Abstract
The article provides information on the development of a new type of reference material (RM) of six priority phthalates (dimethyl phthalate, diethyl phthalate, di-n-butyl phthalate, benzyl butyl phthalate, di-2-ethyl hexyl phthalate, and di-n-octyl phthalate) in methanol solution, provided with metrological traceability to the GET 208–2019 (GET 208) national primary standard. The procedure for RM preparation and certification, including the homogeneity and stability assessment, is demonstrated. Pure organic substances (phthalates) characterised by the GET 208 primary standard were used as the starting material for the RM preparation using gravimetric and volumetric-gravimetric methods. The RM stability was assessed by an isochronous study. The mass fraction and mass concentration of individual phthalates in solution are the certified characteristics of the RM. The contributions from the purity of RM starting materials, preparation procedures, its heterogeneity and long-term instability were taken into account when calculating the uncertainty budget for the RM certified characteristics. The relative expanded uncertainty of certified values does not exceed 2%. As a result, the GSO (CRM) 11,366–2019 (6Ftlt-VNIIM) certified reference material of orthophthalic acid esters (phthalates) in methanol solution was developed and approved. The practical significance of using the GSO (CRM) 11,366–2019 consists in ensuring the metrological traceability of RMs to the corresponding SI units reproduced via the GET 208 national primary standard. The developed CRM can be used for different measuring tasks and metrological works.
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Notes
- 1.
GET 208-2019 National primary standard of the units of mass (molar) fraction and mass (molar) concentration of organic components in liquid and solid substances and materials based on liquid and gas chromatography–mass spectrometry with isotope dilution and gravimetry.). In: Federal Informational Fund on Maintaining the Unity of Measurements. https://fgis.gost.ru/fundmetrology/registry/12/items/1382717.
- 2.
NIST Mass Spectral Library 2014.
Abbreviations
- CERI:
-
Chemicals Evaluation and Research Institute, Japan
- CIL:
-
Cambridge Isotope Laboratories, Inc., USA
- CRM:
-
Certified reference material
- NIM:
-
National Institute of Metrology, China
- NIST:
-
National Institute of Standards and Technology, USA
- NMIJ:
-
National Metrology Institute of Japan
- RM:
-
Reference material
- BBP:
-
Benzyl butyl phthalate
- HPLC–UV:
-
High-performance liquid chromatography-ultraviolet detection
- GSO:
-
Formal name of certified reference material in Russia
- GC–MS:
-
Gas chromatography-mass spectrometry
- DBP:
-
Di-n-butyl phthalate
- DMP:
-
Dimethyl phthalate
- DOP:
-
Di-n-octyl phthalate
- DEHP:
-
Di-2-ethylhexyl phthalate
- DEP:
-
Diethyl phthalate
- VOC:
-
Volatile organic compound
- MB:
-
Mass balance
- MI:
-
Methodological instructions
- NC:
-
Non-volatile compounds
- MC:
-
Major component
- PVC:
-
Polyvinyl chloride
- PRPS:
-
Primary reference pure substance
- RSC:
-
Related structural compound
- RM:
-
Reference material
- CRM:
-
Certified reference material
- TR CU:
-
Technical regulations of the Customs Union
- POS:
-
Pure organic substance
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Acknowledgements
All measurements were carried out using the equipment of Mendeleyev Institute for Metrology (VNIIM).
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A. I. Krylov: research supervision, concept and methodology development.
A. Yu. Mikheeva: analysis of literature data, design of experimental studies, critical analysis of experimental data, revision of the manuscript text.
A. G. Budko: collection of literature data, acquisition and analysis of experimental data, production of CRM, preparation of documents for CRM development and testing, manuscript draft preparation.
I. Yu. Tkachenko: collection of literature data, design of experimental studies, critical analysis of experimental data, revision of the manuscript text.
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The article was prepared on the basis of a report presented at the IV International Scientific Conference “Reference Materials in Measurement and Technology” (St. Petersburg, December 1–3, 2020). 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” 2021;17(3):5–19. https://doi.org/10.20915/2687-0886-2021-17-3-5-19.
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Krylov, A.I., Mikheeva, A.Y., Budko, A.G., Tkachenko, I.Y. (2022). Measurement Assurance of Phtalate Content: A Reference Material of Six Priority Phthalates in Methanol Solution. In: Medvedevskikh, S.V., Sobina, E.P., Kremleva, O.N., Okrepilov, M.V. (eds) Reference Materials in Measurement and Technology . RMMT 2020. Springer, Cham. https://doi.org/10.1007/978-3-031-06285-8_7
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