In this paper we have presented results on spinel nano-materials considering a collection of techniques, which is considered today a state-of the-art in the field of catalyst research (characterization and study of structure/reactivity relationship). Through a selected collection of techniques, experimental as well as theoretical, we illustrate this setup of techniques on the characterization of spinels (ZnAl2O4) through XAS and by anomalous wide angle X-ray scattering (AWAXS). The effect of Al/Zn substitution was investigated as well and related Co/Al spinels were investigated on their catalytic properties using OFT. The catalytic properties towards NO, O-2, and NH3 are explored for the very first time on the Co/Al spinet surfaces, and possible reaction mechanisms proposed. (C) 2015 Elsevier B.V. All rights reserved.