In situ Co, Cu and Ni nanoparticles were synthesized by chemical reduction of the absorbed Co (II), Cu (II) and Ni (II) ions inside hydrogel networks prepared from 2-acryl-amido-2-methyl-1-propansulfonic acid (AMPS) and were used as a catalyst system in the generation of hydrogen in hydrolysis of ammonia borane (AB). Several parameters affecting the hydrolysis reaction such as the type of the metal, the amount of catalyst, the initial concentration of AB, and temperature, were investigated. The activation energy values in the hydrolysis reaction of AB solution in the presence p(AMPS)-Co, p(AMPS)-Cu and p(AMPS)-Ni catalyst systems were calculated as E(a) = 47.7 kJ mol(-1), 48.8 kJ mol(-1) and 52.8 kJ mol(-1), respectively. Thus, the catalytic activity of the metal nanoparticles prepared inside the same hydrogel matrix was found to be Ni < Cu < Co. Copyright (C) 2011, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.