基体分离-电感耦合等离子体质谱法测定高纯硒中13种杂质元素
Matrix Separation and Determination of 13 Impurity Elements in High Purity Selenium by Inductively Coupled Plasma Mass Spectrometry
投稿时间:2019-03-14  修订日期:2019-04-27
DOI:10.16495/j.1006-3757.2019.02.013
中文关键词:  基体分离  电感耦合等离子体质谱法  高纯硒  杂质元素
英文关键词:matrix separation  inductively coupled plasma mass spectrometry  high purity selenium  impurity element
基金项目:
作者单位
胡芳菲 国标(北京)检验认证有限公司, 北京 100088 
于磊 国标(北京)检验认证有限公司, 北京 100088 
宋永清 国标(北京)检验认证有限公司, 北京 100088 
王长华 国标(北京)检验认证有限公司, 北京 100088 
祝利红 国标(北京)检验认证有限公司, 北京 100088 
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中文摘要:
      采用基体分离-电感耦合等离子体质谱法(ICP-MS)测定高纯硒中13种痕量杂质元素含量,优化了试验条件.利用二氧化硒在真空条件下升华温度低的特点挥发基体硒,选择合适的内标元素,考察基体效应的影响.结果表明,选择Cs作为待测元素的内标更合适.测定硒残留量小于100 μg/mL的样品,不影响各待测元素.方法检出限为0.007~0.033 μg/g,RSD为5.7%~19%,加标回收率在90.2%~115%之间,可以满足高纯硒中痕量杂质元素含量的测定.
英文摘要:
      An inductively coupled plasma mass spectrometric method after matrix separation was developed for the determination of 13 impurity elements in high purity selenium. Selenium was separated under low sublimation temperature and vacuum conditions. An appropriate internal standard element was chosen and the influence of matrix effect was investigated. The results showed that caesium was the appropriate internal standard element for the elements to be measured, with residual selenium under 100 μg/mL, and do without interference for the determination of impurity elements. The limit of determination was 0.007~0.033 μg/g, the relative standard deviation was 5.7%~19% and the spiked recovery was 90%~115%. This method can be used to determine trace elements in high purity selenium of 99.999 9%.
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