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Rapid and in-situ determination of epoxy equivalent weight of bisphenol-based epoxides by micro-Raman spectroscopy

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Abstract

The need for rapid, fast and nondestructive determination of the epoxy equivalent weight (EEW) of the resins was the underlying motivation to develop and propose an accurate and efficient method by means of micro-Raman spectroscopy. Three bands of interest that were assigned to the epoxide vibrations (around 640, 918 and 1250 cm−1), were marked. Their intensities were determined and used in the development of the one-band fitting model that was separately tested for several liquid and solid bisphenol A- and/or bisphenol F-based epoxy resins whose EEW span in a rather wide range from 150 to 900 g/Eq. In addition, the same Raman spectra were used to build a partial least-squares (PLS) regression model for the determination of EEW that overcome the problems related to the different aggregate states of the epoxy resin. The elimination of the occurring baseline shift, for both models, was surpassed by the normalization of the 1600–1610 cm−1 band that is not correlated to EEW and originates from the resin backbone chain vibrations. The EEW of each resin was also accurately determined by a standard titration method and the obtained results were used as reference values. This work represents the first attempt to highlight the micro-Raman spectroscopy as a promising analytical technique for quantitative estimation of the EEW of bisphenol-based epoxy resins. The proposed method could be possibly extended for the other epoxide materials, and further consistent with the process analytical technique (PAT) requirements.

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Authors and Affiliations

  1. Institute of Chemistry, Faculty of Natural Sciences and Mathematics, Ss. Cyril and Methodius University in Skopje, Arhimedova 5, 1000, Skopje, North Macedonia

    Petre Makreski

  2. Research Centre for Environment and Materials, Macedonian Academy of Sciences and Arts, Krste Misirkov 2, 1000, Skopje, North Macedonia

    Aleksandra Ivanoska-Dacikj & Gordana Bogoeva-Gaceva

  3. Faculty of Pharmacy, Ss. Cyril and Methodius University in Skopje, Majka Tereza 47, 1000, Skopje, North Macedonia

    Nikola Geskovski & Olga Gigopulu

  4. Faculty of Technology and Metallurgy, Ss. Cyril and Methodius University in Skopje, Rugjer Bošković 16, 1000, Skopje, North Macedonia

    Gordana Bogoeva-Gaceva

Authors
  1. Petre Makreski
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  2. Aleksandra Ivanoska-Dacikj
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  3. Nikola Geskovski
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  4. Olga Gigopulu
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  5. Gordana Bogoeva-Gaceva
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Contributions

Conceptualization: Petre Makreski, Gordana Bogoeva-Gaceva, Nikola Geskovski, Aleksandra Ivanoska-Dacikj; Methodology: Petre Makreski, Nikola Geskovski, Aleksandra Ivanoska-Dacikj, Gordana Bogoeva-Gaceva; Formal analysis and investigation: All authors; Writing—original draft preparation: Petre Makreski, Nikola Geskovski, Aleksandra Ivanoska Dacikj; Writing—review and editing: All authors; Resources: Gordana Bogoeva-Gaceva, Petre Makreski; Supervision: Petre Makreski, Gordana Bogoeva-Gaceva.

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Correspondence to Petre Makreski.

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Makreski, P., Ivanoska-Dacikj, A., Geskovski, N. et al. Rapid and in-situ determination of epoxy equivalent weight of bisphenol-based epoxides by micro-Raman spectroscopy. J Polym Res 30, 92 (2023). https://doi.org/10.1007/s10965-023-03471-6

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