The effect of preparation method (sol-gel, wet mixing or coprecipitation) on the surface structure of zinc aluminate is reported. Coprecipitated and sol-gel prepared ZnAl2O4 were found to be present spinel structure. If calcium was added during synthesis, it was found to be deposited on top of the spinel surface while, if tin was added, the surface of ZnAl2O4 was reconstructed. These aluminates were impregnated with platinum and tested in the isobutane dehydrogenation. The characterization techniques used were LEIS and X-ray diffraction.