The alkaline hydrolysis of polyacrylonitrile staple fibers was investigated for evaluation as superabsorbent materials. Studies were performed to analyze the hydrolysis of fibers and the quantification of the developed functional groups, such as carboxyl and amide groups as well as changes in the nitrile content by means of MicroATR. Dyeing of the samples with methylene blue was carried out to monitor the carboxyl groups formed during the hydrolysis. A gradual decrease in the nitrile groups and built up of the carboxyl and the amide groups was observed during the hydrolysis. Microscopic investigation carried out to investigate the surface structure of hydrolyzed fibers. Hydrolysis led to surface nonhomogeneity and erosion that was dependent on the hydrolysis conditions. The fibers showed good water retention behavior, making them superabsorbent materials. The dyeing showed more intense coloration in the surface region of the modified fibers. (C) 2004 Wiley Periodicals, Inc.