In this study several complementary methods as XRD, HRTEM, O-2 and H-2 adsorption, as well as H-2-O-2 titration were used for characterization of the metallic phase in 0.5-3.0 wt.% Pt/ZnAl2O4 catalysts. Three nanocrystalline ZnAl2O4 spinels used as a supports were prepared by the solvothermal and co-precipitation method. It was found that irrespective of the preparation method they form very good support materials with a high capacity to achieve high platinum dispersion. O-2 and H-2 chemisorption data showed metal dispersion up to 90% and good correspondence with HRTEM results was observed. The H-2-O-2 titration method may be applied for determination of Pt dispersion only in the high-loaded Pt/ZnAl2O4 catalysts. The catalytic performances of Pt supported on the prepared spinels were evaluated in the propane total oxidation reaction. (C) 2010 Published by Elsevier B.V.