Piassava (Attalea funifera) fibers subjected to several surface chemical treatments and as-received raw fibers were compared with respect to their thermal and tensile behaviors. The thermal degradation of the raw fibers was characterized by three main stages that corresponded to water release at low temperatures, decomposition of hemicellulose, and decomposition of alpha cellulose. Mercerization acted mainly on hemicellulose removal, and there was no change in the hydrophilic behavior of the fibers. The removal of hemicellulose split the fibers into microfibrils and favored the thermal decomposition of alpha cellulose. The same behavior was observed when the fibers were subjected to mercerization and acetylation. The fibers subjected to only acetylation showed thermal behavior similar to that of the raw fibers. With the acetylation treatment, a minor decrease in the hydrophilic character of the fibers was noted. Despite some differences in the thermal behavior, the tensile strengths of the raw and treated fibers were statistically equal. Complementary Fourier transform infrared and scanning electron microscopy analysis corroborated the thermogravimetric analysis/differential thermogravimetry results. (C) 2010 Wiley Periodicals, Inc. J Appl Polym Sci 120: 2508-2515, 2011