The geothermal history of natural resins from different geographical locations was studied in terms of their age assessment and structure–properties relations. Thermal properties of resin samples were analyzed by thermogravimetry (TG) and differential scanning calorimetry (DSC), whereas infrared spectroscopy was used for analysis of the resins structure. Relative dependence between thermal parameters and degree of resin maturity was found. Glass transition process and thermal events during heating of raw materials were investigated by advanced stochastic-modulated DSC method, known as TOPEM®, that allowed to determine the “true” glass transition temperature in the first heating scan. It was observed that TG method is insufficient for the resin age assessment, although it was found that there is a certain correlation between the glass transition temperature, estimated by TOPEM® DSC, and resin age. The natural resins proved to be reactive and sensitive material under elevated temperatures up to 200 °C. Subsequent processes of evaporation, relaxation and curing without significant mass loss related to degradation were observed during heating of resin samples. The aging rate in natural resins has been assessed using the intensity of 1730 cm−1 and 1646 cm−1 band after deconvolution of IR spectra. It may be assumed that younger resins are characterized by relatively higher reactivity (higher number of C=C bonds) and lower oxidation level.
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This study was supported by the Research Grant No. 61.9012.1908.00.0 from AGH University of Science and Technology and the research Grant No. 61.9012.1908 from Polish Geological Institute-National Research Institute. Authors would also like to thank Dr. Daniel Fragiadakis, Naval Research Laboratory, USA, who develops and maintains the software Grafity (distributed free of charge at grafitylabs.com), which was used for our data analysis. Authors thanks Polymer Materials Laboratory from ŁUKASIEWICZ—Polish Center for Technology Development—for kind use of thermo-analytical equipment. Special thanks are directed to Anselm Krumbiegel for providing the resin samples that were collected by his father.
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Fig. S1. IR spectra of selected natural resins after normalization and deconvolution (spectral range of 1900–1500 cm−1 at room temperature): a RU/S/3 and DE/B/28, b PL/GD/1 with ID/SJ/7 (DOC 376 kb)
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Pagacz, J., Naglik, B., Stach, P. et al. Maturation process of natural resins recorded in their thermal properties. J Mater Sci 55, 4504–4523 (2020). https://doi.org/10.1007/s10853-019-04302-0