Free amino groups in @-chitin from squid pen were acetylated to obtain N-acetylated Pchitin. After careful control of degree of acetylation, thermal and mechanical properties of P-chitin and N-acetylated @-chitin were compared. The structural differences of P-chitin and N-acetylated 6-chitin were characterized by Fourier transform infrared (FTIR) and wide-angle x-ray diffraction (WAXD) analysis. The results indicated that the crystallinity of N-acetylated P-chitin was higher than that of @-chitin and N-acetylated @-chitin exhibited characteristics similar to a-chitin. Equilibrium water content (EWC) of P-chitin reached to about 50% and this hydrophilic nature was assumed to be caused by a relatively weak hydrogen bonding force of @-chitin with parallel main chains. On the other hand, EWC of N-atetylated @-chitin was 40% due to the introduction of ordered structure. 0-chitin and N-acetylated @-chitin have the tensile strength of 0.4 and 0.7 Mpa in the swollen state, respectively. Viscoelastic properties and thermal relaxation behaviors were investigated by dynamic mechanical thermal analysis (DMTA). DMTA spectra of these samples showed that a-transition peaks of @-chitin and N-acetylated @-chitin were observed a t 170 and 190°C, respectively. These relaxation peak maxima were assigned to be their glass transition temperature. In addition, a second relaxation peak of &chitin resulting from acetamide groups was found at 112OC and a broad relaxation peak of N-acetylated P-chitin at around 81-1OO0C. As a result of thermogravimetric analysis, 10% weight loss temperatures of 6chitin and N-acetylated @-chitin were 270 and 285OC, respectively. 0 1996 John Wiley & Sons, Inc.