Abstract
1H and 13C NMR spectroscopy was used for the study of corn starch plasticized with urea and/or glycerol. The information on the interactions between plasticizers and starch macromolecules as well as the arrangement of starch macromolecules depending on the storage time (from 1 day to 52 weeks), were obtained from the broad-line and magic-angle spinning 1H NMR spectra measured at 22 °C and within the range from 30 to 140 °C and the cross-polarization magic-angle spinning (CP MAS) 13C NMR spectra measured at 30 °C. The 1H chemical shifts for the groups of the plasticizer molecules enabled characterization of the interactions between urea and glycerol molecules in starch plasticized with a mixture of urea and glycerol. With increasing temperature, the signal related to water molecules gradually vanished due to water evaporation, and resolved 1H peaks associated with starch macromolecules were detected above 100 °C. The free water amount in the thermoplastic starch samples was also estimated using MAS 1H NMR spectra. Formation of double helices due to sample ageing was observed through the CP MAS 13C NMR spectra.
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