Bulk nickel aluminate (NiAl2O4) was synthesised by co-precipitation at a Ni/Al mole ratio of 1:2 (stoichiometric ratio). The prepared sample was reduced at different temperatures, in the 300 to 850 degrees C range, and obtained assays were analysed by a wide range of analytical techniques (XFR, XRD, H-2-chemisoprtion, H-2-TPR, DRS UV vis NIR, FTIR, Al-27 MAS NMR, NH3-TPD, CO2-TPD, TPO) and tested for the APR of glycerol. The spinel precursor allowed the formation of small and stable Ni particles (< 14 nm) upon reduction with good performance in the APR of glycerol (NiAI-850 93% conversion, 57% conversion to gas, at 250 degrees C/45 bar and WHSV 24.5 h(-1)). Hydrogen was the main gaseous product and the activation temperature did not substantially alter selectivity to gaseous products; however, selectivity to intermediate oxygenated liquid compounds was substantially modified. Overall, glycerol dehydrogenation route was dominant at high reduction temperature. The good stability of the spinel led to stable H-2 yield in the long-term runs (50 h) and proved potential to be used in the APR of glycerol.