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使用流动注射结合固相预富集和碰撞/反应池-四极杆电感耦合等离子体质谱检测法测定海水中溶解态钴、铁、铅和钒时的不确定度贡献。

Uncertainty contributions to the measurement of dissolved Co, Fe, Pb and V in seawater using flow injection with solid phase preconcentration and detection by collision/reaction cell-quadrupole ICP-MS.

作者信息

Clough Robert, Sela Hagit, Milne Angela, Lohan Maeve C, Tokalioglu Serife, Worsfold Paul J

机构信息

Biogeochemistry Research Centre, School of Geography, Earth and Environmental Sciences, Plymouth University, Plymouth PL4 8AA, United Kingdom.

Biogeochemistry Research Centre, School of Geography, Earth and Environmental Sciences, Plymouth University, Plymouth PL4 8AA, United Kingdom; Nuclear Research Centre, Negev, PO Box 9001, Beer-Sheva, Israel.

出版信息

Talanta. 2015 Feb;133:162-9. doi: 10.1016/j.talanta.2014.08.045. Epub 2014 Aug 23.

Abstract

A flow injection manifold incorporating a solid phase chelating resin (Toyopearl AF-Chelate-650) is reported for the preconcentration of dissolved metals from seawater, with a focus on investigating the effect of the loading pH, wash solution composition and wash time. Cobalt, iron, lead and vanadium have been used as target analytes with contrasting oceanographic behaviour. Quadrupole ICP-MS has been used for detection to make the approach accessible to most laboratories and a collision/reaction cell has been incorporated to minimise polyatomic interferences. Results for the seawater CRM NASS-6 and two GEOTRACES reference materials were in good agreement with the certified/consensus values, demonstrating the suitability of the approach for the determination of trace metals in seawater. The experimental design used allowed a thorough investigation of the uncertainty contribution from each method parameter to the overall expanded uncertainty of the measurement. The results showed that the parameters making the largest contributions were the precision of the peak area measurement and the uncertainty associated with the slope of the calibration curve. Therefore, these are the critical parameters that should be targeted in order to reduce the overall measurement uncertainty. For iron, the wash blank also gave a measureable contribution.

摘要

本文报道了一种流动注射系统,该系统包含固相螯合树脂(Toyopearl AF-Chelate-650),用于对海水中溶解的金属进行预富集,重点研究了负载pH值、洗涤溶液组成和洗涤时间的影响。钴、铁、铅和钒被用作目标分析物,它们在海洋学行为上具有差异。采用四极杆电感耦合等离子体质谱进行检测,以使大多数实验室都能采用该方法,并引入了碰撞/反应池以尽量减少多原子干扰。海水标准物质NASS-6和两种全球变化痕量元素研究(GEOTRACES)参考物质的检测结果与认定值/共识值高度一致,证明了该方法适用于海水中痕量金属的测定。所采用的实验设计能够全面研究每个方法参数对测量总扩展不确定度的不确定度贡献。结果表明,贡献最大的参数是峰面积测量的精密度和与校准曲线斜率相关的不确定度。因此,为了降低总体测量不确定度,这些是应关注的关键参数。对于铁而言,洗涤空白也有可测量的贡献。

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