Standards
The issue of the role of VNIIMS as the leading scientific organization in the field of legal metrology and the leading scientific and practical centre for metrological support of various sectors of the national economy is considered. The paper provides information on the equipment of the institute with standards in the field of physical and chemical measurements. The characteristics of experimental sample of the State Primary Standard of the unit of catalytic activity – katal, characteristics and fields of application of state standards of units of the VNIIMS in the field of physical and chemical measurements are given. The describes the plans of VNNIMS in accordance with the List of Critical Technologies of the Russian Federation, state programs for the development of industries.
Reference materials
Introduction The introduction indicates the need for the use of permanent magnets in various technology fields. The necessity of measuring the limit magnetic hysteresis loop for the correct calculation of magnetic system parameters is considered. The main sources of error when measuring boundary hysteresis loops are given. The practical impossibility of verifying blocks of magnetic measuring systems element-by-element is noted. This paper is devoted to the development of reference materials (RMs) for the magnetic properties of hard magnetic materials based on Nd2Fe14B, a highly anisotropic intermetallic compound.
Materials and measuring methods Nd-Fe-B permanent magnets were selected as the material for developing the RMs. RM certified values were established using a CYCLE‑3 apparatus included in the GET 198‑2017 State Primary Measurement Standard for units of magnetic loss power, magnetic induction of constant magnetic field in a range from 0.1 to 2.5 T and magnetic flux in a range from 1·10–5 to 3·10–2 Wb.
Results and its discussion Based on the experimentally obtained boundary hysteresis loops, the magnetic characteristics were evaluated, the interval of permitted certified values was set, the measurement result uncertainty of certified values was estimated, the RM validity period was established and the first RM batch was released.
Conclusion On the basis of conducted studies, the RM type for magnetic properties of NdFeB alloy-based hard magnetic materials was approved (MS NdFeB set). The developed RM set was registered under the numbers GSO 11059–2018 / GSO 11062–2018 in the State RM Register of the Russian Federation.
Modern express methods of analytical control are widely used for monitoring the quality of oxide materials. However, the possibilities of these methods are currently limited by the lack of versatile homogeneous reference materials (RMs). Such RMs can be produced most effectively by vitrification methods. In this connection, glassy RMs based on bismuthborate systems are of great interest. In the earlier research, bismuth-borate RMs were used for comparison purposes in determining the composition of complex oxide systems using the X-ray fluorescence method. This work considers issues associated with the synthesis and application of bismuth-borate glassy RMs for determining the content of transition elements in oxide compounds and mixtures using luminescence analysis. Luminescence analysis was used as a research method due to its high selectivity and low detection limits with respect to elemental impurities in controlled objects (usually constituting 1 · 10–6–1 · 10–4 wt %). Bismuth-borate glassy RMs are shown to be capable of luminescence under UV radiation in the visible range at the temperature of 77 K. It is established that the introduction of the oxides of transition and rare earth elements (REE) into the RM composition leads to the quenching of the exciton emission band in the glasses studied at 77 K, as well as to the appearance of bands typical of REE ion radiation both at 77 K and at 298 K. Glassy RMs doped with transitionelement oxides are found to quench the luminescence of both bismuth and REE ions at the temperature of 77 K. On the basis of the results obtained, procedures for determining the content of quenching elements in oxide materials have been developed. The metrological characteristics of these procedures have been evaluated.
This paper presents the results of the identification procedure certification and subsequent quantitative determination of the active ingredients of two-component injectable medicines (active ingredient and solvent) using Raman spectroscopy. The main objective of the research was to select approaches for estimating the metrological characteristics of the measurement procedure, which include consideration of the methodological parameters and provide the metrological traceability of measurement results to SI units. According to this purpose, the GVET 176‑1‑2010 State Secondary Measurement Standard for units of mass fraction, mass (molar) concentration of components in solid and liquid substances and materials based on volumetric titration was used. The following substances were chosen as the research objects for estimating the metrological characteristics of the measurement procedure: ascorbic acid, novocaine and sodium thiosulphate. The authors of the work have demonstrated the measurement-procedure certification results, whose accurate determination was confirmed by the results of interlaboratory comparisons. The obtained results confirmed the accuracy of the identification procedure and subsequent quantitative determination, which proves its applicability for the determination of the active ingredients in two-component injectable medicines. In addition, the possibility of developing reference materials based on the medicines under study is indicated. Further development of this study may be directed at the development of an identification procedure and its certification, with subsequent quantitative determination of the active ingredients of injectable medicines having three components as well as those having a more complex composition.
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