电感耦合等离子体质谱法测定纳米硅粉中20种杂质元素

发布时间：2018-05-29 10:54

  本文选题：电感耦合等离子体质谱法(ICP-MS) + 纳米硅粉　； 参考：《冶金分析》2017年12期

【摘要】：采用HNO_3和HF体系溶解样品,通过选择合适的待测同位素和干扰系数校正法克服了质谱干扰,以~(45)Sc为内标测定Li、B、Mg、Al、P、Ca、V、Cr、Mn、Co、Ni、Cu和Zn,以~(103)Rh为内标测定Ga、Cd、Sn、Sb、Ba和Pb,建立了电感耦合等离子体质谱法(ICP-MS)对纳米硅粉中20种杂质元素的测定方法。实验发现,在溶样时加入1.0mL 30g/L甘露醇溶液,同时控制蒸发消解温度为120℃可有效抑制元素B的挥发损失,进而提高了测定元素B的准确性;采用加热蒸发消解挥Si的方法处理样品后,待测溶液中Si的质量浓度低于100mg/L,不仅可以消除Si基体对测定的干扰,而且也消除了对元素P测定的干扰;采取增加泵速并使用10%氨水(V/V)和10%HNO_3(V/V)交替冲洗的方式可消除元素B的记忆效应。以各元素的质量浓度为横坐标,其对应的离子强度为纵坐标绘制校准曲线,各元素校准曲线的相关系数均在0.999 9以上,方法检出限为0.000 3~0.30μg/g,背景等效浓度为0.001 1~4.9μg/g。采用实验方法对纳米硅粉实际样品中各元素进行测定,所得结果的相对标准偏差(RSD,n=9)为1.1%~7.6%,加标回收率在90%~108%之间。采用电感耦合等离子体原子发射光谱法(ICP-AES)进行方法对照试验,测定B、P、Al、Ca、Mg、Fe的结果与实验方法基本一致。
[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，

本文编号：1950619