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Proton, thermal and mechanical relaxation characteristics of a complex biomaterial (de-fatted date-pits) as a function of temperature

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Abstract

Thermal (differential scanning calorimetry, DSC), proton (low-frequency nuclear magnetic resonance, LF-NMR), and mechanical (differential mechanical thermal analysis, DMTA) relaxations were measured for defatted date-pits as a function of temperature. DSC showed three types of relaxations, lower one structural relaxation (i.e. − 5 °C), followed by a glass transition (i.e. 136 °C) and solids melting–decomposition (i.e. 171 °C). LF-NMR showed three pools of protons, rigid, semi-rigid and mobile. Rigid protons showed two types of relaxations, first one low temperature increase (− 80 to − 40 °C), plateau region (− 60 to − 40 °C) and a positive peak at 120 °C, and semi-rigid showed maximum peak at − 5 °C and minimum peak at 150 °C. Mobile protons showed low relaxation (− 80 to − 40 °C), a maximum peak at 70 °C and a minimum peak at 130 °C. The maximum peak (i.e. − 5 °C) of semi-rigid protons was similar to the DSC structural change, while the maximum peak of rigid protons (120 °C) was similar to DSC glass transition (i.e. 136 °C). The minimum peak of the semi-rigid protons (i.e. 150 °C) was similar to the solids melting–decomposition (171 °C). DMTA showed five regions of mechanical relaxations, glassy region (i.e. onset at 32 °C), glass transition (i.e. 32–85 or 87 °C), first reaction region with a plateau or peak (85–140 °C), second reaction region (87–174 °C), and softening or decomposition region (223 or 242 °C). Mechanical glass showed completely different relaxation as compared to the protons and thermal relaxations. This study showed that LF-NMR, DSC and DMTA could be used to explore the relaxations of a material at nano-, micro- and macro-levels.

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Acknowledgements

The authors would like to express thanks to the Sultan Qaboos University for its support towards this research project. This work was funded by the His Majesty Trust Funds (SR/AGR/FOOD/19/01).

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Authors and Affiliations

  1. Department of Food Science and Nutrition, College of Agricultural and Marine Sciences, Sultan Qaboos University, P. O. Box 34, 123, Muscat, Oman

    Maha Al-Khalili, Nasser Al-Habsi, Mohamed Al-Khusaibi & Mohammad Shafiur Rahman

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  1. Maha Al-Khalili
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  2. Nasser Al-Habsi
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Correspondence to Nasser Al-Habsi.

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Al-Khalili, M., Al-Habsi, N., Al-Khusaibi, M. et al. Proton, thermal and mechanical relaxation characteristics of a complex biomaterial (de-fatted date-pits) as a function of temperature. J Therm Anal Calorim 148, 3525–3534 (2023). https://doi.org/10.1007/s10973-023-11943-6

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