Abstract
This article presents information on the development of a new type of certified reference material (CRM) of the mass fraction of dioxins in animal fat, assured with metrological traceability. A procedure for preparing and certifying the CRM is provided. GC-LRMS in combination with isotopic dilution was used as an analytical method for establishing certified characteristics. The uncertainties induced by the CRM inhomogeneity and instability were estimated in order to account for their contribution to the combined uncertainty of the obtained certified values. In addition, the results of interlaboratory comparisons (ILC) studies for an experimental batch of the developed CRM are presented. Measurement results provided by ILC participants are shown to be in good agreement with the certified characteristics of the CRM. The certified values of the mass fractions of dioxins (PCDF group) in the CRM are established to vary from 1 to 1000 ng/kg, with the relative expanded uncertainty ranging from 10 to 20%.
Keywords
- Certified reference materials
- Dioxin
- Certified value
- Uncertainty
- Traceability
- Mass balance method
- Inhomogeneity
- Stability
This is a preview of subscription content, access via your institution.
Buying options



Abbreviations
- HpCDD:
-
Heptachlorodibenzo-p-dioxins
- HpCDF:
-
Heptachlorodibenzofurans
- HxCDF:
-
Hexachlorodibenzofurans
- HxCDD:
-
Hexachlorodibenzo-p-dioxins
- OCDD:
-
Octachlorodibenzo-p-dioxin
- OCDF:
-
Octachlorodibenzofuran
- PeCDD:
-
Pentachlorodibenzo-p-dioxins
- PeCDF:
-
Pentachlorodibenzofurans
- TCDD:
-
Tetrachlorodibenzo-p-dioxins
- TCDF:
-
Tetrachlorodibenzofurans
References
The effects of herbicides in South Vietnam. Part A. Summary and conclusion (1974) National Academy of Sciences, Washington
Ambient water quality criteria 2,3,7,8-tetrachlorodibenzo-p-dioxin: report EPA-400/5-84/007 (1984) Office of water regulations and standards, Washington
Vysochin VI (1989) Dioxin and related compounds: analytical review. GPNTB SO AN SSSR, Novosibirsk (in Russ.)
Gough M (1986) Dioxin, agent orange: the facts. Plenum press, NY
Fedorov LA (1993) Dioxins as an environmental hazard: a retrospective and prospects. Nauka, Moscow (in Russ.)
Maistrenko VN, Klyuev NA (2004) Ecological and analytical monitoring of persistent organic pollutants. BINOM. Laboratoriya znanii, Moscow (in Russ.)
Drugov YS, Rodin AA (4th eds) (2006) Gas chromatographic analysis of polluted air: a practical guide. BINOM. Laboratoriya znanii, Moscow (in Russ.)
Registries of dioxins and furans. National and regional PCDD/PCDF emissions (1999) United Nations Environment Program, Geneva
Stockholm Convention on Persistent Organic Pollutants (2001) Stockholm
Pozdnyakov SP, Rumak VS, Sofronov GA, Umanova NV (2006) Dioxins and human health. Nauka, Saint Petersburg
TR CU 021/2011 Technical Regulations of the Customs Union “On food safety” (2018). Available via Eurasian Economic Union. https://docs.eaeunion.org/pd/ru-ru/0102880/pd_16052018. Accessed 20 Sept 2018
Commission Regulation (EC) No 1881/2006 Setting maximum levels for certain contaminants in foodstuffs. Official J Eur Union 49 (L 364)
GOST 31792-2012 (2014) Fish, marine invertebrates and their products. Determination of dioxins and dioxin-like polychlorinated biphenyls by the chromatographic mass-spectrometric method. Standartinform, Moscow (in Russ.)
PND F 13.2: 3.64—08 (2014) Methods of measuring the mass concentration of polychlorinated dibenzo-n-dioxins and dibenzofurans in the atmospheric air of the working area using chromatography and mass spectrometry. Moscow (in Russ.)
Method 1613 Rev. B (1994) Tetra-through octa-chlorinated dioxins and furans by isotope dilution HRGC/HRMS, U.S. Environmental protection agency office of water engineering and analysis division, Washington, p 89
ISO 18073:2004 (2013) Water quality—determination of tetra- to octa-chlorinated dioxins and furans—method using isotope dilution HRGC/HRMS. ISO
EN 1948-2 (2006) Stationary source emissions—determination of the mass concentration of PCDDs/PCDFs and dioxin-like PCBs—part 2: extraction and clean-up of PCDDs/PCDFs
EN 1948-3 (2006) Stationary source emissions—determination of the mass concentration of PCDDs/PCDFs and dioxin-like PCBs—part 3: identification and quantification of PCDDs/PCDFs
JIS K 0311-1999 (1999) Method for determination of tetra-through octa-chlorodibenzo-p-dioxins, tetra-through octa-chlorodibenzofurans and coplanar polychlorobiphenyls in stationary source emissions, Japanese Standards Association
Mutual recognition of national measurement standards and calibration and measurement certificates issued by national metrological institutes. CIPM MRA Agreement of 14.10.1999 (1999). Available via ROSSTANDART Federal Information Foundation for ensuring the uniformity of measurements. https://fgis.gost.ru/fundmetrology/registry/7. Accessed 20 Sept 2018 (in Russ.)
RMG 55-2003 GSI (2004) Standard samples of the composition of pure organic substances. Methods of testing. Main principles. Izdatel’stvo standartov, Moscow (in Russ.)
Duewer DL, Parris RM, White E, May WE, Elbaum H (2004) An approach to the metrologically sound traceable assessment of the chemical purity of organic reference materials. Special Publication NIST SP, 1012
Certified Reference Materials catalogue (2018) Joint Research Centre—Institute for Reference Materials and Measurements (JRC-IRMM). https://ec.europa.eu/jrc/en/reference-materials/catalogue. Accessed 20 Sept 2018
Approved types of reference materials RF (2018) ROSSTANDART Federal Information Foundation for ensuring the uniformity of measurements, Moscow. https://fgis.gost.ru/fundmetrology/registry/19. Accessed 20 Sept 2018
Wellington laboratories current catalogue inc 2016–2018 (2018) Wellington laboratories, Canada. https://well-labs.com/products/catalogue. Accessed 20 Sept 2018
Dioxin and furan method standards, standard mixtures, and reference materials (2018) Cambridge Isotope Laboratories. http://shop.isotope.com/category.aspx?id=10032753. Accessed 20 Sept 2018
Standard reference materials (2018) National Institute of Standards and Technology. https://www.nist.gov/srm
MUK-99 (1999) Guidelines for the identification and isomer-specific determination of polychlorinated dibenzo-p-dioxins and dibenzofurans in meat, poultry, fish, products and by-products from them, as well as in other fat-containing products and feed by chromatography mass spectrometry. Moscow (in Russ.)
De Bièvre P (1993) Isotope dilution mass spectrometry as a primary method of analysis. Anal. Proc. https://doi.org/10.1039/ap9933000328
Milton MJT, Quinn TJ (2001) Metrologia 38:289–296
ILAC-G12:2000 Guidelines for the Requirements for the competence of reference material producers
Kaarls R (2018) The consultative committee for metrology in chemistry and biology—CCQM. J Chem Metrol 12(1):1–16. https://doi.org/10.25135/jcm.11.17.12.060
GOST ISO Guide 35—2015 (2016) Reference materials—general and statistical principles of certification. Standartinform, Moscow (in Russ.)
RMG 93–2015 (2016) GSI Evaluation of the metrological characteristics of certified reference materials. Standartinform, Moscow (in Russ.)
Budko AG, Mikheeva AYu, Krylov AI (2017) On the accuracy and reliability of the results of measurement of polychlorinated dibenzo-(p)-dioxins and dibenzofurans. The results of interlaboratory comparisons. In: Materials of the III All-Russian Conference “analytical chromatography and capillary electrophoresis”. Kuban State University, Krasnodar, 21–27 May 2017
Acknowledgements
The authors express their sincere gratitude to the staff of the Scientific Production Association “Typhoon”, Scientific-Technical Centre of Radiation and Chemical Safety and Hygiene of the Federal Medical Biological Agency of Russia (STC RCSH), A. N. Severtsov Institute of Ecology and Evolution, Kuban State Agrarian University and Federal Office of Consumer Protection and Food Safety (BVL), Germany, for their participation in interlaboratory comparisons.
Author Contribution Statement
Budko A. G.: Preparation of the reference material, collection and analysis of experimental data, literature review, preparation of the manuscript draft;
Mikheeva A. Y.: Literature review, revision of the manuscript;
Krylov A. I.: Critical analysis and revision of the manuscript.
Author information
Authors and Affiliations
Corresponding author
Editor information
Editors and Affiliations
Rights and permissions
Copyright information
© 2020 Springer Nature Switzerland AG
About this paper
Cite this paper
Budko, A.G., Mikheeva, A.Y., Krylov, A.I. (2020). Metrological Assurance of Dioxin Measurements. A Certified Reference Material for Measuring the Dioxin Mass Fraction in Animal Fat. In: Medvedevskikh, S., Kremleva, O., Vasil’eva, I., Sobina, E. (eds) Reference Materials in Measurement and Technology. RMMT 2018. Springer, Cham. https://doi.org/10.1007/978-3-030-32534-3_2
Download citation
DOI: https://doi.org/10.1007/978-3-030-32534-3_2
Published:
Publisher Name: Springer, Cham
Print ISBN: 978-3-030-32533-6
Online ISBN: 978-3-030-32534-3
eBook Packages: Chemistry and Materials ScienceChemistry and Material Science (R0)