Two groups of cobalt (Co) catalysts, supported on SBA-15 and MCM-41, respectively, were prepared by incipient wetness impregnation and tested for their Influence on the thermal decomposition of acetyl cellulose gamma-Al2O3 supported Co catalysts were investigated as a comparison A thermogravimetric analyser coupled with a mass spectrometer (TG-MS) was used to examine the influence of catalyst loading, support material and the presence of additional water vapour on H-2 production and selectivity. Normalization of the raw MS data enabled semi-quantitative analysis of the product gas distribution, which facilitated reliable comparison between different experimental conditions. Catalysts were characterized by physisorption, chemisorption. TGA, XRD, SEM and TEM. SBA-15 and MCM-41 supported catalysts significantly elevated the yield and selectivity of H-2, under dry Ar and with the injection of additional water vapour, when compared with the gamma-Al2O3 support 15 wt %Co/SBA-15 and 10 wt %Co/MCM-41 were identified as the most active catalysts from the two groups with indicative yields of 202 and 303 ml H-2/g cellulose, respectively The 10 wt %Co/MCM-41 catalyst gave with the highest H-2 selectivity reaching 21 7% of the dry product gas (C) 2010 Elsevier B.V All rights reserved.