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<p>The use of reference materials is the most accessible tool for ensuring metrological traceability of the measurement results in various industries, while the main criterion for selecting a&#xa0;reference material is based on its metrological characteristics, including the uncertainty of the certified value and verified metrological traceability. One of the sources of uncertainty of the certified reference material value is the characterization method selected by its manufacturer. The paper describes a&#xa0;method for characterizing a&#xa0;reference material based on the results of an interlaboratory experiment using algorithms from GOST 8.532-2002 “State system for ensuring the uniformity of measurements (GSI). Certified reference materials of composition of substances and materials. Interlaboratory metrological certification,” ISO 33405:2024 “Reference materials—Approaches for characterization and assessment of homogeneity and stability,” and other documents. The reliability of the estimates of uncertainty of the certified reference material value was analyzed based on the results of an interlaboratory experiment. It is shown that in some cases, the above-mentioned uncertainty of the certified value is significantly lower than the uncertainty of the measurement procedures used during the interlaboratory experiment, and sometimes is lower than the uncertainty of the utilized calibration means, including reference materials. This creates an illusion among the developers and producers of reference materials, leading them to believe that high accuracy of characterization of such reference materials (comparable to that of the methods based on the use of reference standards) can be achieved by conducting an interlaboratory experiment. The paper describes cases of unjustified underestimation of the uncertainty of the certified reference material values due to various reasons, including low-efficiency methods of mathematical treatment of the interlaboratory experimental results. Such low efficiency is associated with an unjustified exclusion of the results obtained in certain laboratories from the estimates of the certified reference material values. The uncertainty of the certified reference material values can also be underestimated when a&#xa0;statistical model that forms the basis for the algorithms for processing the results of the interlaboratory experiment is inconsistent with the actual experimental data. Various algorithms for estimating the certified values and standard uncertainty of characterization of reference materials based on the interlaboratory experimental results were analyzed. It was shown that in order to estimate such uncertainty in terms of high resistance to outliers, it is feasible to use the approach proposed by Maurice Cox. Based on this approach, original algorithms have been developed, which can be used for estimating the commutability of reference materials, as well as for other purposes. To increase confidence in the results of determining the metrological characteristics of reference materials in the Russian Federation, and to ensure harmonization with the international documents, the use the Maurice Cox algorithm was recommended when revising GOST 8.532-2002.</p>

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Reference materials: selection of algorithm for estimating the certified value and its uncertainty based on the results of an interlaboratory experiment

  • 期刊论文

  • 发表日期：

    2025年11月1日

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  • E. P. Sobina,
  • P. M. Aronov,
  • P. V. Migal,
  • V. V. Studenok,
  • S. V. Medvedevskikh

摘要

The use of reference materials is the most accessible tool for ensuring metrological traceability of the measurement results in various industries, while the main criterion for selecting a reference material is based on its metrological characteristics, including the uncertainty of the certified value and verified metrological traceability. One of the sources of uncertainty of the certified reference material value is the characterization method selected by its manufacturer. The paper describes a method for characterizing a reference material based on the results of an interlaboratory experiment using algorithms from GOST 8.532-2002 “State system for ensuring the uniformity of measurements (GSI). Certified reference materials of composition of substances and materials. Interlaboratory metrological certification,” ISO 33405:2024 “Reference materials—Approaches for characterization and assessment of homogeneity and stability,” and other documents. The reliability of the estimates of uncertainty of the certified reference material value was analyzed based on the results of an interlaboratory experiment. It is shown that in some cases, the above-mentioned uncertainty of the certified value is significantly lower than the uncertainty of the measurement procedures used during the interlaboratory experiment, and sometimes is lower than the uncertainty of the utilized calibration means, including reference materials. This creates an illusion among the developers and producers of reference materials, leading them to believe that high accuracy of characterization of such reference materials (comparable to that of the methods based on the use of reference standards) can be achieved by conducting an interlaboratory experiment. The paper describes cases of unjustified underestimation of the uncertainty of the certified reference material values due to various reasons, including low-efficiency methods of mathematical treatment of the interlaboratory experimental results. Such low efficiency is associated with an unjustified exclusion of the results obtained in certain laboratories from the estimates of the certified reference material values. The uncertainty of the certified reference material values can also be underestimated when a statistical model that forms the basis for the algorithms for processing the results of the interlaboratory experiment is inconsistent with the actual experimental data. Various algorithms for estimating the certified values and standard uncertainty of characterization of reference materials based on the interlaboratory experimental results were analyzed. It was shown that in order to estimate such uncertainty in terms of high resistance to outliers, it is feasible to use the approach proposed by Maurice Cox. Based on this approach, original algorithms have been developed, which can be used for estimating the commutability of reference materials, as well as for other purposes. To increase confidence in the results of determining the metrological characteristics of reference materials in the Russian Federation, and to ensure harmonization with the international documents, the use the Maurice Cox algorithm was recommended when revising GOST 8.532-2002.