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Measurement of Carbon Isotope Ratio in Vanillin Using the CM-CRDS Method: Achieving an Expanded Uncertainty Below 0.1‰

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Reference Materials in Measurement and Technology (RMMT 2022)

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Abstract

Isotopic analysis is an effective method for quality control and detection of adulterated food products, with the elemental analyzer isotope ratio mass spectrometry (EA-IRMS) being the conventional approach, specified in relevant regulatory documents. Although measuring the carbon isotope ratio by combustion module cavity ring-down spectroscopy (CM-CRDS) has gained significant interest for isotope analysis of food products, its metrological characteristics remain understudied for analysis of the isotopic composition of vanillin. Therefore, this article focuses on the development of a measurement procedure of the carbon isotope ratio in vanillin in preparation for the international key comparison CCQM-K167 “Carbon Isotope Delta Measurements of Vanillin”. The experimental part of the research was carried out using the reference installation included in the State primary standard for units of molar fraction, mass fraction, and mass concentration of components in gases GET 154-2019. The expanded uncertainty (at k = 2) of this measurement method was < 0.09‰, which is comparable to the best measurements obtained by the EA-IRMS method. The achieved results validate the applicability of the CM-CRDS method for quality control and detection of adulterated vanillin.

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Notes

  1. 1.

    FR.1.31.2012.13424 Method for measuring the 13C/12C isotope ratio of ethanol in beer and beer drinks by isotope mass spectrometry. Available via FIF EUM. https://fgis.gost.ru/fundmetrology/registry/16/items/282517. Accessed 11 November 2022 (In Russ.).

    FR.1.31.2013.15529 The methodology establishes the procedure for determining the ratio of 18O/16O isotopes of exogenous and endogenous water in wines and musts. Available via FIF EUM. https://fgis.gost.ru/fundmetrology/registry/16/items/281364. Accessed 11 November 2022 (In Russ.).

    FR.1.31.2014.17273 Method for measuring the ratio of carbon isotopes 13C/12C in alcoholic beverages of grape origin by isotope mass spectrometry. Available via FIF EUM. https://fgis.gost.ru/fundmetrology/registry/16/items/280000. Accessed 11 November 2022 (In Russ.).

    FR.1.31.2016.24753 Method for measuring the oxygen isotope ratio, 18O/16O of exogenous and endogenous water in wines and musts by isotope mass spectrometry. Available via FIF EUM. https://fgis.gost.ru/fundmetrology/registry/16/items/298716. Accessed 11 November 2022 (In Russ.).

    FR.1.31.2016.24962 Method for measuring ethanol isotope ratios in cognacs and cognac distillates by isotope mass spectrometry. FR.1.31.2016.24962 Method for measuring ethanol isotope ratios in cognacs and cognac distillates by isotope mass spectrometry. Available via FIF EUM. https://fgis.gost.ru/fundmetrology/registry/16/items/298746. Accessed: 11 November 2022 (In Russ.).

    FR.1.31.2017.28360 Method for measuring the ratios of carbon, oxygen, hydrogen isotopes of ethanol to detect the presence of synthetic alcohol in alcoholic products, as well as in alcohol-containing food flavorings by isotope mass spectrometry. Available via FIF EUM. https://fgis.gost.ru/fundmetrology/registry/16/items/299163. Accessed 11 November 2022 (In Russ.).

    FR.1.31.2018.31997 Method for measuring the ratio of oxygen isotopes 18O/16O of the water component of ciders and poiret by isotope mass spectrometry. Available via FIF EUM. https://fgis.gost.ru/fundmetrology/registry/16/items/495958. Accessed 11 November 2022 (In Russ.).

  2. 2.

    GET 154-2019 State Primary Standard of Units of Mole Fraction, Mass Fraction and Mass Concentration of Components in Gas and Gas Condensate Environments: Custodian Institute VNIIM im. D. I. Mendeleev. Available via FIF EUM. https://fgis.gost.ru/fundmetrology/registry/12/items/1365155. Accessed 11 November 2022 (In Russ.).

  3. 3.

    104th meeting of the CIPM (Session I), 9 to 10 March 2015. Available via BIPM. https://www.bipm.org/en/committees/ci/cipm/104-_1-2015. Accessed 11 November 2022.

  4. 4.

    UME CRM 1312 Certificate of the Reference Material Honey (unadulterated). Available via. https://rm.ume.tubitak.gov.tr/sertifika/ume_crm_1312_certificate.pdf. Accessed 11 November 2022.

  5. 5.

    IAEA-CH-3 Cellulose. Available via. https://nucleus.iaea.org/sites/ReferenceMaterials/Pages/IAEA-CH-3.aspx. Accessed 11 November 2022.

  6. 6.

    IAEA-600 Caffeine. Available via: https://nucleus.iaea.org/sites/ReferenceMaterials/Pages/IAEA-600.aspx. Accessed 11 November 2022.

  7. 7.

    IAEA-CH-7 Polyethylene. Available via. https://nucleus.iaea.org/sites/ReferenceMaterials/Pages/IAEA-CH-7.aspx. Accessed 11 November 2022.

  8. 8.

    NIST RM 8539 NBS 22 oil (carbon and hydrogen isotopes in oil). Available via. https://www.sigmaaldrich.com/RU/en/product/sial/nistrm8539. Accessed 11 November 2022.

  9. 9.

    CMC Quick search. Available via CIPM MRA database (KCDB). https://www.bipm.org/kcdb/cmc/quick-search?includedFilters=&excludedFilters=&page=0&keywords=VNIIM+ isotope. Accessed 11 November 2022.

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Acknowledgements

All measurements were carried out using the equipment of the Research Department of State Standards in the Field of Physical and Chemical Measurements No. 242, D. I. Mendeleyev Institute for Metrology. The author expresses his gratitude to the workers and Anna V. Kolobova, Cand. Sci. (Eng.), Head of the Research Department No. 242.

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Authors and Affiliations

  1. D. I. Mendeleyev Institute for Metrology, Saint Petersburg, Russia

    Ian K. Chubchenko

Authors
  1. Ian K. Chubchenko
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Correspondence to Ian K. Chubchenko .

Editor information

Editors and Affiliations

  1. UNIIM—Affiliated Branch of the D. I. Mendeleyev Institute for Metrology, Yekaterinburg, Russia

    Egor P. Sobina

  2. UNIIM—Affiliated Branch of the D. I. Mendeleyev Institute for Metrology, Yekaterinburg, Russia

    Sergey V. Medvedevskikh

  3. UNIIM—Affiliated Branch of the D. I. Mendeleyev Institute for Metrology, Yekaterinburg, Russia

    Olga N. Kremleva

  4. All-Russian Scientific Research Institute for Optical and Physical Measurements, Moscow, Russia

    Ivan S. Filimonov

  5. All-Russian Scientific Research Institute for Metrological Service, Moscow, Russia

    Elena V. Kulyabina

  6. D. I. Mendeleyev Institute for Metrology, Saint Petersburg, Russia

    Anna V. Kolobova

  7. Saint Petersburg State University, PetroAnalytica LLC, Saint Petersburg, Russia

    Andrey V. Bulatov

  8. All-Russian Scientific Research Institute of Physicotechnical and Radio Engineering Measurements, Moscow, Russia

    Vladimir I. Dobrovolskiy

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Conflict of Interests

The article was prepared on the basis of a report presented at the V International Scientific Conference “Reference Materials in Measurement and Technology” (Yekaterinburg, September 13–16, 2022) as well as at the EGU General Assembly 2020 in online format (May 4–8, 2020) [29]. The article was admitted for publication after the abstract was revised, the article was formalized, and the review procedure was carried out.

The version in the Russian language is published in the journal “Measurement Standards. Reference Materials” 2023;19(3):129–144. (In Russ.). https://doi.org/10.20915/2077-1177-2023-19-3-129-144.

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Chubchenko, I.K. (2024). Measurement of Carbon Isotope Ratio in Vanillin Using the CM-CRDS Method: Achieving an Expanded Uncertainty Below 0.1‰. In: Sobina, E.P., et al. Reference Materials in Measurement and Technology . RMMT 2022. Springer, Cham. https://doi.org/10.1007/978-3-031-49200-6_10

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