本文選題：電感耦合等離子體質譜法(ICP-MS) + 納米硅粉　； 參考：《冶金分析》2017年12期

【摘要】：采用HNO_3和HF體系溶解樣品,通過選擇合適的待測同位素和干擾系數校正法克服了質譜干擾,以~(45)Sc為內標測定Li、B、Mg、Al、P、Ca、V、Cr、Mn、Co、Ni、Cu和Zn,以~(103)Rh為內標測定Ga、Cd、Sn、Sb、Ba和Pb,建立了電感耦合等離子體質譜法(ICP-MS)對納米硅粉中20種雜質元素的測定方法。實驗發(fā)現,在溶樣時加入1.0mL 30g/L甘露醇溶液,同時控制蒸發(fā)消解溫度為120℃可有效抑制元素B的揮發(fā)損失,進而提高了測定元素B的準確性;采用加熱蒸發(fā)消解揮Si的方法處理樣品后,待測溶液中Si的質量濃度低于100mg/L,不僅可以消除Si基體對測定的干擾,而且也消除了對元素P測定的干擾;采取增加泵速并使用10%氨水(V/V)和10%HNO_3(V/V)交替沖洗的方式可消除元素B的記憶效應。以各元素的質量濃度為橫坐標,其對應的離子強度為縱坐標繪制校準曲線,各元素校準曲線的相關系數均在0.999 9以上,方法檢出限為0.000 3~0.30μg/g,背景等效濃度為0.001 1~4.9μg/g。采用實驗方法對納米硅粉實際樣品中各元素進行測定,所得結果的相對標準偏差(RSD,n=9)為1.1%~7.6%,加標回收率在90%~108%之間。采用電感耦合等離子體原子發(fā)射光譜法(ICP-AES)進行方法對照試驗,測定B、P、Al、Ca、Mg、Fe的結果與實驗方法基本一致。
[Abstract]:The sample was dissolved in HNO_3 and HF system, and the mass spectrometry interference was overcome by selecting suitable isotope and interference coefficient correction method. A method for the determination of 20 impurity elements in nanocrystalline silicon powder by inductively coupled plasma mass spectrometry (ICP-MS) has been established, in which the content of Cu and Zn is determined by the internal standard of Li Li Bu 45 Sc, and the content of Cu and Zn is determined with the internal standard of Ga-CdSn-Sb-Ba and Pb.The method of inductively coupled plasma-mass spectrometry (ICP-MS) has been established for the determination of 20 kinds of impurity elements in nano-silicon powder. It was found that the evaporation loss of element B could be effectively inhibited by adding 1.0mL 30g/L mannitol solution when the sample was dissolved and the evaporation and digestion temperature was controlled at 120 鈩，

本文編號：1950619