Introduction. The paper gives information on the development of a certified reference material (CRM) for composition of high-purity copper (Cu CRM UNIIM). The CRM is included as the transfer standard into the State primary standard of the mass (molar) fraction and mass (molar) concentration of the component in liquid and solid substances and materials based on coulometry GET 176-2013.

Materials and methods. The CRM represents pieces of oxygen-free copper wire rod, brand KMB, produced according to GOST R 53803-2010, weighing from 0.5 to 1g. The CRM is packed in plastic vials with the capacity of 30 or 50 cm³. The certified characteristic of the CRM is copper mass fraction in copper wire rod, expressed in percentages. The certified value for copper mass fraction was established by the primary method of controlled-potential coulometry using the State primary standard GET 176-2013.

Results. The permitted interval of the certified value for copper mass fraction in the CRM is from 99,950 % to 100,000 %. The relative expanded uncertainty (k=2) of the certified value for copper mass fraction does not exceed 0,030 %; the relative standard uncertainty due to inhomogeneity does not exceed 0.010 %; the relative standard uncertainty due to instability does not exceed 0.010 %. The shelf life of the developed CRM is 10 years provided that standard storage conditions are ensured.

Discussion and conclusions. The developed CRM is included into the State register of type approved RMs under the number GSO 10800-2016. The CRM of high-purity copper (Cu CRM UNIIM) as a transfer standard is intended for reproduction, storage and transfer of the copper mass fraction unit to other reference materials and chemical reagents by the method of comparison using a comparator and by conducting direct measurements. This CRM may also be used:
– for verification of measuring instruments (MIs) according to the state verification schedule described in GOST R 8.735.0-2014,
– for calibration, graduation of MIs; control of metrological characteristics when conducting MI tests, including for the purposes of type approval;
– for validation of measurement procedures, accuracy control of measurement procedures in the process of their implementation.

 

Introduction: Radiochemical production is one of the richest in terms of data for analytical control, high-quality implementation of which is impossible without using type approved reference materials (RMs). Industry-specific institutes used to satisfy the demand for RMs, many of which nowadays have ceased this type of activities due to various reasons. The paper in question covers problems of metrological support in radiochemical production caused by the lack of type approved RMs.

Materials and methods: Technologies used for obtaining homogeneous reference material for radiochemical production are described. Methods and measuring instruments used for certifying RMs are listed.

Results: Results of developing certified reference materials at Mayak Production Association are given. Examples of codeveloping RMs of triuranium octoxide and plutonium dioxide are provided.

Discussion and conclusions: Assessment of the current situation in terms of provision of type approved RMs is given. The paper provides data on availability of raw material, quality of instrument and methodological base in order to create a reference material production site at Mayak Production Association. Results of step-by-step solutions to problems of metrological assurance in radiochemical production are presented. Research prospects of developing RMs for inductively coupled plasma mass spectrometry are outlined. An outlook is given and practical proposals are formulated in the paper. The proposals in question are related to the interaction between institutes and enterprises of the field in terms of developing type approved RMs.

 

The paper presents results of conducting research on the development of a certified reference material (CRM) for specific surface area of quartz sand, which is practically non-porous and therefore has low specific surface area value ~ 0.8 m²/g. The standard uncertainty due to RM inhomogeneity, the standard uncertainty due to RM instability, as well as the standard uncertainty due to characterization were estimated using the State Primary Standard GET 210‑2014 for Units of Specific Absorption of Gases, Specific Surface Area, Specific Volume, and Pore Size of Solid Substances and Materials. The metrological characteristics of the CRM were determined using a low-temperature gas adsorption method. Krypton was used as an adsorbate to increase measurement accuracy.

 Introduction. Activities of FSBI “VIMS” are aimed at ensuring accuracy and comparability of the results of mineralogical analyses accompanying exploration and technological work. Evaluation of the research result quality is carried out with the help of various metrological instruments, one of which is an interlaboratory comparison test.

Purpose. The purpose of interlaboratory comparison tests (ICTs) is to assess the results of X-ray quantitative phase analysis of an artificial mixture of minerals and to confirm the level of competence of testing laboratories.

Methods. The procedure for conducting interlaboratory comparison tests is as follows: development of the programme and its approval; collecting and registering applications from laboratories, willing to participate in the ICT programme; preparation and simultaneous sending of control samples with accompanying information materials to those participating in the experiment; statistical processing of obtained results; drawing up, approval and circulation of documents confirming participation of the laboratories. The control sample is a homogenized artificial mixture of minerals (quartz, kaolinite, calcite and pyrite). The accuracy (quality) control of test results was carried out by X-ray quantitative phase analysis.

Results. The ICT results showed a high level of competence of testing laboratories. For unreliable and unsatisfactory results percentages total less than 11%, the percentage for unfulfilled results is equal to zero. Interlaboratory comparison tests in mineralogical works are an important means for controlling competence of testing laboratories.

Actuality of the research. The need for the development and validation of analysis methods of reagents used for the introduction of elements into reference materials, certified according to the procedure of preparation. The purpose. Development and certification of methods for determining the content of the main component in the reagents used to prepare reference materials. Research methods. Gravimetry, titration, atomic emission spectral analysis with arc excitation, atomic emission spectral analysis with inductively coupled plasma as an excitation source, mass spectral analysis with inductively coupled plasma as ion source. Results. The characteristics of the error of the measurement results are estimated, the Certificates of Attestation of the methods are received, the information is included in the Federal Information Fund.