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Matrix-assisted photochemical vapor generation for determination of trace bismuth in Fe-Ni based alloy samples by inductively coupled plasma mass spectrometry

机译:基质辅助光化学蒸气,电感耦合等离子体质谱法测定Fe-Ni基合金样品中的痕量铋

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摘要

As the impurities in alloy may affect its mechanical and physical properties, the determination of trace elements is important to ensure the quality of alloy. However, accurate determination of trace impurities in alloy samples is a big challenge due to their complicated matrix and low concentrations. In this work, matrix-assisted photochemical vapor generation (PVG) was developed for the determination of impurity in alloy samples by inductively coupled plasma mass spectrometry (ICPMS). Bismuth was selected as the target element, which is detrimental to the strength of alloy even at very low concentration. The transition ions existed in alloy worked as the "sensitizers" for the efficient PVG of bismuth, and only formic acid and acetic acid were required for the analysis of alloy samples after digestion. This largely reduced the risks of sample contamination and analyte loss in multiple sample pretreatment involved in conventional analytical methods. The PVG efficiency of bismuth was greatly enhanced, making the sensitive and simple determination of trace analytes in alloy samples feasible. The limit of detection (LOD, 3 sigma) for Bi was found to be 0.4 ng L-1 corresponding to 0.54 ng g(-1) for analysis of 0.5 g of alloy sample. A relative standard deviation (RSD) of 1.1% was obtained from seven replicate measurements of 0.5 mu gL(-1) Bi3+ in sample matrix. The proposed method was successfully applied for the determination of Bi in two certified reference materials (Fe-Ni based alloys GBW01621 and GBW01622).
机译:随着合金中的杂质可能影响其机械和物理性质,痕量元素的测定对于确保合金的质量是重要的。然而,由于其复杂的基质和低浓度,准确测定合金样品中的痕量杂质是一个很大的挑战。在这项工作中,通过电感耦合等离子体质谱(ICPMS)来开发用于测定合金样品中的杂质的基质辅助光化学蒸气产生(PVG)。选择铋作为靶元素,即使在非常低的浓度下也是对合金强度有害的。合金中存在的过渡离子作为“敏化剂”为铋的有效PVG,并且仅在消化后分析合金样品所需的甲酸和乙酸。这在很大程度上减少了在常规分析方法中涉及的多种样品预处理中的样品污染和分析物损失的风险。铋的PVG效率大大提高,使得合金样品中可行的痕量分析物的敏感和简单测定。发现Bi的检测极限(LOD,3 sigma)为0.4ng L-1,对应于0.54ng g(-1),用于分析0.5g合金样品。从样品矩阵中的0.5μGL(-1)Bi3 +的七次重复测量中获得1.1%的相对标准偏差(RSD)。所提出的方法成功地应用于两种认证的参考材料(Fe-Ni基合金GBW01621和GBW01622)测定BI的测定。

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