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Abstract <p>A procedure is developed for acid digestion of black shale samples weighing up to 1000 mg in an open system. The procedure involves the destruction of the mineral matrix with a fivefold excess of ammonium bifluoride at 230°C for 6 h, followed by the reagent removal through distillation and the subsequent treatment of the residue with a mixture of perchloric and nitric acids to achieve the complete dissolution. The resulting solution remains stable over time and serves as the basis for the direct determination of more than 60 elements using a combination of ICP–MS and ICP–AES techniques. The method enables the quantification of gold, silver, and rhodium directly in the post-decomposition solution with the computational correction of spectral interferences. The method was tested on certified reference black shale materials from the Baikal–Vitim province SLg-1 and SChS-1 (Sukhoi Log deposit, Irkutsk district, Russia). The study also presents analytical results for their updated counterparts, SLg-1A and SChS-1A.</p>

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Sample Preparation of Large Mass Black Shale Samples Using Ammonium Bifluoride for ICP–MS/AES Instrumental Analysis

  • 期刊论文

  • 出版模式：

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  • 发表日期：

    2025年7月25日

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  • V. P. Kolotov,
  • V. I. Kazin,
  • E. A. Zakharchenko,
  • I. N. Gromyak

摘要

Abstract

A procedure is developed for acid digestion of black shale samples weighing up to 1000 mg in an open system. The procedure involves the destruction of the mineral matrix with a fivefold excess of ammonium bifluoride at 230°C for 6 h, followed by the reagent removal through distillation and the subsequent treatment of the residue with a mixture of perchloric and nitric acids to achieve the complete dissolution. The resulting solution remains stable over time and serves as the basis for the direct determination of more than 60 elements using a combination of ICP–MS and ICP–AES techniques. The method enables the quantification of gold, silver, and rhodium directly in the post-decomposition solution with the computational correction of spectral interferences. The method was tested on certified reference black shale materials from the Baikal–Vitim province SLg-1 and SChS-1 (Sukhoi Log deposit, Irkutsk district, Russia). The study also presents analytical results for their updated counterparts, SLg-1A and SChS-1A.