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<p>In this study, an in-house inductively coupled plasma optical emission spectrometry (ICP-OES) method was developed and validated for the determination of major and selected minor/trace elements in calcite mineral matrices. The method is based on a modified acid dissolution procedure adapted from ASTM C1301-22, using hydrochloric acid (HCl), nitric acid (HNO₃), and hydrofluoric acid (HF) microwave digestion without lithium borate fusion. Method validation was performed in accordance with ISO/IEC 17,025 and Eurachem guidance using certified reference material BCS-CRM 513, hereafter referred to as the CRM. Validation parameters included repeatability, intermediate precision, recovery, trueness, selectivity/matrix-effect assessment, robustness, limits of detection (LOD), limits of quantification (LOQ), linearity, and measurement uncertainty. The evaluated oxides (CaO, MgO, SiO₂, Al₂O₃, Fe₂O₃, MnO, K₂O, and SrO) showed satisfactory analytical performance. Relative standard deviation (RSD) values were low under repeatability and intermediate-precision conditions. Recovery values ranged from 99.9% to 101.3%, indicating negligible systematic bias. Measurement uncertainty, estimated using a top-down approach, was dominated mainly by intermediate precision and remained suitable for routine analysis. The validated method is reliable, robust, and fit for purpose for the quantitative analysis of major and minor oxides in calcite matrices.</p>

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Validation of ICP-OES method and estimation of measurement uncertainty for the determination of major and trace elements in calcite minerals

  • 期刊论文

  • 发表日期：

    2026年6月14日

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  • Fatih Turan,
  • Gül Akar Şen,
  • Sezai Şen

摘要

In this study, an in-house inductively coupled plasma optical emission spectrometry (ICP-OES) method was developed and validated for the determination of major and selected minor/trace elements in calcite mineral matrices. The method is based on a modified acid dissolution procedure adapted from ASTM C1301-22, using hydrochloric acid (HCl), nitric acid (HNO₃), and hydrofluoric acid (HF) microwave digestion without lithium borate fusion. Method validation was performed in accordance with ISO/IEC 17,025 and Eurachem guidance using certified reference material BCS-CRM 513, hereafter referred to as the CRM. Validation parameters included repeatability, intermediate precision, recovery, trueness, selectivity/matrix-effect assessment, robustness, limits of detection (LOD), limits of quantification (LOQ), linearity, and measurement uncertainty. The evaluated oxides (CaO, MgO, SiO₂, Al₂O₃, Fe₂O₃, MnO, K₂O, and SrO) showed satisfactory analytical performance. Relative standard deviation (RSD) values were low under repeatability and intermediate-precision conditions. Recovery values ranged from 99.9% to 101.3%, indicating negligible systematic bias. Measurement uncertainty, estimated using a top-down approach, was dominated mainly by intermediate precision and remained suitable for routine analysis. The validated method is reliable, robust, and fit for purpose for the quantitative analysis of major and minor oxides in calcite matrices.