In this study, hydrogels were synthesized from 2-acrylamido-2-methyl-1-propansulfonic acid (AMPS) via a photo polymerization technique. Approximately 100 nm Ni metal nanoparticles were generated in situ inside these p(AMPS) hydrogel networks and used as a catalyst in hydrogen production by hydrolysis of sodium boron hydride in a basic medium. The effects of several parameters on the hydrolysis reaction such as the amount of catalyst, the initial concentration of NaBH4, and the temperature were investigated. The activation energy, activation enthalpy and activation of entropy for the reaction were calculated as 42.28 kJ mol(-1), 39.59 kJ mol(-1) and -171.67 J mol(-1) K-1, respectively. (C) 2010 Professor T. Nejat Veziroglu. Published by Elsevier Ltd. All rights reserved.