Chitosan/carboxymethyl cashew gum polyelectrolyte complexes were synthesized using different proportions of chitosan (CH) and carboxymethyl cashew gum (CMCG). The optimum CH:CMCG ratio was 25:75, which produced highest product yield. Polyelectrolyte (PEC) samples were characterized by thermogravimetric analysis and FT-I R spectroscopy. Parameters such as initial and maximal degradation temperatures and activation energy were determined. Activation energies follows the order CMCG > CH > PECs samples. Infrared analysis from residual products after heating at 280 degrees C in different times indicated that cleavage of the glycosidic bond and formation of unsaturated products occurred. (c) 2005 Elsevier Ltd. All rights reserved.