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高分辨等离子体质谱法直接测定高纯镓中的痕量元素
引用本文:谢华林,聂西度,唐有根.高分辨等离子体质谱法直接测定高纯镓中的痕量元素[J].分析化学,2006,34(11):1570-1574.
作者姓名:谢华林  聂西度  唐有根
作者单位:1. 湖南工学院化工系,衡阳,421008
2. 中南大学化学化工学院应化系,长沙,410083
基金项目:湖南省自然科学基金;湖南省教育厅青年基金
摘    要:建立高分辨电感耦合等离子体质谱法(HR-ICP-MS)测定高纯镓样品中Be、Mg、A l、S i、Ti、V、Cr、Mn、Fe、Co、N i、Cu、Zn、Ge、As、Mo、Ag、Cd、In、Sb、Ba、Pb、B i等痕量元素的方法。样品用HNO3 HC l经微波消解后,试液直接进样用HR-ICP-MS法同时测定上述元素,在高分辨质谱测量模式下避免了大量的质谱干扰,详细地研究了HC l和高纯镓所产生的基体效应,以Sc、Rh、Tl作为内标元素校正了基体效应,讨论和确定了实验的最佳测定条件。结果表明,23种痕量元素的检出限在0.001~0.21μg/L之间;回收率在89.8%~111.6%之间,相对标准偏差(RSD)小于3.3%。

关 键 词:高分辨电感耦合等离子体质谱  高纯镓  痕量元素  质谱干扰  基体效应  内标
收稿时间:02 18 2006 12:00AM
修稿时间:2006-02-182006-04-17

Direct Determination of Trace Elements in High Purity Gallium by High Resolution-Inductively Coupled Plasma-Mass Spectrometry
Xie Hualin,Nie Xidu,Tang Yougen.Direct Determination of Trace Elements in High Purity Gallium by High Resolution-Inductively Coupled Plasma-Mass Spectrometry[J].Chinese Journal of Analytical Chemistry,2006,34(11):1570-1574.
Authors:Xie Hualin  Nie Xidu  Tang Yougen
Institution:1,Department of Chemical Engineering , ttunan Institute of Technology, Hengy ang 421008;2,School of Chemistry and Chemical Engineering, Central South University, Changsha 410083
Abstract:An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of Be, Mg, Al, Si, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ge, As, Mo, Ag, Cd, In, Sb, Ba, Pb, and Bi elements in high purity gallium was described. The sample was dissolved in HNO3 and HCl by microwave digestion, then the above 22 elements in the solution were detected directly by HR-ICP-MS. Most of the spectral interferences could be avoided by measuring in the high resolution mode (HRM). The matrix effects because of the presence of excess HCl and Ga were evaluated. Correction for matrix effects was made using Sc, Rh and Tl as internal standards. The conditions of the determination were optimized and discussed. The result showed that the detection limit of the method was in the range of 0.001–0.21 μ g l?1, the relative standard deviation (RSD) was less than 3.3% and the recovery of the samples was in the range of 89.8%–111.6%.
Keywords:High resolution-inductive coupled plasma mass spectrometry  high purity gallium  trace(elements)  spectral interferences  matrix effect  internal standards
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