基体酸化分离-电感耦合等离子体质谱法测定高纯硒中Al、Fe、Sn、Te、Sb、Ti、Ga、Pb、Ge

发布时间：2018-04-14 11:35

本文选题：电感耦合等离子体质谱(ICP-MS) + 高纯硒　；参考：《质谱学报》2017年03期

【摘要】：建立了硒酸化分离-电感耦合等离子体质谱(ICP-MS)测定高纯硒中Al、Fe、Sn、Te、Sb、Ti、Ga、Pb、Ge等9种痕量杂质元素的方法。利用基体硒酸化生成硒酸具有低沸点的特性分离基体,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。还研究了酸的加入量对分离效果的影响;测定不同基体~(74)Se和~(76)Se残留下~(74)Ge(丰度R=36.28%)和~(76)Ge(丰度R=7.61%)的值;将该方法与挥发二氧化硒分离基体法、阳离子交换分离富集法进行对照,比较了方法的有效性。结果表明,在硫酸高温冒烟下,酸的加入量为4mL时,可以实现基体99.99%分离;基体对~(74)Ge和~(76)Ge的干扰可以完全消除。挥发二氧化硒分离基体法及阳离子交换分离富集法的对照实验表明,在选定的实验条件下,方法检出限(3σ)介于0.01~0.02μg/g,相对标准偏差(RSD)为2.5%~5.3%,加标回收率为90%~110%。此方法快速、简便、准确可靠,能够满足纯度为5N(99.999%)的高纯硒中9种杂质元素的测定。
[Abstract]:A method was developed for the determination of nine trace impurity elements such as Al _ (Fe _ (()) Fe _ (())) _ (T _ (2)) _ (()) _ (SB) ~ ((2)) ~ ((2)) ~ ((1)) in high purity selenium by inductively coupled plasma mass spectrometry (ICP-MS).The low boiling point of selenic acid can be used to separate the matrix, which can effectively overcome the interference of the matrix to the measuring elements and the contamination of the instrument sample system.The effect of acid addition on the separation effect was also studied, and the values of 74 GE (abundance rn 36.28) and 76G (abundance RX 7.61g) were determined under the residues of different matrices, and the results were compared with the separation and enrichment method of volatile selenium dioxide and cation exchange.The effectiveness of the method is compared.The results show that the matrix can be separated 99.99% when the acid content is 4mL at high temperature and the interference of the matrix can be completely eliminated.The relative standard deviation (RSDs) of volatile selenium dioxide separation matrix method and cation exchange separation and enrichment method was 2.5 ~ 5.3and the recovery rate was 90 ~ 110g / g under selected experimental conditions, the detection limit of the method was between 0.01g / g and 0.02 渭 g / g, and the relative standard deviation (RSDs) was 2.5 渭 g / g, respectively.The method is rapid, simple, accurate and reliable, and can be used for the determination of 9 impurity elements in high purity selenium.
【作者单位】：西北有色金属研究院;西安交通大学金属强度国家重点实验室;
【基金】：国家自然科学基金项目(50603020,50773062) 陕西省自然科学基金项目(2013K09-27) 中央高校基本科研基金项目(XJJ2014124,XJJ2013130)资助
【分类号】：O657.63;TN304.13

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