电感耦合等离子体质谱法测定锰铁中痕量铅锡锑

建立了电感耦合等离子体质谱法（ICP-MS）同时测定锰铁中痕量铅、锡和锑的分析方法。采用HCl、HNO₃、HF和HClO₄溶解样品, 过氧化氢还原氧化锰, 内标法和基体匹配来校正基体效应, 通过优化质谱仪测量参数, 选择²⁰⁸Pb、¹¹⁸Sn和¹²¹Sb作为待测元素同位素, 测定了锰铁中铅、锡、锑含量。研究结果表明：铅、锡、锑校准曲线的线性相关系数在0.999以上, 检出限(质量分数)分别为0.0005%、0.00008%、0.00011%, 样品测定结果与ICP-AES法相符, 相对标准偏差（n=10）分别为3.5%(铅)、7.2%(锡)、5.9%(锑)。该方法分析周期短, 精密度和准确度能满足测量要求。

Determination of trace lead,tin and antimony in ferromanganese by inductively coupled plasma mass spectrometry

A method for simultaneous determination of trace lead, tin and antimony by inductively coupled plasma mass spectrometry(ICP-MS) was established. By using HCl, HNO₃, HF and HClO₄ for dissolving sample, hydrogen peroxide to reduce manganese oxide, internal standard method and matrix matching to correct the matrix effect and by optimizing the measurement parameters of mass spectrometer and selecting ²⁰⁸Pb, ¹¹⁸Sn and ¹²¹Sb as isotopes, The content of lead, tin and antimony was determined. The result indicated that the linear correlation coefficients of calibration curves all were more than 0.999 and the detection limit (mass fraction) for lead, tin and antimony was 0.000 5%, 0.000 08% and 0.000 11%, respectively. The determination results were consistent with that of ICP-AES. The RSDs were 3.5% (lead), 7.2% (tin) and 5.9% (antimony). The method could meet the requirement in precision and accuracy, and possessed of short cycle.