Standards
This article discusses the problem of verification of heavy scales by currently existing methods that involve the use of reference weights and the possibility of expanding the scope of force standards for verification of heavy scales. The essence of the problem is the existence of technological and economic difficulties in the application of these methods of transferring a measurement unit, as well as the incompatibility between the normalized metrological characteristics of mass measuring instruments and force standards.
The authors proposed a new method for transferring a measurement unit to heavy scales using force-reproducing hydraulic machines as force standards. Within the research, this method was tested, the requirements for force standards used for verification of heavy scales were formed, and experimental studies were carried out in order to verify the compliance of force standards with these requirements. On the example of hydraulic force-reproducing machines, the compliance of force standards with these requirements was shown.
There is described an approach to the metrological support of measurements of large masses using force standards. In view of the relative ease of the method implementation, a new method of transferring a measurement unit based on this approach has the prospect of becoming the most common and accessible method for verification of heavy scales. Therefore, it is advisable to expand the scope of existing 1st category force standards.
An especially important direction in metrological science is ensuring the accuracy of vacuum measurements, which is crucial for industry. In Russia, predominantly foreign vacuum gauges with a vacuum measurement range PNPI – PVPI 0.1–1000 Pa are used as reference vacuum gauges for verification and calibration of vacuum gauges. On the basis of the analysis of the characteristics of reference vacuum gauges used in Russia based on various methods for measuring gas pressure, it can be argued that the most accurate and common measurement method among reference vacuum gauges is the strain method. However, the strain method has a number of limitations associated with the need to introduce the following corrections: correction for the residual pressure in the comparative chamber, correction for the influence of temperature effects during temperature control of the primary measuring transducer.
The purpose of this work was to study the compliance of the metrological characteristics of a vacuum gauge based on a new strain-frequency method for measuring the absolute gas pressure with the requirements for reference vacuum gauges given in state verification schemes in the field of vacuum measurements.
The main research methods were the study of the metrological characteristics of the strain-frequency vacuum gauge, taking into account the correction for the residual pressure in the comparative chamber; corrections for the influence of temperature effects during temperature control of the primary measuring transducer, as well as for the compliance of the method with the requirements of state verification schemes in the field of vacuum measurements. An assessment of the accuracy indicators of the strain-frequency method for measuring the absolute gas pressure based on the analysis of the measurement equation, taking into account the assessment of the components of the uncertainty sources, is given. The obtained results have shown the possibility of using the strain-frequency method of pressure measurement, with the exception of the correction for the residual pressure in the comparative chamber, corrections for the influence of temperature effects during temperature control of the primary measuring transducer in reference vacuum gauges that meet the requirements of state verification schemes in the field of vacuum measurements.
As a result of the study, it was found that the expanded uncertainty of the result of measuring pressure with a vacuum gauge based on the new strain-frequency method does not exceed 2 %. This makes it possible to use this method in reference vacuum gauges.
The practical significance of the developed scientific and methodological principles, and technological solutions for calculating and manufacturing the primary measuring transducer of a vacuum gauge based on a new method for measuring low absolute pressure lies in the possibility to manufacture the primary measuring transducer at Russian enterprises using domestic technologies of microsystem technology.
Reference materials
The study discusses the issues of improving the accuracy of measuring high hydrogen concentrations in the development of storage materials in the hydrogen energy industry. The purpose of the study was to develop reference materials for calibration of the hydrogen analyzers at high concentrations. The main methods for determining the hydrogen content in materials were analyzed. It was established that the extraction method in an inert gas medium has found the widest application. The main methods for determining the hydrogen content in materials are analyzed, it is established that the extraction method in an inert gas medium has found the widest application. The need for calibration of analyzers on reference materials with a high hydrogen concentration was noted. Reference materials of titanium alloy VT-1-0 with hydrogen concentration up to (4.0±0.1) wt.% have been developed. The optimal parameters for the analysis were selected. On the example of the hydrogen analyzer RHEN602 (LECO, USA), calibration was carried out on the developed reference materials to obtain a calibration dependence. The reliability of the obtained calibration curve with the application of stoichiometric zirconium hydride was estimated. The confidence interval of the resulting calibration curve was ±10 %. It has been established that the calibration on the developed materials makes it possible to analyze materials with a hydrogen content of 0.5 to 4.0 wt.%. The practical significance of the study lies in the development of reference materials that can be applied to calibrate hydrogen analyzers operating on the principle of melting in an inert gas medium at a high hydrogen concentration.
Modern methods of analysis of substances and materials
Pure organic substances are the first and key link in the chain of metrological traceability in organic analysis. In most cases, purity determination of the organic substance is a non-trivial task, the solution of which requires preliminary theoretical study and understanding of the capabilities of instrumental methods for developing a pertinent analytical procedure.
Within the study, an algorithm for determining the purity of a separate group of organic compounds – ortho-phthalic acid esters (phthalates) was developed based on the mass balance model and the general algorithm for characterizing substances suitable for isolation or purification by distillation. An additional classification of probable impurities (into five types A – E) depending on their qualitative and quantitative characteristics is proposed, as well as suitable analytical methods for measuring impurities and confirming the identity of the main component are identified.
The proposed algorithm was implemented on the State Primary Standard GET 208 to determine the purity of six priority phthalates: dimethyl phthalate, diethyl phthalate, di-(n-butyl) phthalate, benzyl butyl phthalate, di-(2-ethylhexyl) phthalate, and di-(n-octyl) phthalate. Certified pure phthalates were used to create a certified reference material for the composition of a solution of orthophthalic acid esters (phthalates) in methanol (6Ftlt-VNIIM) GSO 11366–2019.
The study revealed that the adapted algorithm considers the specifics of work with the phthalates group and the features of the separation of probable impurities within the MB model, and is universal for all congeners of the group, but does not exclude the natural constraints of the mass balance method.
TO BE DISCUSSED
The accelerated implementation of digital technologies in the economy and social sphere is one of the national priorities in the Russian Federation. One of the components of this stage of industrial development is the creation of a comprehensive cloud platform for the complete automation of metrological centers and the implementation of the strategy for ensuring the uniformity of measurements ≪Metrology 4.0≫. Considering the numerous advantages of implementing digital systems and services, the integration of digital systems into life is associated with a number of difficulties, such as the lack of a single API protocol in the exchange of databases, the lack of unified standardized directories, etc.
The purpose of this study is compilation of information about existing foreign and national cloud-based solutions in the field of ensuring the uniformity of measurements, identification of their shortcomings and finding solutions to emerging problems, taking into account the conditions of modern technologies.
The main research methods were an analysis of the current situation in terms of metrological digital services in the Russian Federation, as well as in Germany, India in the USA and other countries. A comparison of approaches to the construction and prospects of the metrological cloud is carried out. The problems of introducing innovative technologies are described. The study using the example of FSIS ≪ARSHIN≫ showed that this digital service used in the Russian Federation does not have comprehensive functionality for organizing the metrological activities of enterprises and has limitations that do not allow moving to a new stage of digitalization. The main disadvantages of FSIS ≪ARSHIN≫ include the following: insufficient expansion of the coverage of measuring instruments, the impossibility of automatic processing of information about measuring instruments, as well as the lack of infrastructure for obtaining direct measuring information through cloudbased technologies.
As part of solving the problem, the author proposed a scheme for improving the FSIS ≪ARSHIN≫ system which includes: an algorithm for creating a uniform standard for the formation of systems for processing, storing and analyzing data of measuring instruments and reference materials; the creation of universal digital directories that allow describing measuring instruments for the formation of the scope of accreditation in the configurator of the Federal Accreditation Service; the creation of a unique identification number for the measuring instrument and reference material; the implementation of a secure mechanism for unique identification, verification and transmission of data on a measuring instrument based on blockchain technologies.
This scheme can be integrated into the FSIS ≪ARSHIN≫ and undergo trial operation without additional financial costs from the budget of the Russian Federation. This approach of gradually increasing the digital capabilities of the state, as well as ensuring safe work with large amounts of data, makes it possible for further digitalization and the prospect of developing a system for ensuring the uniformity of measurements in the Russian Federation.
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