The catalytic decomposition of CH 4 for the production of pure H 2 is carried out over Ni supported on hydroxyapatite [Ca 5 (PO 4 ) 3 (OH)] catalysts at 650°C and atmospheric pressure. CH 4 decomposition activity is decreased with time on stream and finally deactivated completely. The physicochemical properties of the fresh catalysts are characterized by XRD, DTA/TG, TPR and SEM techniques along with CHNS analyses of the used samples. It is found that the 30 wt% Ni/HAp displayed higher H 2 production rates over the other Ni loadings, which is correlated with Ni metal surface area measured by O 2 pulse chemisorption.