We report the preparation of metal nanoparticles in various formulations inside p(2-acrylamido-2-methyl-1-propansulfonic acid; p(AMPS)) hydrogels and their utilization as a catalyst in hydrolysis of NaBH(4). The swollen, flexible p(AMPS) network was used for metal ion loading and reduction in situ for the preparation of Co:Ni nanoparticles as bimetallic clusters in various formulation, and Co and Ni bimetallic catalysts as Co + Co, Co + Ni, Ni + Co and Ni + Ni. In addition to utilization of hydrogels as support materials, the p(AMPS)-metal nanoparticle system was used as catalyst to generate hydrogen in the hydrolysis of NaBH(4) with very high yield. Various parameters for the hydrolysis reaction were determined and the activation parameters were calculated. For the first time, inclusion of ferrite magnetic particles to control hydrogen generation on demand by using an externally applied magnetic field to remove the hydrogel-catalyst system from the hydrolysis medium is reported. Copyright (C) 2011, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.