Ni, Rh and Pd incorporated mesoporous MCM-41, MCM-48, HMS and SBA-15 samples were synthesized and were characterized using XRD, ICP/EDX and N(2) adsorption-desorption at 77.4 K. The hydrogen adsorption studies in the synthesized materials were performed at 77.4 K (up to 112 kPa) and 303 K (up to 4000 kPa). The hydrogen adsorption isotherms of pristine and transition metals incorporated mesoporous materials at 77.4 K were completely reversible reflecting physisorption of hydrogen in these materials. The hydrogen adsorption isotherms at 303 K were not reversible showing the chemisorption of hydrogen in these materials at 303 K. Hydrogen sorption studies showed that transition metal modification improved the hydrogen storage capacity of mesoporous materials at 303 K. The desorption of the adsorbed hydrogen by heating up to 500 K from the mesoporous materials were also carried out for studying the recovery of adsorbed hydrogen from transition metal incorporated mesoporous materials. (C) 2009 Professor T. Nejat Veziroglu. Published by Elsevier Ltd. All rights reserved.