电感耦合等离子体质谱法测定电解金属锰中痕量元素

摘要

电解金属锰样品用HNO3+HC1经微波消解后,直接用电感耦合等离子体质谱法(ICP-MS)同时测定了试液中Na、Mg、Ti、V、Co、Ni、Cu、Zn、As、Mo、Cd、Sb、Pb等13种痕量元素.通过优化仪器工作参数、选择适宜待测元素的同位素以及选用干扰元素校正方程克服了质谱干扰,使用内标元素消除了基体干扰.结果表明,Mg、V、Co、Ni、Cu、Zn、As、Mo、Cd、Sb、Pb等11种痕量元素的检出限在0.001～0.086 μg/L之间,Na和Ti元素的检出限在0.16～0.19μg/L之间.将本方法用于测定电解锰样品,加标回收率在95％～106％之间,相对标准偏差(RSD)小于3.5％.方法与其它分析方法对照,结果一致.%After electrolytic manganese metal sample was digested by HNO3 + HC1 with microwave, thirteen trace elements (Na, Mg, Ti, V, Co, Ni, Cu, Zn, As, Mo, Cd, Sb and Pb) in solution were determined simultaneously by inductively coupled plasma mass spectrometry (ICP-MS). The mass spectral interference was overcome by optimizing the instrumental operation parameters, selecting appropriate isotopes for testing elements and using correction equation of interference elements. The matrix interference was eliminated by using internal standard element. The results showed that the detection limits of eleven trace elements (Mg, V, Co, Ni, Cu, Zn, As, Mo, Cd, Sb and Pb) were 0. 001-0. 086 μg/L, and that of Na and Ti were 0. 16-0. 19 μg/L. The proposed method has been applied to the determination of electrolytic manganese metal sample. The results were consist with those obtained by other analytical methods with recoveries of standard addition of 95%-l06% and relative standard deviation (RSD) less than 3. 5 %.