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

机译:使用直接汞分析仪同时燃烧制剂汞同位素分析及汞汞的检测

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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 2 sigma (0.05-0.12 parts per thousand) is similar to the solution standard RM8610 (2 sigma = 0.09 parts per thousand). 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. (C) 2021 Elsevier B.V. All rights reserved.
机译:汞(Hg)稳定同位素特征被广泛用于了解环境中的汞循环。CV-MC-ICP-MS测定汞同位素比值的样品制备方法因实验室设施和样品类型而异。在这里,我们提出了一种在测定汞同位素组成之前制备固体样品的新方法。我们使用直接汞分析仪(测量总汞)进行样品燃烧、合并和分析。在汞从合并器中热释放和检测后,分析物气体进入由10%HCl/BrCl(5:1,vol/vol)组成的捕集溶液。我们发现,汞空白值小于样品分析期间引入的汞的1%,汞检测不会因修改系统而改变,90%以上的引入汞在捕集溶液中回收。汞同位素结果在统计学上与之前发布的认证标准物质的可接受值不可区分,2西格玛(0.05-0.12份/1000)的不确定度与溶液标准RM8610(2西格玛=0.09份/1000)相似。这种新方法允许在15分钟内制备用于汞同位素分析的固体样品。它的另一个优点是在同时检测和制备过程中尽量减少样品质量的使用。(c)2021爱思唯尔B.V.保留所有权利。

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