Response Surface Methodology for the Optimization and Characterization of Cassava Starch‐graft‐Poly(acrylamide)

Abstract

AbstractResponse surface methodology (RSM) was employed for the synthesis of cassava starch‐graft‐poly(acrylamide) using ceric ammonium nitrate as free radical initiator. Concentration of acrylamide, concentration of ceric ammonium nitrate, reaction temperature and duration of reaction were optimized using a 4‐factor 3‐level Box‐Behnken design. The dependent variables were percentage grafting (%G) and grafting efficiency (GE). Second order polynomial relationships were obtained for %G and GE, which explained the main, quadratic and interaction effects of factors. The highest%G and GE obtained were 174.8% and 90.7%, respectively. The optimum values of parameters predicted through RSM were 20 g acrylamide/10 g dry starch, 3.3 g/L ceric ammonium nitrate, 180 min reaction duration and 45ºC temperature with a %G of 190.0. For GE, the predicted levels of factors for the optimum value of 90.8% were 17.5 g acrylamide/10 g dry starch, 4.1 g/L ceric ammonium nitrate, 180 min reaction duration and 55ºC temperature. The graft reaction was confirmed by FTIR analysis, where the absorption bands corresponding to the C=O stretching and N‐H bending of the –CONH2 group were observed. Scanning electron microscopic studies on grafted starches revealed that the granular structure of the starch was affected by the reaction. X‐ray diffraction analysis showed that the crystallinity of starch was decreased as a result of grafting and the reduction was higher for the grafted starches with higher percentage grafting.