The water-soluble solids comprised of the ionic complex between chitosan and acetic acid, chitosonium acetate, are converted into chitin by heating. The thermally-induced conversion of a water-soluble chitosonium acetate in film form into a water-insoluble chitin film was examined by thermal analysis (DMTA, TGA, DSC, and TMA) and by solid state C-13-NMR spectroscopy. Results indicate that tan delta-transitions occur at increasingly high temperatures, and over progressively wider temperature ranges, as the transformation progresses. Likewise, the storage modulus, log E’, increases as the chitosonium acetate film undergoes "cure" and converts to chitin. Cure kinetic parameters are obtained using the model proposed by Provder et al. modified for glass transition temperature (T-g). The results suggest the existence of two sequential first order reactions, an initial and a late cure reaction, having activation energies of approximately 15 and 21 kcal/mol, respectively.