Generate QR code
Open Access
Subscription Access
Reference method for measuring the content of phthalates in polymer matrices: analytical and metrological approaches
https://doi.org/10.32446/0368-1025it.2022-10-64-72
Abstract
The article presents information on the development of a reference method of measurements (RMM) the mass fraction of ethers of orto-phthalic acid (dimethyl phthalate, diethyl phthalate, di(n-butyl)phthalate, benzylbutyl phthalate, di(2-ethylhexyl)phthalate and di(n-octyl)phthalate) in polymer matrices based on polyvinyl chloride by gas chromatography/mass spectrometry with isotopic dilution. The research materials of each stage of the measurement procedure and the parameters of their optimization in terms of improving the accuracy of the measurement results of the RMM are presented. The sources of uncertainty are studied and the contributions of all components to the total standard uncertainty of the RMM measurement results are minimized. Metrological characteristics of RMM have been established: the measurement range is from 10 mg/kg to 5000 mg/kg, the standard deviation (SD) under repeatability conditions is 2 %, the SD under intermediate precision conditions is 3 %, the relative extended uncertainty is from 6 to 8 %. The results of the key international comparisons CCQM-K133 “Phthalate esters in Polyvinyl Chloride (PVC)” are presented as an objective confirmation of compliance with the RMМ.
About the Authors
A. I. Krylov
D. I. Mendeleyev Institute for Metrology
Russian Federation
Russian Federation
Anatoliy I. Krylov
St. Petersburg
A. G. Budko
D. I. Mendeleyev Institute for Metrology
Russian Federation
Russian Federation
Aleksandra G. Budko
St. Petersburg
A. Y. Mikheeva
D. I. Mendeleyev Institute for Metrology
Russian Federation
Russian Federation
Alena Y. Mikheeva
St. Petersburg
I. Y. Tkachenko
D. I. Mendeleyev Institute for Metrology
Russian Federation
Russian Federation
Irina Y. Tkachenko
St. Petersburg
G R. Nezhikhovskiy
D. I. Mendeleyev Institute for Metrology
Russian Federation
Russian Federation
Gennady R. Nezhikhovskiy
St. Petersburg
References
1. EPA M ethod 606 – Phthalate ester, U.S. Environmental Protection Agency, 1984, 20 p.
2. Canad ian Environmental Protection Act Bis(2-ethylhexyl) phthalate. Priority substances list. Assessment Report, 1994. 29 p.
3. Europ ean Union Scientifi c Committee on Toxicology, Ecotoxicology and the Environment European Commission Decision 1999/815/EC, Offi cial Journal of the European Communities, 1999, L315, vol. 42, рр. 46–49.
4. Майстренко В. Н., Клюев Н. А. Эколого-аналитический мониторинг стойких органических загрязнителей. М.: БИНОМ. Лаборатория знаний, 2004. 323 с. [Maistrenko V. N., Klyuev N. A., Ecological and analytical monitoring of persistent organic pollutants, Moskow, BINOM. Laboratoriya znaniy Publ., 2004, 323 p. (In Russ.)].
5. RECOM MENDATIONS Commission Recommendation (EU) 2019/794 of 15 May 2019 on a coordinated control plan with a view to establishing the prevalence of certain substances migrating from materials and articles intended to come into contact with food, Offi cial Journal of the European Union, 2019, L129/37, vol. 62, рр. 1–89.
6. Ghada Zaki, Tamer Shoeib, Science of the Total Environment, 2018, vol. 618, рр. 142–150. https://doi.org/10.1016/j.scitotenv.2017.10.337
7. Qion g Luo, ZeHua Liu, Hua Yin, Zhi Dang, Neng-wu Zhu, Zhang Lin, Yu Liu, Water Research, 2018, vol. 147. https ://doi.org/10.1016/j.watres.2018.10.002
8. Маркова О. Л., Ганичев П. А., Еремин Г. Б., Зарицкая Е. В. Миграция фталатов из упаковочных материалов для бутилированной воды. Pезультаты международных исследований // Здоровье – основа человеческого потенциала: проблемы и пути их решения. 2020. Т. 15 . № 1. С. 416–427 [Markova O. L., Ganichev P. A., Yeremin G. B., Zaritskaya E. V., Phthalate migration from packing materials for bottled water. Findings of international studies, Health is the basis of human potential: problems and ways to solve them, 2020, vol. 15, no 1, pp. 416–427].
9. Бродский Е. С., Шелепчиков А. А., Агапкина Г. И. и др. Сложные эфиры фталевой кислоты в почвах Москвы // Вестник Московского Университета. Сер. 17. Почвоведение. 201 9. № 2. С. 44–48 [Brodskiy E. S., Shelepchikov A. A., Agapkina G. I., Tikhonova M. O., Paramonova T. A., Lipatov D. N., Content of phthalates esters in soils of Moskow-city, Bulletin of the Moscow University, Soil science, 2019, no. 2, pp. 44–48. (In Russ.)].
10. Горшков А. Г., Бабенко Т. А., Кустова О. В. и др. Приоритетные фталаты в пелагиали и прибрежной зоне оз. Байкал // Химия в интересах устойчивого развития. 2017. № 4. С. 375–383. https://doi.org/10.15372/KhUR20170403 [Gorshkov A. G., Babenko T.A., Kustova O.V., Izosimova O.N., Shishlyannikov C.M., Chemistry for Sustainable Development, 2017, no. 4, pp. 351–359. https://doi.org/10.15372/CSD20170403].
11. De Bi èvre P., Analytical Proceedings, 1993, no. 30, рр. 328–333. https://doi.org/10.1039/AP9933000328
12. Milto n M. J. T., Quinn T. J., Metrologia, 2001, vol. 38, no. 4, 289. https://doi.org/10.1088/0026-1394/38/4/1
13. Крылов А. И., Михеева А. Ю., Будко А. Г. и др. Метрологическое обеспечение измерений содержания фталатов: стандартный образец состава раствора шести приоритетных фталатов в метаноле // Эталоны. Стандартные образцы. 2021. № 17(3). С. 5–19. https://doi.org/10.20915/2687-0886-2021-17-3-5-19 [Krylov A. I., Mikheeva A. Y., Budko A. G., Tkachenko I. Yu., Metrological support of phthalate content measurements: reference material for the composition of a solution of six priority phthalates in methanol, Measurement Standards. Reference Materials, 2021, vol. 17, no. 3, pp. 5–19. (In Russ.)].
14. Fankh auser-Noti A., Grob K., Anal. Chem. Acta., 2007, vol. 582, no. 2, рр. 353–360. https://doi.org/10.1016/j.aca.2006.09.012
15. БЭС – Большой энциклопедический словарь. Химия. М.: Научное издательство «Большая Российская Энциклопедия», 2000. 790 с. [BES – Bol’shoj enciklopedicheskij slovar’. Himiya [A large encyclopedic dictionary. Chemistry], Moskow, Scientifi c publishing house “Bol’shaya Rossijskaya Enciklopediya”, 2000, 790 p. (In Russ.)].
16. Руководство ЕВРАХИМ / СИТАК. Количественное описание неопределённости в аналитических измерениях: Пер. с англ. Р. Л. Кадиса, Г. Р. Нежиховского, В. Б. Симина под общ. ред. Л. А. Конопелько. 3-е изд. СПб: НПО «Профессионал», 2016. 149 с. [EURACHEM / CITAC Guide CG 4. Quantifying Uncertainty in Analytical Measurement, Third Edition, 2012].
Review
For citations:
Krylov A.I., Budko A.G., Mikheeva A.Y., Tkachenko I.Y., Nezhikhovskiy G.R. Reference method for measuring the content of phthalates in polymer matrices: analytical and metrological approaches. Izmeritel`naya Tekhnika. 2022;(10):64-72. (In Russ.) https://doi.org/10.32446/0368-1025it.2022-10-64-72
Views:
183
Email this article 