The interest in replacing synthetic polymers by biodegradable materials from renewable resources is steadily increasing. In this work, cassava starch grafted with different content of polystyrene (PS) was synthesized via free-radical polymerization using suspension polymerization technique. Thermal data of pure starch and the grafted starch with different content of PS were collected by simultaneous thermogravimetric (TG)–differential scanning calorimetry (DSC) setup in open alumina pans. Separately, typical DSC measurements were conducted in standard aluminum pans with lid. The data obtained by different methods are correlated and discussed. Morphology of cryogenic fracture surface of starch sample was studied by scanning electron microscopy. In order to obtain more reliable data about the processes taking place during the thermal treatment, the changes of surface morphology of starch treated at different temperatures are observed.
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