Abstract
The requirements for thermal analysis instruments are increasing in terms of extending the measurement ranges and improving their accuracy with scientific and technological progress in the field of metrological supervision, chemical, and pharmaceutical industries. The study of determining the melting point of organic substances is of particular relevance for the metrological support of the applied thermal analysis instruments and traceability to the base physical units. The purpose of the research was to test the possibility of using organic substances based on sodium acetate and sodium methanesulfonate as phase transition temperature standards for candidate materials to certified reference materials (CRMs) for the phase transition temperature traceable to the SI unit “temperature.” The procedure for measuring the phase transition temperature (melting point) was performed by differential scanning calorimetry using the thermal analyzer STA 449 F5 JUPITER from the State Primary Standard GET 173-2017. The determination of the CRM certified value was carried out in accordance with GOST ISO Guide 35-2015; the contributions to the uncertainty due to heterogeneity of the starting materials were evaluated; the short- and long-term stabilities of the materials were studied.
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Notes
- 1.
Federal Information Fund for Ensuring the Uniformity of Measurements. Available via FIF EUM. https://fgis.gost.ru/fundmetrology/registry/19. Accessed 10 October 2022 (In Russ.).
- 2.
FIF 59055-14 Instruments for measuring the melting point. Available via FIF EUM. https://fgis.gost.ru/fundmetrology/registry/4/items/372174. Accessed 10 October 2022 (In Russ.).
FIF 67807-17 Instruments for measuring the melting point. Available via FIF EUM. https://fgis.gost.ru/fundmetrology/registry/4/items/381782. Accessed 10 October 2022 (In Russ.).
- 3.
GET 173-2017 State primary standard of units of mass fraction, mass (molar) concentration of water in solid and liquid substances and materials: UNIIM—Affiliated Branch of the D. I. Mendeleyev Institute for Metrology. Available via FIF EUM. https://fgis.gost.ru/fundmetrology/registry/12/items/397857. Accessed 10 October 2022 (In Russ.).
- 4.
GSO 11070-2018 Reference materials benzophenone melting point type-approved (CO C13H10O). Available via FIF EUM. https://fgis.gost.ru/fundmetrology/registry/19/items/593689. Accessed 10 October 2022 (In Russ.).
- 5.
GSO 11071-2018 Reference materials of the approved type of melting point of benzoic acid (CO C7H6O2). Available via FIF EUM. https://fgis.gost.ru/fundmetrology/registry/19/items/394949. Accessed 10 October 2022 (In Russ.).
- 6.
M.241.0036/RA.RU.311866/2022 Method for measuring the phase transition temperatures of sodium methanesulfonate (CH3NaO3S) and anhydrous sodium acetate (C2H3O2Na) by differential scanning calorimetry: UNIIM—Affiliated Branch of the D. I. Mendeleyev Institute for Metrology. Available via FIF EUM. https://fgis.gost.ru/fundmetrology/registry/16/items/1399257. Accessed 10 October 2022 (In Russ.).
- 7.
FIF 41280-14 Melting point analyzers. Available via FIF EUM. https://fgis.gost.ru/fundmetrology/registry/4/items/351558. Accessed 10 October 2022 (In Russ.).
FIF 85498-22 Melting point analyzers. Available via FIF EUM. https://fgis.gost.ru/fundmetrology/registry/4/items/1399531. Accessed 10 October 2022 (In Russ.).
- 8.
GET 34-2020 State primary standard of temperature unit in the range from 0 to 3200 °C: D. I. Mendeleyev Institute for Metrology. Available via FIF EUM. https://fgis.gost.ru/fundmetrology/registry/12/items/1385580. Accessed 10 October 2022 (In Russ.).
- 9.
GSO 11928-2022/GSO 11929-2022 reference materials of phase transition temperatures (set of SS TPKR). Available via FIF EUM. https://fgis.gost.ru/fundmetrology/registry/19/items/1399806. Accessed 10 October 2022 (In Russ.).
Abbreviations
- TA:
-
Thermal analysis
- DSC:
-
Differential scanning calorimetry
- FIF EUM:
-
Federal information fund for ensuring the uniformity of measurements
- CRM:
-
Certified reference material
- RTD:
-
Resistance temperature detector
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Acknowledgements
The research did not receive financial support in the form of a grant from any organization in the public, commercial or non-profit sectors. All measurements were performed using the equipment of the D. I. Mendeleyev Institute for Metrology.
Author Contributions
Shipitsyn A. P.—development of a methodology/procedure, implementation of a formal analysis, writing a draft version of the article, conducting research work; Nepomiluev A. M.—development of the research concept, conducting research work; Tyurnina A. E.—manuscript revision and editing.
Conflict of Interest
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). 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(1):17–27 (In Russ.). https://doi.org/10.20915/2077-1177-2023-19-1-17-27.
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Shipitsyn, A.P., Nepomiluev, A.M., Tyurnina, A.E. (2024). Certified Reference Materials for the Phase Transition Temperature of Organic Substances Based on Anhydrous Sodium Acetate and Sodium Methansulfonate. 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_23
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