the spike recoveries of 95. 5%-106. 1%,and RSDs of 1. 1%-1. 9%. The method has been successfully applied to the determination of trace Te in LBE samples.

关 键 词：巯基棉 铅铋共晶合金 电感耦合等离子体质谱(ICP-MS) Te 

分 类 号：O657.63[理学—分析化学]