Efficient benchtop acid digestion of organic-rich sediments for ICP-MS analyses: testing analytical procedures on NIST 2702 standard reference material

Review of the Bulgarian Geological Society Pub Date : 2023-12-01 DOI:10.52215/rev.bgs.2023.84.3.73

Lora Bidzhova, Emiliya D. Raeva, Gatien L. F. Morin, Svetoslav V. Georgiev

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Abstract

Trace element abundances in organic-rich sediments are widely used in various fields of the geosciences, yet few contributions discuss the effectiveness of low-cost benchtop acid digestion techniques for such samples. Here, we tested three different sample preparation methods (acid digestion in closed and open vessels, and fusion) on twelve powder aliquots of organic-rich sediment, standard reference material NIST 2702. Comparison of newly obtained ICP-MS and LA-ICP-MS results with their respective certificate values, facilitates the assessment of digestion efficiency and the effects of vessel size, acid mixture, and other parameters on the recoveries of 29 trace elements. Our results show that benchtop digestion of organic-rich sediment in closed 7 mL PFA vessels using HF+HNO3+HClO4 mixture is more efficient compared with open vessel digestion treated with the same acid mixture (± HCl), with closed or open vessel digestions without HClO4, and with LA-ICP-MS measurements on fused glass discs.

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用于 ICP-MS 分析的富含有机物沉积物的高效台式酸消化：在 NIST 2702 标准参考材料上测试分析程序

富含有机物的沉积物中的痕量元素丰度被广泛应用于地球科学的各个领域，但很少有人讨论低成本的台式酸消解技术对这类样品的有效性。在此，我们对 12 份富含有机沉积物的粉末等分样品（标准参考材料 NIST 2702）测试了三种不同的样品制备方法（在封闭和开放容器中进行酸消解以及熔融）。将新获得的 ICP-MS 和 LA-ICP-MS 结果与各自的证书值进行比较，有助于评估消化效率以及容器大小、酸混合物和其他参数对 29 种微量元素回收率的影响。我们的结果表明，使用 HF+HNO3+HClO4 混合物在封闭的 7 mL PFA 容器中对富含有机物的沉积物进行台式消解，与使用相同酸混合物（± HCl）处理的开放式容器消解、不使用 HClO4 的封闭式或开放式容器消解以及在熔融玻璃圆盘上进行 LA-ICP-MS 测量相比，效率更高。

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Review of the Bulgarian Geological Society

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