Preview

Measurement Standards. Reference Materials

Advanced search
Vol 20, No 1 (2024)
View or download the full issue PDF (Russian)
31-46 388
Abstract

Reference materials certified using State primary standards form the basis for ensuring metrological traceability to the corresponding measurement units. The article presents the results of the development of a series of new reference materials for the composition of pure organic substances, intended primarily for calibrating chromatographic equipment with various types of detection.

The developed reference materials ensure traceability of the results of verification (calibration) of standards and measuring instruments, as well as measurement results in various areas of state regulation to ensure the uniformity of measurements. Certified values of reference materials were established by an indirect method – t he mass balance method. Metrological traceability of certified values is ensured by direct measurements on the State Primary Standard GET 208. Reference materials are pure substances packaged in glass ampoules (n-dodecane, n-heptane, n-hexadecane, benzene) or vials (hexachlorobenzene, lindane, reserpine, caffeine, glucose, sucrose, anthracene). The mass fraction of the main component of the reference material is in the range from 98.00 to 99.99 %, the relative expanded uncertainty (at k = 2, P = 0.95) does not exceed 0.5 %. The shelf life of reference materials is established by the accelerated aging method and is 3 years under recommended storage conditions.

The article is of interest to industry specialists –  metrologists, chemists, ecologists who control technological processes in various fields of activity, including the food and chemical industries, environmental protection, and scientific research.

The described reference materials are commercially available to all interested parties.

This study can provide empirical material for research in the field of serial production of reference materials, which can be used as a basis for the certification of other substances –  similar organic substances.

47-58 409
Abstract

The deep integration of the Russian economy into the global economy at the turn of the XX–XXI centuries did not bypass the production of reference materials (RM). Domestic testing, verification, and calibration laboratories receive some RMs from abroad. The number of these RMs is an extremely relevant issue at the moment, since the global competition of national economies for the right to dominate their own markets with state-limited borders has intensified.

The strategy of the Russian Federation aimed at achieving the maximum level of sovereignty and independence of the national production sector extends to the sphere of metrological support for the activities of business entities. The practical implementation of this strategy requires a comprehensive analysis of the information presented in the Federal Information Fund for Ensuring the Uniformity of Measurements (FIF EUM) on the number of foreign RMs, the scope of their application, and an understanding of the structure of demand for foreign RMs within the country. At the same time, it is necessary to form an idea of the technical capabilities of producing domestic RMs.

The article provides solutions to most of the problems stated above. The data presented by the authors can be the basis for making management decisions in the field of production and circulation of metrological support equipment for production.

Standards

7-15 485
Abstract

A method for obtaining homogeneous deformation along the length of the measuring section of a uniform-strength beam and the possibility of its application as part of a working deformation standard are considered. The results of the analysis of the bending model and the design of a uniform-strength beam are presented. In the focus of attention are the parameters included in the measurement equation and related to methodological factors, as well as influencing the result of relative deformation measurements. The subjects of research are the presence of contact friction forces, heterogeneity of material properties, the special nature of the load application (bending, torsion, the presence of residual stresses in the body, geometrical parameters of the calibration beam, orientation of primary transducers on the beam, application of bending load, measurement of deflection and displacement of the neutral layer). The advantages and disadvantages of using a uniform-strength beam for determining the characteristics of primary strain transducers during testing, calibration, and verification were established. The deviation of signals of primary transducers located outside the axial cross-section when oriented along the beam axis and along the force lines converging at the point of load application was experimentally revealed. The error due to the orientation of the primary transducers on the beam depending on the angle between the lateral faces can range from 0.15 to 0.23 %. The study adds to the theoretical knowledge base on the possibility of using a cantilever uniform-strength beam as a load-bearing element in calibration installations. The conclusions may be useful for testing, calibrating, and verifying primary strain transducers.

17-30 307
Abstract

Viscosity is the most important property of liquid medium, determining the quality, as well as the possibility of their processing and transportation. Viscosity measurements are performed in many industries to control technological processes in which viscosity is one of the controlled parameters of the final product. Accuracy of viscosity measurements is also necessary in medicine and biology to organize research for new materials.

This review article raises issues of measuring liquid viscosity using the capillary method, reveals the factors and reasons justifying the emergence of the capillary method as the main method of high-precision measurements used in many countries.

The author describes two standard complexes from GET 17–2018 State Primary Standard of Dynamic and Kinematic

Liquid Viscosities. The first is EK GET 17/1-KVI designed for reproducing, storing, and transmitting a unit of kinematic viscosity in the temperature range from 20 to 40 °C. The second is EK GET 17/2-KVN designed for reproducing, storing, and transmitting a unit of kinematic viscosity in the temperature ranges from –40 to +20 °C and from 40 to 150 °C. The focus is on the operating principle and main metrological characteristics of these reference complexes, as well as the results of international key comparisons involving them.

In the future, the research materials may influence the development vector of means and methods for measuring liquid viscosity.

Information. News. Events

Modern methods of analysis of substances and materials

59-84 401
Abstract

The article raises the problem of incomparability of measurement results obtained by different methods of measuring fat content in food products and food raw materials. The problem identified by the author can be solved by developing metrological support for measurements in the food industry. The purpose of the study is to analyze methods for measuring fat content in food products and food raw materials, as well as to revise the state of their metrological support. A brief description, applications, advantages and limitations of extraction-gravimetric, butyrometric, refractometric, chromatographic, ultrasonic, turbidimetric, NMR, and IR spectroscopic methods for measuring fat content are presented. Standardized measurement techniques regulated in national (GOST R), interstate (GOST), and international (ISO, AOAC) standards are analyzed, taking into account the method used, areas of application, and metrological characteristics. An overview of testing equipment and measuring instruments for implementing various methods for determining fat content is given. Particular attention is paid to the consideration of certified express analyzers of food products and food raw materials. A list of certified reference materials for the composition of dairy and grain-milk products, fish and meat products, oilseeds and their processed products, compound feed, egg powder and wheat crackers with a certified value of the mass fraction of fat is provided, their metrological characteristics and certification methods are listed. Based on the results of the study, the main features and problems of ensuring the uniformity of measurements of fat content in food products and food raw materials were formulated, and perspective directions for the development of metrological support were identified.

93-103 289
Abstract

The accuracy of the forecasting method and its prior estimation when predicting changes in the error of the working measurement standard are one of the key issues. In the course of studying these issues, a number of components of the forecasting error were assessed, and various methods and mathematical models of forecasting were compared. A comparative analysis showed that the studied mathematical model for individual forecasting of changes in the error of a working standard available at «Mathematical model for predicting changes in the value of the critical component of the error of the working measurement standard of the unit of magnitude taking into account prior information» has higher accuracy in comparison with the considered known forecasting methods. The estimates of the parameters of the forecasting function obtained with the application of the model under consideration available at «Determination of parameters for metrological maintenance of measuring instruments by the technical and economic criterion», using the expressions of the transition to forecasting the probability of metrological serviceability of the working measurement standard, specific costs for metrological maintenance, and damage from the use of the working measurement standard in the state of metrological failure, allow to substantially increase the validity of decisions to refine the value of the interval between the certification of the working standard, which is initially established (within the framework of the ITCM).

85-92 244
Abstract

One of the main directions of modern activity of metrology researchers is to provide the real sector of the economy of the Russian Federation with reference materials that have no analogues in the country. The article discusses the research of highly efficient materials for fuel cladding (fuel elements) in the active zones of thermal reactors, the scope of which is wide. The purpose of the study is the development of samples of the composition of the zirconium alloy to establish and control the stability of the calibration curves of spectrometers when determining the mass fraction of hydrogen, provided that the metrological and technical characteristics of the reference material meet the requirements of the measurement procedure. The main methods for determining the hydrogen content in materials are analyzed. It has been established that the method of glow discharge optical emission spectroscopy has found the widest application. It has also been established that zirconium alloys are chosen as the main material in most cases.

The need to create samples for constructing a calibration curve for spectrometers for measuring the hydrogen content in a zirconium alloy is noted. Samples of zirconium alloy Zr-1Nb (grade Э110) have been developed to construct a calibration curve using a glow discharge emission spectrometer for measurements with a mass fraction of hydrogen from 0.034 to 0.498 %. Calibration is carried out using the developed samples to obtain a calibration curve using the example of an emission glow discharge spectrometer of the GD Profiler2 type. The relative error of the hydrogen mass fraction obtained during calibration does not exceed ± 10 %.

The practical significance of the study lies in the development of samples that can be used to calibrate spectrometers based on the method of glow discharge optical emission spectroscopy.



ISSN 2687-0886 (Print)