In this work, methyl acrylate grafted cellulose fibers were hydrolyzed in an aqueous NaOH solution to obtain a superabsorbent hydrogel. The effect of process variables, such as the hydrolysis reaction time, temperature, and NaOH concentration, during alkaline hydrolysis were carefully determined and optimized. The degree of hydrolysis was estimated on the basis of the determination of the carboxylate group contents. The material loss during hydrolysis followed a first-order reaction mechanism. The differences in the behavior of the grafted fibers during hydrolysis could be explained by their structural differences. (C) 2007 Wiley Periodicals, Inc.