In this work, the chitosan flake was converted to carboxymethyl chitosan (CMCS) by
carboxymethylation process using monochloroacetic acid in alkaline condition. The structure of carboxymethyl chitosan was confirmed by NMR, FT-IR, XRD, TGA and SEM techniques. The average molecular weight of carboxymethyl chitosan was obtained by viscometry method. The carboxymethylation reaction of chitosan was optimized for the reaction time, reaction temperature, amount of chitosan, amount of monochloroacetic acid. Response surface methodology (RSM) was used to analyze degree of substitution, degree of acetylation and yield with respect to reaction conditions. At the optimization reaction condition the degree of substitution, degree of acetylation (%) and yield (%) values are 0.56, 33.99 and 78.2, respectively.