真空蒸馏分离-电感耦合等离子体质谱法测定高纯碲中9种杂质元素

Vacuum Distillation Separation/Enrichment and Determination of Nine Impurities in High Purity Tellurium by ICP-MS

建立了真空蒸馏分离-ICP-MS法测定高纯碲中的9种杂质元素的方法。采用真空蒸馏技术使基体碲与待测元素分离,有效克服了基体对待测元素的干扰和对仪器进样系统的污染。通过优化仪器参数和加入内标,提高了分析准确度。研究了温度和时间对分离效果的影响。当称样量为1.000 g时,最佳分离条件为450℃和3 h。将本方法与ICP-AES-直接溶样法、GD-MS法进行了对照,结果表明,本方法准确可靠。在选定的实验条件下,方法检出限(3σ)为1.4～6.1 ng/g,相对标准偏差为(RSD)为2.8%～7.3%,加标回收率为94.8%～103.0%。本方法简单实用,能够满足大量纯度为5N(99.999%)和6N(99.9999%)的高纯碲中9种杂质元素的测定。

A method was developed for the determination of nine different impurities in high purity tellurium by ICP-MS after vacuum distillation separation.The interferences on analytes and the pollution of sample introduction system were efficiently avoided by separation impurity elements from matrix Te.By optimizing the instrumental parameters and addition of internal standards,the analytical accuracy was further improved.The influences of temperature and time on separation effects have been studied.It showed that the optimal separating temperature and time were 450 ° C and 3 h,respectively,when sample weight was 1.0000 g.The analytical results proved to be accurate and validated by comparison of proposed method with ICP-AES and GD-MS.Under optimized conditions,the detection limits of 1.4-6.1 ng/g and the RSDs of 2.8%-7.3% were obtained,and the recoveries of standard addition were 94.8%-103.0%.The method was suitable for the determination of impurities in high purity tellurium of 99.999% and 99.9999%.