Analytical procedure for environmental and seafood safety monitoring of total mercury content, based on the external calibration methodology and cold vapor generation inductively coupled plasma mass spectrometry determination, was validated according to the requirements of international guidelines and standards. Marine samples with varying levels of mercury: marine biota, marine sediment and costal sea waters were used in this study. A full validation approach in line with the ISO/IEC 17025 and Eurachem guidelines was followed. With this in mind, blanks, selectivity, working range (1.2 ng kg −1 to 240 ng kg −1 ), linearity (0.9991), recovery (97 % to 103 %), repeatability (< 2.5 %), intermediate precision (< 3.5 %), limit of detection (0.72 ng kg −1 ) and limit of quantification (1.10 ng kg −1 ) were systematically assessed. The uncertainty of measurement results was estimated according to the recommendations of the Guide to the expression of Uncertainty in Measurement. The relative expanded uncertainty was in the range between 14.2 % and 15.8 % ( k = 2) for marine biota and sediment samples, respectively, and rise up to 32.8 % ( k = 2) on the total mercury mass fraction in costal seawater at the level of 5 ng kg −1 . The major contribution to the combined uncertainty was found to come from the uncertainty associated with the correction for recovery and procedural blanks. The performance of validated procedure was demonstrated by its application to the low-level Hg content seawater samples, received in the frame of Proficiency Testing Scheme, conducted by the Quality Assurance of Information in Marine Environment Monitoring in Europe. The result for total mercury content in marine sediment IAEA-475 was used as the contribution of the IAEA in the characterization campaign of the IAEA-475 candidate certified reference material. The demonstrated SI traceability of obtained results is a prerequisite for their further comparisons with monitoring data obtained in different place and time.

中文翻译：

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冷蒸汽发生和电感耦合等离子体质谱测定后不同海洋舱室总汞含量的环境监测

基于外部校准方法和冷蒸汽发生电感耦合等离子体质谱法测定的环境和海产品总汞含量安全监测的分析程序，根据国际指南和标准的要求进行了验证。本研究使用了不同汞含量的海洋样品：海洋生物群、海洋沉积物和沿海海水。遵循了符合 ISO/IEC 17025 和 Eurachem 指南的完整验证方法。考虑到这一点，空白、选择性、工作范围（1.2 ng kg -1 至 240 ng kg -1 ）、线性（0.9991）、回收率（97 % 至 103 %）、重复性（< 2.5 %）、中间精度（< 3.5 %)、检测限 (0.72 ng kg -1 ) 和定量限 (1.10 ng kg -1 ) 被系统地评估。测量结果的不确定度是根据《测量不确定度表达指南》的建议估算的。海洋生物群和沉积物样本的相对扩展不确定度分别在 14.2 % 和 15.8 % ( k = 2) 之间，并且在沿海海水中的总汞质量分数上升到 32.8 % ( k = 2) 5 ng kg -1 的水平。发现对组合不确定度的主要贡献来自与回收率和程序空白校正相关的不确定度。验证程序的性能通过其应用于低水平 Hg 含量海水样本来证明，这些样本是在欧洲海洋环境监测信息质量保证组织进行的能力测试计划框架内收到的。IAEA-475 海洋沉积物中总汞含量的结果被用作 IAEA 在 IAEA-475 候选认证参考材料表征活动中的贡献。所获得结果的证明 SI 可追溯性是将其与不同地点和时间获得的监测数据进一步比较的先决条件。