In this work the catalytic performance of NiAl2O4 catalyst in the partial oxidation of methane (CH4(1)/O-2(0.5)/N-2(8.5) and 4800 mLCH(4)g(-1) h(-1)) was investigated. This bulk catalyst resulted more active (70% conversion at 625 degrees C) than alumina supported nickel catalysts prepared by conventional impregnation (11%Ni/Al2O3-30% conversion at 625 degrees C and 14%Ni/Al2O3-65% conversion at 625 degrees C) and a commercial platinum catalyst (1%Pt/Al2O3-30% conversion at 625 degrees C). Further, the behaviour of NiAl2O4 was comparable to that of a commercial rhodium catalyst (1%Rh/Al2O3-75% conversion at 625 degrees C). Fresh and spent catalysts were characterised by N-2-physisorption, H-2-TPR,UV-vis-DRS,WDXRF, XRD,TGA-MS, TEM and Raman spectroscopy. After catalyst reduction CH4 conversion over bulk NiAl2O4 was associated with the formation of large amounts of metallic nickel crystallites with a relatively small size. Although significant coking was noticed, conversion and selectivity to H-2/CO were not significantly affected after prolonged time on stream. (C) 2012 Elsevier B.V. All rights reserved.