Ensuring the uniformity of measurements (EUM) in the field of temperature measurements, in particular radiation thermometry is one of the main tasks of metrology solved at the state level. The system of metrological support (MS) of radiation thermometry means requires continuous maintenance at the level that meets modern requirements of science, technology, and industry. In order to develop and improve the EUM system in radiation thermometry, a number of measures have been taken in recent years, namely: a new standard base has been developed, including the creation of the State primary standard (SPS) of a temperature unit in the range from 0 °C to 3 200 °C, implementing a new definition of kelvin; a new State verification schedule (SVS) has been developed, which regulates the transfer of the temperature unit to working means from the SPS.

To reduce the load on the SPS, decrease the loss of accuracy in the transfer of a unit of thermodynamic temperature and meet the increased requirements for metrological support of measuring instruments, a secondary standard (SS) of a temperature unit was created and studied in accordance with the new definition of kelvin. It included high-temperature blackbody based on fixed points of pure metals and eutectics, a blackbody and comparators that ensure the transfer of a temperature unit in the range from 961.78 °C to 3 200 °C.

Based on the results of the research, the created State secondary standard (reference standard) of the temperature unit in the range from 961.78 °C to 3 200 °C was approved by the order of Rosstandart dated November 21, 2022 No. 2931 and fully meets the requirements in accordance with the SVS for temperature MI.

The present study aims to generalize the experience of creating state reference materials (GSOs) of active substances and determine their main characteristics, standardized both in the State Pharmacopoeia of the Russian Federation and in the regulatory documents of the measurement uniformity assurance system. In connection with the violation of supply chains, the acquisition and use of foreign reference active substances became quite problematic or even impossible. As a consequence of the current difficult situation with the insufficient nomenclature of GSOs, the domestic manufacturers and developers faced urgent problems in creating them. The development of antimicrobial reference active substances will solve urgent issues of strengthening the technological sovereignty of Russia, minimize the import dependence of the Russian economy, as well as ensure the targets of the Strategy for Scientific and Technological Development of the Russian Federation to be achieved. The conclusions of the study can be applied in creating GSOs to substitute imported reference materials or surpass their level.

Virus-like particles (VLPs) have long attracted the attention of biologists and metrologists due to their dual nature. Despite their similarity to viruses, VLPs lack a virus DNA or RNA, thereby posing no threat of infection. The development of methods for the creation and standardization of VLPs, as well as for monitoring their characteristics, represents an important problem in the field of biotechnology and molecular biology. In this work, we aim to substantiate the requirements, methods, and instruments used to ensure the traceability of VLP-based certified reference materials (CRMs). The following methods for characterization of biological and physicochemical properties of such CRMs were considered: mass balance; high-performance liquid chromatography-mass spectrometry (HPLC–MS); gas chromatography-mass spectrometry (GC–MS); Karl Fischer coulometric titration; ion chromatography; inductively coupled plasma mass spectrometry; and isotope dilution. It was established that VLP-based CRMs should meet the following requirements: the presence of molecular patterns common to many pathogenic biological agents (PBAs) but absent in the organism; traceability to SI units (Systeme international d’unites, SI); the absence of own genetic material; the presence only of inactivated homogenous strains when used for vaccine delivery. VLP-based CRMs facilitate metrological support in the field of medicine and vaccine production.

The development of calibration procedures, as well as the certification of readily available reference materials (RMs) and the improvement of their metrological characteristics, are topical issues for thermal analysis methods. In the course of the work, the necessity of conducting a study in order to expand the range of CRMs for temperature and enthalpy of phase transitions is substantiated. The substantiation of the choice of the measurement procedure and starting materials is given. The conditions for conducting experiments are described in detail, and the choice of these conditions is justified. The developed CRMs passed the metrological examination and were included in the Register of approved types of reference materials FIF EUM as a set of certified reference materials for temperature and specific enthalpy of phase transitions (set SOTSF-2) GSO 11890–2022/GSO 11896–2022. The practical significance of the obtained results is as follows: certified reference materials allow expanding the possibility of establishing and monitoring the stability of the calibration characteristics of thermal analysis installations and measuring instruments; certification of measurement procedures (methods) and accuracy control of the measurement results of the phase transition temperature of metals, metal salts, metal oxides, and polymeric materials, organic and inorganic substances.

Over 30 standards and certified measurement techniques are currently used in Russia to determine carbon, oxygen, and hydrogen isotope ratios. The techniques implemented in these documents are based on foreign reference materials (RMs). Similar domestically-produced RMs are not available, which makes the use of these techniques limited in the near future. This study aims to develop a certified RM (CRM) for the isotopic composition of carbon dioxide for ¹³C-urea breath tests. The following objectives were formulated: to develop a technique for obtaining RMs; to manufacture an RM pilot batch; to carry out type approval tests. The RM was manufactured by gravimetric mixing of carbon dioxide of two different isotopic composition from different sources with synthetic air. The mixing ratio was calculated using a specially developed technique. The RM stability was tested by an accelerated aging procedure. Following type approval tests, the developed CRM was included in the Federal Information Fund for Ensuring the Uniformity of Measurements under the registration number GSO 11999–2022. The practical significance of the obtained results is related to the possibility of using the developed CRM for improving the accuracy and validity of ¹³C-urea breath tests. Compared to the analogs, the developed CRM demonstrates a higher chemical purity.

Establishment and control of metrological characteristics of measurements of absorbed ionizing radiation doses in the range of 0.01 and 200 kGy by reference materials is an urgent task due to their wide application in various industries. The most convenient means of metrological support for transferring a unit of absorbed dose rate of intense photon, electron, and beta radiation to measuring instruments in radiation technologies are reference materials with established metrological traceability to the International System of Units (SI). In the present study, a method for expanding the dynamic range of measuring the absorbed dose of high-intensity ionizing radiation by radiochromic film dosimetry systems was considered and tested. The accuracy (uncertainty) of dose measurements was estimated depending on the initial optical density of the radiation-sensitive layer of the radiochromic composition. The possibility of expanding the dose characteristics and improving the metrological characteristics of the existing reference materials of absorbed dose (in water) for use as secondary standards (Measures) of the absorbed dose of ionizing radiation reproducing and (or) storing one or more points of the selected measurement scale of the absorbed dose with increased accuracy (uncertainty) of the measured values of the absorbed dose (in water) in an extended dynamic range was shown.

Electrical steel is a soft magnetic material used in the manufacture of various electrical equipment intended for the transmission and conversion of electricity and used mainly in alternating magnetic fields of industrial frequencies. The key properties of such a material are AC magnetic properties, which are standardized when assessing the compliance of the material with the requirements of both Russian and foreign standards. The article presents information about the aspects of the development of reference materials for AC magnetic properties of electrical cold-rolled non-oriented steel made in the form of strips for the Epstein frame. The main feature of these reference materials is that the value of one of the two certified characteristics (specific power of magnetic losses) is transmitted directly from the State primary standard, and the other (magnetic induction amplitude) is determined in accordance with a certified measurement procedure. Their use will provide the possibility of a comprehensive and reliable determination of the magnetic characteristics of samples of non-oriented electrical steel normalized in accordance with the requirements of current standards.

This article reviews the usage experience and development prospects of four state primary reference measurement procedures (SPRMPs) created to provide metrological support of measurements in the food and agricultural industries. The SPRMPS certified in 2016–2019 include those of the mass fraction of fat, ash, and carbohydrates in food products and raw materials; of the mass fraction of crude fat (oil content) in oilseeds and related products. The mass fraction of fat, crude fat, and oil content is measured using the Randall method; the mass fraction of ash is determined by the thermogravimetric method; the mass fraction of carbohydrates (total sugar) is defined by iodometric titration. The considered SPRMPs were used to develop reference materials (RMs) for the composition of dairy and meat, egg powder, starch, baby food, oilseeds, related products, and compound feeds. SPRMPs implementation required extending the range of the manufactured RMs for new product groups. High-precision procedures for measuring the mass fraction of fat in liquid dairy products, fish, pastry, confectionery, and pasta products, as well as the mass fraction of lactose in liquid dairy products were developed and certified to describe the characteristics of dairy, pollock fillets, and wheat crackers composition.  

Accurate and reliable measurements of the composition of air environments (workplace air, ambient air, industrial air emissions) form a solid basis for decision making in the area of environmental quality. This article deals with the problem of developing and testing techniques for measuring air quality parameters. The disadvantages of the existing techniques are identified. A methodology for creating appropriate techniques is proposed. Procedures for developing reference materials (RMs) for internal and external quality control of measurement results are described, along with approaches to estimating the metrological characteristics of measurement techniques. The process of applying measurement techniques is specified. It is shown that techniques for measuring air quality parameters may be divided for two basic stages, i. e., the stage of analytical sampling and the stage of measuring the required indicators in this sample. This approach expands the possibilities of developing and certifying such techniques, thereby increasing the reliability of measurement results. Using the developed approach, the authors have successfully developed 12 techniques for measuring air quality parameters and four certified reference materials (CRMs). Works in this direction are continued.

Caffeine has traditionally been used to assess and control the metrological characteristics of liquid chromatographs. In recent years, with increasing requirements for the traceability of measurement results, the use of caffeine as a reagent for verification, calibration, and type approval tests has started to contradict the effective regulations governing measurement uniformity. This study aims to develop and test a procedure of caffeine quantification in caffeine via primary coulometric titration for the metrological support of high-performance liquid chromatography (HPLC) with an accuracy of no more than 1 % abs. In the course of work, a detailed analysis of methods for determining caffeine content in various matrices was carried out; in addition, a procedure for determining caffeine mass fraction in caffeine via coulometric titration was developed and tested. A comparison of the obtained results with caffeine mass fraction measurements performed using HPLC confirmed the commutativity of coulometric titration and HPLC. The developed procedure of caffeine quantification in caffeine via primary coulometric titration employing GET 176 can be used to develop a caffeine composition reference material and to provide metrological traceability of HPLC measurements on its basis to state primary standards reproducing the «mass fraction of components» and to SI units (Systeme international d’unites, SI).  

In this work, we develop a procedure for reproducing the units of bismuth mass fraction in metallic bismuth and those of bismuth (III) mass concentration in bismuth nitrate solutions by controlled-potential coulometry based on the GET 176-2019 State primary standard of mass (molar, atomic) fraction units and mass (molar) concentration of components in liquid and solid substances and materials based on coulometry. The results obtained can be used when manufacturing certified reference materials (CRMs) for the composition of high-purity bismuth and CRMs for the composition of solutions of bismuth (III) ions directly traceable to GET 176-2019. These CRMs may find application in pharmacological, metallurgical, and nuclear industries.

An urgent task for accredited testing laboratories is to estimate the uncertainty of test results. In Charpy pendulum impact test the sources of the main contributions from the measuring instrument to the uncertainty of the result are: the angle of rise and the angle of fall of the pendulum, force exerted by the pendulum, and the distance from the axis of rotation to the center of strike. The aim of the work is to describe the method for estimating the uncertainty of the results of Charpy pendulum impact test based on information about the calibration of the impact testing machine and traceability to the reference material of impact energy (absorbed energy) of steel grade 45 GSO 11934–2022. The uncertainty estimation method is based on the statistical model from ISO 21748–2017. Uncertainty estimation was carried out for a pendulum impact tester TE JBW-300 using GSO 11934–2022 type 11 samples according to GOST 9454–78 with a type V-notch concentrator at room temperature. The study found that the greatest contribution to the uncertainty of test results is made by a systematic error associated with traceability to CRM GSO 11934–2022 and a random component of measurements. Accounting of traceability to the CRM GSO 11934–2022 increases the estimate of the uncertainty of the result, but makes it possible to correctly compare the results of two different laboratories, which is of fundamental importance in arbitration tests.

The article analyzes the compliance of Russian legal documents with the Recommendations of the International Organization of Legal Metrology regarding the use of reference materials in the fields covered by the state control and supervision. The problem of ensuring the quality of measurement results is relevant for each laboratory, performing measurements in any fields of activity. In addition to a reliable and proven measurement method, a decisive role in obtaining comparable results is played by reference materials. In order to ensure the traceability of measurements, a reference material must be certified. Certified reference materials are obligatory for the state metrological control and supervision of the quality and safety of food and pharmaceutical products, quality of measurements in clinical laboratories, environmental safety, etc. Considering the important role of reference materials in the process of ensuring the uniformity of measurements in analytical laboratories, this study can contribute to the promotion of ideas for improving the Russian legislative framework in the relevant area.

В этом разделе продолжается публикация сведений о типах стандартных образцов, которые были утверждены Приказами Росстандарта к середине 2023 г. в соответствии с Административным регламентом, в который были внесены изменения согласно Приказу Росстандарта N 1404 от 17.08.2020«О внесении изменений в Административный регламент по предоставлению Федеральным агентством по техническому регулированию и метрологии государственной услуги по утверждению типа стандартных образцов или типа средств измерений» (утв. приказом Федерального агентства по техническому регулированию и метрологии от 12 ноября 2018 г. N 2346). Изменения внесены в целях реализации Федерального закона от 27 декабря 2019 г. N 496-ФЗ «О внесении изменений в Федеральный закон «Об обеспечении единства измерений».

Начиная с 01.01.2021 типы стандартных образцов утверждаются Приказами Росстандарта в соответствии с вступившим в силу Приказом Минпромторга России № 2905 от 28 августа 2020 г. «Об утверждении порядка проведения испытаний стандартных образцов или средств измерений в целях утверждения типа, порядка утверждения типа стандартных образцов или типа средств измерений, внесения изменений в сведения о них, порядка выдачи сертификатов об утверждении типа стандартных образцов или типа средств измерений, формы сертификатов об утверждении типа стандартных образцов или типа средств измерений, требований к знакам утверждения типа стандартных образцов или типа средств измерений и порядка их нанесения».

В свободном доступе более подробные сведения об утвержденных типах СО также можно посмотреть в Федеральном информационном фонде по обеспечению единства измерений на сайте ФГИС Росстандарта – https://fgis.gost.ru/ в разделе «Утвержденные типы стандартных образцов».

В соответствии с требованиями Приказа Минпромторга России от 28.08.2020 г. № 2905 (вступил в силу 01.01.2021 г.) 1 решение о внесении изменений в сведения в части срока действия утвержденного типа стандартных образцов (далее – СО) принимает Федеральное агентство по техническому регулированию и метрологии (Росстандарт) на основании заявления правообладателя утвержденного типа СО 2. К заявлению прилагается заключение по результатам рассмотрения конструкторской, технологической и (или) технической документации стандартного образца, подтверждающее, что изменения в конструкторскую, технологическую и (или) техническую документацию СО не вносились и сведения об утвержденном типе СО, содержащиеся в Федеральном информационном фонде по обеспечению единства измерений, соответствуют технической документации СО. Заявление при внесении изменений в сведения в части срока действия утвержденного типа СО подается не менее, чем за 30 рабочих дней до окончания срока действия утвержденного типа стандартных образцов.

Решение о внесении изменений в сведения об утвержденном типе стандартных образцов принимается Росстандартом в форме приказа с продлением срока действия на последующие 5 лет с даты окончания действия утвержденного типа СО.

СО утвержденного типа, в сведения о которых внесены изменения в части срока действия СО в начале 2023 года, представлены в таблице.