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Design and Pilot Production of a Polish Lake-Water Candidate Certified Reference Material (the MPWN Project)

Metrology & Hallmark

Authors Anna Ruszczyńska, Jakub Karasiński, Marcin Wojciechowski, Andrzej Gawor, Olha Dushna, Dominika Łukasik, Ewa Bulska (University of Warsaw, Faculty of Chemistry, Biological and Chemical Research Centre, Warsaw, Poland), Aldona Kubala-Kukuś, Dariusz Banaś (Jan Kochanowski University of Kielce, Institute of Physics, Kielce, Poland)

Abstract

In the context of European water-monitoring policy, we report a pilot study to develop certified reference material (CRM) for the elemental composition of lake water in Poland. Target measurands and concentration ranges were defined in accordance with the Water Framework Directive, Polish regulations, and the fit-forpurpose needs of monitoring laboratories using instrumentation with diverse analytical performance (from μg·L⁻¹ to tens of μg·L⁻¹ for trace elements and mg·L⁻¹ for major ions). Although inductively coupled plasma mass spectrometry was used for CRM characterisation, the candidate material was formulated to be compatible with routinely available techniques, including atomic absorption spectrometry, flame emission photometry, inductively coupled plasma optical emission spectrometry, and total reflection X-ray fluorescence. The analyte panel includes Al, As, B, Ba, Be, Bi, Cd, Co, Cr, Cu, F, Fe, Hg, Li, Mn, Mo, Ni, Pb, Rb, Sb, Se, Sr, Tl, U, V, Zn, and the major elements Ca, Mg, Na, and K. Following screening of the characteristics of three lakes, the Marksoby site was selected as the source matrix. A 60-L lot was prepared and bottled under controlled conditions (220 units) and evaluated for between- and within-bottle homogeneity to support data comparability. This manuscript documents the selection, preparation, and pre-certification studies. The certification campaign, together with the assignment of certified values and the evaluation of their associated uncertainties, is described in a separate study.

Bibliography

[1] European Parliament and Council of the European Union. Directive 2000/60/EC of the European
Parliament and of the Council of 23 October 2000 establishing a framework for Community action in the field of water policy. Official Journal of the European Communities. 2000;L327:1–73.
[2] European Parliament and Council of the European Union. Directive (EU) 2020/2184 of the European Parliament and of the Council of 16 December 2020 on the quality of water intended for human consumption (recast). Official Journal of the European Union. 2020;L435:1–62.
[3] Dziennik Ustaw Rzeczypospolitej Polskiej. Obwieszczenie Marszałka Sejmu Rzeczypospolitej Polskiej z dnia 14 października 2021 r. w sprawie ogłoszenia jednolitego tekstu ustawy – Prawo wodne. Dz.U. 2021 poz. 2233.
[4] Dziennik Ustaw Rzeczypospolitej Polskiej. Ustawa z dnia 20 lipca 2017 r. - Prawo wodne. Dz.U. 2017 poz. 1566.
[5] Pavoni E, Crosera M, Petranich E, Oliveri P, Klun K, Faganeli J, et al. Trace elements in the estuarine systems of the Gulf of Trieste (northern Adriatic Sea):+A chemometric approach to depict partitioning and behaviour of particulate, colloidal and truly dissolved fractions. Chemosphere. 2020 Aug;252:126517.
[6] Jerez Veguería SF, Godoy JM, de Campos RC, Gonçalves RA. Trace element determination in seawater by ICP-MS using online, offline and bath procedures of preconcentration and matrix elimination. Microchemical Journal. 2013 Jan;106:121–8.
[7] Gaillardet J, Viers J, Dupré B. Trace Elements in River Waters. In: Treatise on Geochemistry. Elsevier; 2003. p. 225–72.
[8] Wysocka I., Determination of rare earth elements concentrations in natural waters - A review of ICP-MS measurement approaches. Talanta. 2021;221:121636.
[9] Rusiniak P, Ruszczyńska A, Wątor K, Bulska E, Kmiecik E. Methodological aspects concerning sampling and determination of total selenium and selenium species in geothermal waters. Bulletin of Geography Physical Geography Series. 2020 Jun 1;18(1):5–16.
[10] International Organization for Standardization. ISO 17034:2016 – General requirements for the competence of reference material producers. Geneva; 2016.
[11] ISO/IEC 17025:2017 General requirements for the competence of testing and calibration laboratories, Edition 3 2017-11.
[12] Olivares IRB, Souza GB, Nogueira ARA, Toledo GTK, Marcki DC. Trends in developments of certified reference materials for chemical analysis - Focus on food, water, soil, and sediment matrices. TrAC Trends in Analytical Chemistry. 2018 Mar;100:53–64.
[13] National Centre for Research and Development (NCBR). DOB-BIO6/16/44/2014: Competition No. 6/2014—Research and development for national defence and security [project]. Warsaw (Poland): NCBR; 2014.
[14] The National Centre for Research and Development in the frame of the project MODAS No. INNOTECH-K1/IN1/43/138947/NCBR/12 for the period 2012–2015, Warsaw, Poland.
[15] Godlewska-Żyłkiewicz B, Leśniewska B, Bulska E, Some problems in the production of hair intercomparison material. Chemical Analysis (Warsaw).2002;47(5):737–746.
[16] Isleyen A, Can SZ, Cankur O, Engin BA, Vogl J, Koenig M, et al., Certification of the total element mass fractions in UME EnvCRM 03 soil sample via a joint research project. Accreditation and Quality Assurance. 2024 Aug 23;29(4):293–301.
[17] Karasiński J, Tetfejer K, Radziński P, Tupys A, Gambin A, Bulska E, et al. Coprecipitation as a One-Step Se Separation for Determination of Isotope Ratios Completed with Revised Uncertainty Evaluation. Anal Chem. 2024 Mar 5;96(9):3763–71.
[18] Bulska E. Metrology in Chemistry. Cham: Springer; 2018. doi:10.1007/978-3-319-99206-8.
[19] PN-EN ISO 17294-2:2024-04. Water quality - Application of inductively coupled plasma mass spectrometry (ICP-MS) - Part 2: Determination of selected elements including uranium isotopes.
[20] International Organization for Standardization. ISO 33400:2026. Reference materials — Vocabulary. Geneva: ISO; 2026.
[21] ISO 33401:2024 Reference materials — Contents of certificates, labels and accompanying documentation, ISO, Geneva.
[22] ISO 33405:2024 Reference materials — Approaches for characterization and assessment of homogeneity and stability, ISO, Geneva.
[23] ISO 33403:2024 Reference materials — Requirements and recommendations for use, ISO, Geneva.
[24] International Organization for Standardization. ISO/TR 33402:2025, Good practice in reference material preparation. Geneva: ISO; 2025.
[25] ISO 15189:2022 Medical laboratories — Requirements for quality and competence, ISO, Geneva.
[26] ISO 5667-3:2024 Water quality — Sampling Part 3: Preservation and handling of water samples, ISO, Geneva.
[27] Fernández-Turiel JL, Llorens JF, López-Vera F, Gómez-Artola C, Morell I, Gimeno D. Strategy for water analysis using ICP-MS. Fresenius J Anal Chem. 2000 Nov 6;368(6):601–6.
[28] Reimann C, Grimstvedt A, Frengstad B, Finne TE. White HDPE bottles as source of serious contamination of water samples with Ba and Zn. Science of The Total Environment. 2007 Mar;374(2–3):292–6.
[29] Rice EW, Baird RB, Eaton AD, editors. 4500-F Fluoride — Ion-Selective Electrode Method. In:
Standard Methods for the Examination of Water and Wastewater. 23rd ed. Washington, DC: American
Public Health Association (APHA); American Water Works Association (AWWA); Water Environment
Federation (WEF); 2017.
[30] Barałkiewicz D, Gramowska H, Kanecka A, Krzyżaniak I, Gołdyn R. Spatial distribution of major and trace elements in the water of Swarzędzkie Lake (Poland) Environ Monit Assess. 2008 Aug
3;143(1–3):327–36.
[31] Siepak M, Marciniak M, Sojka M, Pietrewicz K. Trace Elements in Surface Water and Bottom Sediments in the Hyporheic Zone of Lake Wadąg, Poland. Pol J Environ Stud. 2020 Mar 31;29(3):2327–37.
[32] Gwoździński K, Mazur J, Pieniążek A. Concentrations of Metals in Water of Unmonitored Lakes Near a Landscape Park. Pol J Environ Stud. 2014;23(4):1317–1321.
[33] Hamlin SN. Preservation of samples for dissolved mercury. Water Resources Bulletin. 1989;25(2):255–262. doi:10.1111/j.1752-1688.1989.tb03060.x.
[34] U.S. Environmental Protection Agency. Method 1631, Revision E: Mercury in Water by Oxidation, Purge and Trap, and Cold Vapor Atomic Fluorescence Spectrometry. EPA-821-R-02-019. Washington, DC: U.S. EPA; 2002.
[35] Ricci M, Kourtchev I, Emons H. Chemical water monitoring under the Water Framework Directive with Certified Reference Materials. TrAC Trends in Analytical Chemistry. 2012 Jun;36:47–57.

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Metrology and Hallmark is devoted to the multidisciplinary study and practice of high accuracy engineering and metrology. The journal takes novel achievements in all fields of measurement and instruments science & technology.

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