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采用直接测汞仪进行汞同位素分析和总汞检测的同时燃烧制备。

Simultaneous combustion preparation for mercury isotope analysis and detection of total mercury using a direct mercury analyzer.

机构信息

Harvard John A. Paulson School of Engineering & Applied Sciences, Harvard University, 29 Oxford St, Cambridge, MA, 02138, USA.

Harvard John A. Paulson School of Engineering & Applied Sciences, Harvard University, 29 Oxford St, Cambridge, MA, 02138, USA.

出版信息

Anal Chim Acta. 2021 Apr 15;1154:338327. doi: 10.1016/j.aca.2021.338327. Epub 2021 Feb 17.

DOI:10.1016/j.aca.2021.338327
PMID:33736793
Abstract

Mercury (Hg) stable isotope signatures are widely used to understand Hg cycling in the environment. Sample preparation methods for determining Hg isotope ratios by CV-MC-ICP-MS vary widely among laboratory facilities and sample types. Here, we present a novel and rapid method for preparing solid samples prior to determining Hg isotope composition. We use a direct Hg analyzer (that measures total Hg) for sample combustion, amalgamation and analysis. During the thermal release of Hg from the amalgamator and following detection, the analyte gas enters a trapping solution consisting of 10% HCl/BrCl (5:1, vol/vol). We find Hg blank values are less than 1% of the Hg introduced during sample analysis, Hg detection is not altered by modifying the system, and more than 90% of the introduced Hg is recovered in the trapping solution. Hg isotope results are statistically indistinguishable from accepted values for previously published certified reference materials and uncertainty of 2σ (0.05-0.12‰) is similar to the solution standard RM8610 (2σ = 0.09‰). This new method allows for solid sample preparation for Hg isotope analysis in under 15 min. It has the additional advantage of minimizing use of sample mass during simultaneous detection and preparation.

摘要

汞 (Hg) 稳定同位素特征被广泛用于了解环境中的汞循环。通过 CV-MC-ICP-MS 测定 Hg 同位素比值的样品制备方法在实验室设施和样品类型之间差异很大。在这里,我们提出了一种新颖且快速的方法,用于在确定 Hg 同位素组成之前制备固体样品。我们使用直接 Hg 分析仪(测量总 Hg)进行样品燃烧、汞齐化和分析。在汞齐化器中释放 Hg 并进行检测之后,分析物气体进入由 10% HCl/BrCl(5:1,体积比)组成的捕集溶液。我们发现 Hg 空白值低于样品分析过程中引入的 Hg 的 1%,修改系统不会改变 Hg 的检测,并且超过 90%的引入 Hg 被捕集在捕集溶液中。Hg 同位素结果与先前发表的经过认证的参考物质的公认值在统计学上没有区别,2σ 的不确定度(0.05-0.12‰)与溶液标准 RM8610(2σ=0.09‰)相似。这种新方法允许在不到 15 分钟的时间内完成 Hg 同位素分析的固体样品制备。它还有一个额外的优点,即在同时检测和制备过程中最大限度地减少样品质量的使用。

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