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On the use of certified reference materials for assuring the quality of results for the determination of mercury in environmental samples

机译：关于使用经认证的参考物质确保环境样品中汞含量测定结果的质量

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This work focused on the development and validation of methodologies for the accurate determination of mercury in environmental samples and its further application for the preparation and certification of new reference materials (RMs). Two certified RMs ERM-CC580 (inorganic matrix) and ERM-CE464 (organic matrix) were used for the evaluation of digestion conditions assuring the quantitative recovery of mercury. These conditions were then used for the digestion of new candidates for the environmental RMs: bottom sediment (M_2 BotSed), herring tissue (M_3 HerTis), cormorant tissue (M_4 CormTis), and codfish muscle (M_5 CodTis). Cold vapor atomic absorption spectrometry (CV AAS) and inductively coupled plasma mass spectrometry (ICP MS) were used for the measurement of mercury concentration in all RMs. In order to validate and assure the accuracy of results, isotope dilution mass spectrometry (IDMS) was applied as a primary method of measurement, assuring the traceability of obtained values to the SI units: the mole, the kilogram, and the second. Results obtained by IDMS using n(200Hg)(202Hg) ratio, with estimated combined uncertainty, were as follows: (916 ± 41)/[4.5 %] ng g−1 (M_2 BotSed), (236 ± 14)/[5.9 %] ng g−1 (M_3 HerTis), (2252 ± 54)/[2.4 %] ng g−1 (M_4 CormTis), and (303 ± 15)/[4.9 %] ng g−1 (M_CodTis), respectively. Different types of detection techniques and quantification (external calibration, standard addition, isotope dilution) were applied in order to improve the quality of the analytical results. The good agreement (within less than 2.5 %) between obtained results and those derived from the Inter-laboratory Comparison, executed by the Institute of Nuclear Chemistry and Technology (Warsaw, Poland) on the same sample matrices, further validated the analytical procedures developed in this study, as well as the concentration of mercury in all four new RMs. Although the developed protocol enabling the metrological certification of the reference value was exemplified by the determination of mercury in environmental samples, it could be considered as valid for any certification procedure required whenever new certified RMs are introduced.
机译：这项工作的重点是准确测定环境样品中汞的方法的开发和验证，以及其在新参考材料（RM）的制备和认证中的进一步应用。两种认证的RMs ERM-CC580（无机基质）和ERM-CE464（有机基质）用于评估消解条件，以确保汞的定量回收。然后将这些条件用于消化环境RM的新候选物：底部沉积物（M_2 BotSed），鲱鱼组织（M_3 HerTis），cor组织（M_4 CormTis）和鳕鱼肌肉（M_5 CodTis）。冷蒸气原子吸收光谱法（CV AAS）和电感耦合等离子体质谱法（ICP MS）用于测量所有RM中的汞浓度。为了验证和确保结果的准确性，同位素稀释质谱法（IDMS）被用作主要的测量方法，以确保获得的值可溯源至SI单位：摩尔，千克和秒。通过IDMS使用n（ 200 Hg）/ n（ 202 Hg）比率获得的结果，估计的组合不确定度如下：（916±41）/ [4.5％ ] ng -1 （M_2 BotSed），（236±14）/ [5.9％] ng -1 （M_3 HerTis），（2252±54）/ [ （M_4 CormTis）为（2.4％）ng -1 和（M_CodTis）为（303±15）/ [4.9％] ng g -1 （M_CodTis）。为了提高分析结果的质量，应用了不同类型的检测技术和定量方法（外部校准，标准添加，同位素稀释）。所获得的结果与由核化学与技术研究所（波兰华沙）对相同样品基质执行的实验室间比较得出的结果之间的良好一致性（不到2.5％），进一步验证了在这项研究以及所有四个新RM中的汞浓度。尽管通过对环境样品中的汞进行测定可以举例说明可以对参考值进行计量认证的已开发协议，但只要引入新的认证RM，它就可以视为对所需的任何认证程序均有效。

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