本文選題：電感耦合等離子體質(zhì)譜(ICP-MS) + 高純硒��； 參考：《質(zhì)譜學報》2017年03期

【摘要】：建立了硒酸化分離-電感耦合等離子體質(zhì)譜(ICP-MS)測定高純硒中Al、Fe、Sn、Te、Sb、Ti、Ga、Pb、Ge等9種痕量雜質(zhì)元素的方法。利用基體硒酸化生成硒酸具有低沸點的特性分離基體,有效克服了基體對待測元素的干擾和對儀器進樣系統(tǒng)的污染。還研究了酸的加入量對分離效果的影響;測定不同基體~(74)Se和~(76)Se殘留下~(74)Ge(豐度R=36.28%)和~(76)Ge(豐度R=7.61%)的值;將該方法與揮發(fā)二氧化硒分離基體法、陽離子交換分離富集法進行對照,比較了方法的有效性。結(jié)果表明,在硫酸高溫冒煙下,酸的加入量為4mL時,可以實現(xiàn)基體99.99%分離;基體對~(74)Ge和~(76)Ge的干擾可以完全消除。揮發(fā)二氧化硒分離基體法及陽離子交換分離富集法的對照實驗表明,在選定的實驗條件下,方法檢出限(3σ)介于0.01~0.02μg/g,相對標準偏差(RSD)為2.5%~5.3%,加標回收率為90%~110%。此方法快速、簡便、準確可靠,能夠滿足純度為5N(99.999%)的高純硒中9種雜質(zhì)元素的測定。
[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.
【作者單位】： 西北有色金屬研究院;西安交通大學金屬強度國家重點實驗室;
【基金】：國家自然科學基金項目(50603020,50773062) 陜西省自然科學基金項目(2013K09-27) 中央高�；究蒲谢痦椖�(XJJ2014124,XJJ2013130)資助
【分類號】：O657.63;TN304.13

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