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Starch granules, when subjected to heat treatment in the presence of water or other solvents, undergo a physicochemical transformation, famous as gelatinization. Probing the physicochemical changes will contribute to better understanding of gelatinization processes. This phenomenon induces several changes in the starch granules, such as swelling, amylose exudation, loss of order, improved solubility and digestibility, granule disruption, and higher viscosity. Many different measurement techniques have been reported for investigation of the starch gelatinization process. Amongst all, DSC seems to be the most applicable technique, by which, the heat-flow changes associated with first- and second-order transitions of polymeric materials can be studied over a wide moisture and temperature range.