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Measurement Standards. Reference Materials

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Vol 22, No 3 (2026)
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Information. News. Events

Standards

6-19 11
Abstract

 The detection and prevention of metrological failures of standards during operation is one of the most urgent and significant problems. The most common strategy for operating standards is the scheduled strategy (scheduled verification, scheduled repair); therefore, metrological failures are usually detected only during periodic verification or repair.
At the same time, it is possible to obtain continuous or periodic information about non-standardized metrological and technical characteristics of the standard, and such an analysis could help the operating party, by indirect signs, to conclude that the standard is metrologically faulty or that a failure is imminent. However, such information is rarely used at present.
The aim of the work is to analyze the possibility of using monitoring of the technical condition of standards for timely detection and prevention of metrological failures. The obtained data will improve the reliability of measurement results and the transfer of measurement units from these standards, and enable the transition from a scheduled operation strategy to operation based on actual condition.
As a method for analyzing the results of observations of the technical characteristics of a standard, methods of change-point detection theory are proposed. Using the example of monitoring the fall rate of the piston of pressure standards (dead-weight testers), the data were analyzed using parametric and non-parametric change-point detection methods. The results of detecting metrological failure using change-point detection theory methods coincide with the results obtained using more accurate standards and diagnostics.The findings of the study indicate that monitoring the technical condition of standards can, in some cases, prevent metrological failure. Therefore, there is a basis for the operating organization to switch to a strategy of operating standards based on actual condition.
The article may be useful for developers, testers, and specialists involved in the operation of various standards.

20-31 14
Abstract

Regulatory documents on the calculation of verification and calibration intervals for measuring instruments, such as RMG 74–2004 “Methods for determining verification and calibration intervals of measuring instruments”, G24:2007/OIML D10:2007 “Guidelines for the determination of calibration intervals of measuring instruments”, and a number of others, contain descriptions of methods for the initial selection and adjustment of calibration intervals of measuring instruments. Some of these methods are based on statistical approaches.
However, not all methods presented in the regulatory documents are easy to implement, because not all calibrated measuring instruments contain in their initial data the necessary information for calculating the required normalized indicators of metrological reliability (instability) of measuring instruments. The aims of the study: 1) to develop a method for the verification and adjustment of calibration intervals of measuring instruments based on information that is always contained in calibration certificates of measuring instruments; 2) to test the new method on the example of calibration results of an HIOKI 3532-50 impedance measuring instrument.
In this article, a method for calculating the calibration interval is proposed, which is based on the existence of established requirements for the determined metrological characteristics and statistical analysis of normalized deviations of the metrological characteristics of calibrated measuring instruments from their limit values. The method for adjusting the calibration interval implements the idea of managing and adapting the calibration interval depending on the calibration results. This idea is consistent with the principle implemented in the automatic adjustment method, or the «ladder» method, described in G24:2007/OIML D10:2007. In addition, the proposed method is based on the analysis of a set of normalized deviations, which allows it to be classified as a statistical approach.
The proposed method for the verification and adjustment of calibration intervals of measuring instruments assumes the use of previous calibration results of the measuring instrument when available.
This method for the verification and adjustment of calibration intervals of measuring instruments is easy to apply, requiring only the availability of data on previous calibration results of the calibrated measuring instrument (previous calibration certificates), requirements for the normalized metrological characteristic of the measuring instrument, and the calculation of the parameters presented in the article.
The implementation of the method proposed in the article makes it possible to confirm (verify) or justify a change in the existing calibration interval of a measuring instrument based on statistical analysis.

Modern methods of analysis of substances and materials

32-40 8
Abstract

One of the main technical parameters characterizing the optical system of a pyrometer is the sighting parameter. The value of this parameter enables users to assess the applicability of a pyrometer for solving temperature measurement tasks.
The widespread use of non-contact thermometry measuring instruments, namely pyrometers or radiation thermometers, in various fields of science and industry has recently been driven not only by the expansion of the measured temperature range, reduction of measurement error, repeatability of results and development of service capabilities, but also by the diversity of optical systems of measuring instruments. The optical systems of modern pyrometers make it possible to form a measurement area for both micro- objects and objects with significant spatial characteristics.
The sighting parameter is one of the main technical parameters characterizing the optical system of a pyrometer. The value of the sighting parameter allows users to assess the applicability of a pyrometer for solving temperature measurement tasks. However, in practice, the data declared by pyrometer manufacturers in most cases are of an informational nature, which leads to an increase in temperature measurement error.
In accordance with the requirements of the Federal Law of the Russian Federation «On Ensuring the Uniformity of Measurements», the verification of this characteristic is usually carried out during type approval testing of measuring instruments and within the framework of pyrometer verification services in accordance with the provisions of approved verification procedures. A trend has been identified towards the exclusion of the sighting parameter check from newly approved pyrometer calibration procedures
The article analyzes the current practice of confirming the sighting parameter and proposes a method for automating the verification and control of the sighting parameter. It is assumed that the obtained results and implemented technical solutions will allow the installation for determining the sighting parameter to be included in the newly developed reference working standards of temperature.

41-50 10
Abstract

Order of the Federal Agency for Technical Regulation and Metrology (Rosstandart) № 2152 of September 6, 2024 «On approval of the State verification scheme for measuring instruments of torque» regulates the transfer of the unit without using standards borrowed from other verification schemes only in the range up to 20 kN · m. However, the current reference base in the Russian Federation has not yet ensured the reproduction of the unit of torque in the range exceeding 20 kN · m.
There is a clear demand from science and industry to expand the capabilities of ensuring the uniformity of measurements in the field of large values of the unit of torque, which requires the creation of an evidence base for formulating requirements for the design of a reference installation for reproducing the unit of torque in the range of large values.
The aim of the study presented in this article is to justify to the professional community the possibilities of applying a physico-mathematical model of the torque measurement process for formulating technical requirements for the design of a reference installation.
Using computer modelling, an analysis of the influence of the components was carried out, and the limiting values of the uncertainty of their determination ensuring the target accuracy indicators of the reference installation were established. An uncertainty analysis of torque reproduction by the reference installation was performed using a physico-mathematical model of the static torque measurement process.
As a result, the uncertainty components were ranked according to their degree of influence on the measurement result. Components requiring the application of special technical solutions were identified. Technical requirements for the design of the reference installation were determined.
The obtained results can be used in the design of components of the reference installation, namely, for determining the requirements for the manufacture of parts, the selection of materials, and the formulation of the measurement equation of the reference installation.

51-67 11
Abstract

With the advancement of scientific and technological progress in the fields of metrological supervision, chemical and pharmaceutical industries, ensuring continuous metrological control of measuring instruments used in thermal analysis is of particular importance. A key aspect of solving this problem and ensuring traceability of measurement results to the base units of physical quantities is the high accuracy of determining phase transition temperatures, such as melting, crystallization, sublimation, dropping point, softening point, cloud point and other characteristic temperatures of organic compounds.
Within the framework of this study, an aim was set to evaluate the possibility of using organic compounds based on benzophenone, benzoic acid and caffeine as promising candidates for the development of reference materials for phase transition temperature, ensuring traceability to the unit of temperature (°C).
Measurements of phase transition temperatures (melting temperatures) were carried out using differential scanning calorimetry on a STA 449 F5 JUPITER thermal analyzer, which is part of the State Primary Standard of units of mass fraction and mass (molar) concentration of water in solid and liquid substances and materials GET 173. The certified values of the developed reference materials were established in accordance with the requirements of GOST ISO Guide 35-2015 «General and statistical principles for certification». During the work, the uncertainties due to the heterogeneity of the initial materials were quantitatively assessed, and their short-term and long-term stability was investigated.As a result of the development of the reference materials, the ranges of permissible certified values for melting temperature were established: from 47.0 to 50.0 °C –  for benzophenone; from 121.0 to 124.0 °C –  for benzoic acid; from 234.0 to 238.0 °C –  for caffeine.
A comparative analysis of the obtained certified values with reference data given in the International Temperature Scale ITS-90 and NIST reference materials showed a high degree of agreement. The deviations were: for benzophenone –  within ±0.3 °C; for benzoic acid and caffeine –  within ± 0.65 °C. The differences are mainly due to the chemical purity of the substances. Measurement results for benzoic acid with a purity of 99.99 % and above agree within ± 0.01 °C.
The theoretical significance of the work lies in the experimental confirmation of the effectiveness of differential scanning calorimetry for the development of certified reference materials for phase transition temperatures. The result was the development of a set of CRMs (BBK SO UNIIM), registered in the Federal Information Fund for Ensuring the Uniformity of Measurements under the numbers GSO 12725-2024 / GSO  12727-2024.
The practical value of the obtained results lies in expanding the possibilities for calibration and control of thermal analysis measuring instruments, validation of the relevant measurement procedures, as well as ensuring the reliability and accuracy of determination of phase transition temperatures for a wide range of materials, including metals, their salts and oxides, polymers, organic and inorganic compounds.

68-87 11
Abstract

Modern food industry imposes high requirements on product quality and safety, which includes the need for continuous monitoring of harmful impurities and determination of the content of auxiliary substances, among which flavor carriers play an important role: triacetin (E1518), benzyl alcohol (E1519), and propylene glycol (E1520). These substances may be present in food products and beverages, playing an important role in stabilizing taste and odor, or acting as emulsifiers and preservatives. The content of flavor carriers in alcoholic products must comply with the strict requirements of regulatory documents, since some chemical compounds can have a negative impact on consumer health when permissible concentrations are exceeded.
An analysis of the regulatory documentation revealed insufficient development of analytical procedures for the determination of flavor carrier components in alcoholic beverages. The development of a gas chromatographic procedure for the selective quantitative and qualitative determination of volatile organic impurities, including flavor carriers in vodkas and special vodkas, is a timely, important and relevant task, which determined the aim of this study.
The procedure was developed using Agilent 6850, 7820, 7890A gas chromatographs with flame ionization detectors. To confirm identification, chromatography-mass spectrometry was employed using a Maestro 7820 gas chromatograph with a mass-selective detector. Separation of components was performed on a high-polarity HP-FFAP capillary column. ChemStation software A.10.02 and B.04.03 was used for data processing. The objects of the study were model solutions and vodka samples.During the work, the chromatographic behavior of the target analytes was studied, and optimal chromatographic conditions were selected to ensure the best separation of 24 target analytes. Calibration solutions were prepared corresponding to the beginning, middle, and end of the intended measurement range of mass concentrations; metrological characteristics were calculated, and validation studies of the procedure were carried out.
As a result of the research, the «Procedure for the determination of the mass concentration of volatile organic impurities in vodkas» was developed, metrologically certified, and implemented in industry. The conducted studies provide a basis for the development of reference materials for volatile organic impurities in vodkas to ensure the uniformity, accuracy and reliability of measurements, and for the purpose of implementing import substitution policy.

88-100 9
Abstract

The measurement of percentage elongation after fracture is a method-dependent procedure whose results are not traceable to a corresponding standard of the unit of the same quantity. The standardized methods used in laboratory practice (e. g., GOST 1497–2023 “Metals. Methods of tensile testing”) allow a wide variability of regimes and therefore possess substantial uncertainty, which makes the development of a national metrological instrument of the highest accuracy for verifying the accuracy of testing and certifying reference materials an urgent task.
The aim of the study was to develop and validate a State Primary Reference Measurement Procedure for measuring percentage elongation after fracture under static tension of cylindrical steel specimens, ensuring an absolute expanded uncertainty of no more than 0.24 %.
Cylindrical specimens of steels (carbon, low-alloy, corrosion-resistant) and foreign-made reference materials were used as test objects. To eliminate subjective errors of measurements with contact instruments, an optical method using a video measuring microscope certified as a standard unit of length 4 grade was applied. Dynamic effects were minimized by strictly limiting the loading rate in the elastic region to the range of 3 to 4 N/(mm² s). To calculate the methodological components of the uncertainty budget related to the operation of mark-recognition algorithms and operator qualification (density of manual joining of the fractured specimen parts), the multivariate analysis of variance (ANOVA) was applied.
A detailed uncertainty budget for this type of testing has been developed, and the final equation for the maximum value of expanded uncertainty has been derived. The equivalence of the developed procedure to the international basis for comparison was statistically confirmed using the Cochran-Cox criterion. Based on interlaboratory comparisons, the highest accuracy of the State Primary Reference Measurement Procedure compared with the standard method GOST 1497–2023 has been mathematically proven. The developed State Primary Reference Measurement Procedure ensures results of the highest accuracy without direct traceability to state primary standards. The procedure is intended for establishing the certified values of reference materials for mechanical characteristics of steels, as well as for arbitration testing, correctness and within-laboratory precision control, and verification of software of tensile testing machines.

Guidance materials. Regulations. Standards

101-110 8
Abstract

This paper presents the first summary in Russian scientific periodicals on metrology of the fundamental provisions of the new international standards of the ISO 33400 –  ISO 33408 series. An overview of the changes in documents that previously had the status of ISO/REMCO Guides is provided. Plans for their implementation into Russian and interstate practice of production and application of reference materials are outlined.
The main international standard that must be met by the activities of calibration and testing laboratories is ISO/IEC17025:2017 «General requirements for the competence of testing and calibration laboratories». This standard requires the use of reference materials produced by competent producers. One way to confirm such competence is compliance with the requirements of ISO 17034:2016 “General requirements for the competence of reference material producers”. To meet the requirements of ISO 17034, Technical Committee ISO/TC334 transformed the ISO/REMCO Guides into the ISO 33400 series of standards:
• ISO 33400 Reference materials –  Vocabulary;
• ISO 33401:2024 Reference materials –  Contents of certificates, labels and accompanying documentation;
• ISO/TR33402:2025 Good practice in reference material preparation;
• ISO 33403:2024 Reference materials –  Requirements and recommendations for use;
• ISO 33405:2024 Reference materials –  Approaches for characterization and assessment of homogeneity and stability;
• ISO 33406:2024 Approaches for the production of reference materials with qualitative properties;
• ISO 33407:2024 Guidance for the production of pure organic substance certified reference materials;
• ISO 33408:2025 Guidance for the production of pure inorganic substance certified reference materials.
The translation of the listed international documents into Russian was carried out by specialists of the Scientific Methodological Centre of the State Service for Reference Materials for the Composition and Properties of Substances and Materials (SMC GSSO). Technical versions of the documents reviewed in this article are available on the portal of the State Service for Reference Materials for the Composition and Properties of Substances and Materials (GSSO) at https://gsso.ru/about_proj_remco/.

Aspects of Maintaining the State Register of Type Approved Reference Materials



ISSN 2687-0886 (Print)