Gipronickel Institute LLC, St. Petersburg, Russia

L. E. Yakovleva, Chief Specialist, Testing Analytical Center, e-mail: YakovlevaLE@nornik.ru
N. P. Shikhareva, Head of the Reference Materials Sector, Testing Analytical Center
Yu. A. Efimova, Leading Engineer, Testing Analytical Center, Candidate of Chemical Sciences

The Gipronickel Institute`s Testing Analytical Center (TAC) develops certified reference materials (RM) for metrological support of measurements during quality control of nickel, cobalt, copper and industrial products of MMC Norilsk Nickel`s plants. The following areas of development of RM of an approved type are presented in the Gipronickel Institute`s TAC: RM of oxide composition (cobalt, copper, nickel); RM for composition of metals (cobalt, copper, nickel) and RM for composition of industrial products. The methods for determination of the metrological characteristics of RMs are considered:
– calculation and experimental preparation procedure;
– comparison method with RMs of an approved type that have established traceability;
– application of an interlaboratory experiment.
RMs are intended to establish and control the stability of the calibration characteristics of measuring instruments when determining the composition of nickel, cobalt and copper by physicochemical methods for compliance with the requirements of both national and international standards. Traceability of certified RM values to the unit of quantity “mass fraction of component” is ensured by the consistency of the certified RM values with the measurement results obtained on the State Primary Standard. RM tests to confirm the metrological characteristics for the purpose of RM type approval are carried out at the Ural Research Institute of Metrology (branch of the D. I. Mendeleev All-Russian Institute for Metrology). The use of reference materials allows to take into account the requirements of consumers for the quality of cobalt, nickel, and copper produced by MMC Norilsk Nickel. To certify reference materials for the composition of nickel oxide (NOD set) and copper oxide (COD set), methods for measuring the mass fractions of impurities in nickel and copper samples have been developed and certified.

1. GOST R ISO 17034–2021. General requirements for the competence of reference material producers. Introduced: 01.12.2021.
2. GOST 8776–2010. Cobalt. Methods of chemical-atomic-emission spectral analysis. Introduced: 01.04.2011.
3. GOST 31382–2009. Copper. Methods of analysis. Introduced: 01.04.2010.
4. GOST 6012–2011. Nickel. Methods of chemical-atomic-emission spectral analysis. Introduced: 01.01.2013.
5. GOST 8.531–2002. State system for ensuring the uniformity of measurements. Reference materials of composition of solid and disperse materials. Ways homogeneity assessment. Introduced: 01.03.2003.
6. ISO Guide 33405:2024. Reference materials – Approaches for characterization and assessment of homogeneity and stability. Available at: https://www.iso.org/standard/84226.html (accessed: 05.05.2024).
7. Sobina E. P., Aronov P. M., Migal P. V., Kremleva O. N. et al. Algorithms for assessing the homogeneity of reference materials of composition and properties of disperse and solid materials. Etalony. Standartnye obraztsy. 2023. No. 3. pp. 77–91.
8. ISO Guide 35:2006. Reference materials - General and statistical principles for certification. Available at: https://www.iso.org/standard/32269.html (accessed: 10.12.2022).
9. MI 1992-98. State system for ensuring the uniformity of measurements. Metrological certification of reference materials of the substances and materials composition according to the preparation procedure. Basic provisions. Introduced: 01.07.1999.
10. RMG 60-2003. State system for ensuring the uniformity of measurements. Attested mixtures. General requirements for development. Introduced: 01.07.2004.
11. Sobina A. V., Terentyev G. I., Shimolin A. Yu., Zyskin V. M. The role of the state primary standard based on GET 176 coulometry in ensuring traceability of analytical measurement results. Almanakh sovremennoy metrologii. 2018. No. 14. pp. 28–32.
12. Korotkov V. A., Velikaya T. I., Poslavskaya E. S. Developing the atomic spectrometry techniques for cobalt and nickel analysis. Tsvetnye Metally. 2020. No. 12. pp. 94–101.
13. Stakheev A. A., Stolboushkina T. P. Multi-element reference material for inductively coupled plasma methods: development and testing. Etalony. Standartnye obraztsy. 2021. No. 2. pp. 49–57.
14. International database for Certified Reference Materials and their producers COMAR. Certificate entry for Nickel oxide (NiO) ZRM-RS5. Available at: https://www.comar.bam.de/showCertificate/236850 (accessed: 10.10.2024).
15. Grigorovich K. V. New possibilities of modern methods to determine gasforming impurities in metals. Zavodskaya laboratoriya. Diagnostika materialov. 2007. No. 1. pp. 24–27.
16. GOST 8.532–2002. State system for ensuring the uniformity of measurements. Certified reference materials of composition of substances and materials. Interlaboratory metrological certification. Content and order of work. Introduced: 01.03.2003.
17. MI 3174-2009. Recommendation. State system for ensuring the uniformity of measurements. Establishing traceability of certified values of reference materials. Introduced: 01.02.2009.
18. GOST 13938.13–93. Copper. Methods for determination of oxygen. Introduced: 01.01.1995.
19. Pankov A. N., Zyryanova I. N., Kremleva O. N., Volodina E. M. et al. The need and potential for import substitution of reference materials in the Russian Federation: analysis of data from the Foundation for Ensuring the Uniformity of Measurements. Etalony. Standartnye obraztsy. 2024. No. 1. pp. 47–58.
20. Kolpakova E. K., Khuzagaleeva R. K., Stepanovskikh V. V. Planning an interlaboratory experiment in the production of reference materials of JSC ISO and statistical processing of the obtained results. Zavodskaya laboratoriya. Diagnostika materialov. 2023. No. 2. pp. 28–32.
21. ISO 33401:2024. Reference materials — Contents of certificates, labels and accompanying documentation. Available at: https://www.iso.org/standard/84222.html (accessed: 12.01.2024).