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首页> 外文期刊>Analytica chimica acta >Determination of the total and extractable mass fractions of cadmium and lead in mineral feed by using isotope dilution inductively coupled plasma mass spectrometry
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Determination of the total and extractable mass fractions of cadmium and lead in mineral feed by using isotope dilution inductively coupled plasma mass spectrometry

机译：同位素稀释电感耦合等离子体质谱法测定矿物质饲料中镉和铅的总质量分数和可萃取质量分数

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This paper describes the determination of the total and extractable mass fractions of Cd and Pb in mineral feed test sample distributed by the Community Reference Laboratory for Heavy Metals in Feed and Food (CRL-HM), in the frame of the fifth interlaboratory comparison for the European Union National Reference Laboratories (NRL). The developed in this study protocol for the total and extractable mass fractions of Pb and Cd in mineral feed sample is based on isotope dilution inductively coupled plasma mass spectrometry (ID ICP-MS). The applied dual spiking approach reduced by 50% the number of analytical steps. The addition of hydrofluoric acid in the digestion step was found necessary to ensure a full decomposition and complete isotope equilibration. Quadrupole inductively coupled plasma mass spectrometer equipped with collision reaction interface (CRI) was employed for the measurements of Cd and Pb. Two methods for the determination of Cd were applied and compared. In the first one the high molybdenum content was reduced by introduction of matrix separation step followed by standard ICP-MS mode measurement, whereas in the second one CRI mode was used for the determination of Cd without preliminary matrix separation. The estimation of the combined uncertainty was performed according to the ISO guidelines. Uncertainty propagation was used as a tool for validation of proposed analytical procedure. Contributions from the correction for moisture content, sample homogeneity, procedural blank, instrumental background and dead time effects were evaluated in both cases. The largest uncertainty contributors for Cd and Pb is due to the within bottle homogeneity of the mineral feed sample - 50.3% and 90% respectively. The IUPAC data for isotope composition are the second major contributor to the combined uncertainty of the result for the total mass fraction of Cd in mineral feed - 43.3%. However, the ID ICP-MS results achieved from the two series of samples (partial and total extraction) were in excellent agreement within uncertainty, irrespective of the method used for extraction. The ID ICP-MS results for the total and extractable mass fractions of Cd and Pb in feed sample were compared with the results obtained with external calibration approach and routinely applied in the daily analytical practice of the Belgium National Reference Laboratory for trace elements in food and feed.
机译：本文在第五次实验室间比较的框架内，描述了由饲料和食品中的重金属共同参考实验室（CRL-HM）分发的矿物饲料测试样品中Cd和Pb的总质量分数和可萃取质量分数的测定。欧盟国家参考实验室（NRL）。本研究方案中开发的用于矿物饲料样品中Pb和Cd的总和可萃取质量分数的方法是基于同位素稀释电感耦合等离子体质谱（ID ICP-MS）。所应用的双重加标方法减少了50％的分析步骤。发现在消化步骤中添加氢氟酸对于确保完全分解和同位素完全平衡是必要的。配备了碰撞反应接口（CRI）的四极电感耦合等离子体质谱仪用于Cd和Pb的测量。应用和比较了两种测定Cd的方法。在第一种方法中，通过引入基质分离步骤，然后进行标准ICP-MS模式测量，降低了高钼含量，而在第二种方法中，使用CRI模式无需预先进行基质分离即可测定Cd。组合不确定度的估计是根据ISO准则进行的。不确定性传播被用作验证拟议分析程序的工具。在这两种情况下，均评估了水分含量校正，样品均一性，程序空白，仪器背景和死区时间影响的贡献。 Cd和Pb的最大不确定因素是矿物饲料样品的瓶内均匀性-分别为50.3％和90％。同位素组成的IUPAC数据是造成矿物饲料中Cd总质量分数-43.3％的结果综合不确定性的第二大因素。但是，无论采用哪种提取方法，从两个系列的样品（部分提取和全部提取）获得的ID ICP-MS结果在不确定性内都具有极好的一致性。将饲料样品中Cd和Pb的总质量分数和可萃取质量分数的ID ICP-MS结果与通过外部校准方法获得的结果进行比较，并将其常规应用于比利时国家参考实验室的日常分析中，以分析食品和饲料中的痕量元素。饲料。

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