This paper describes the development of TiO 2 and ZnO particles by a chemical route, using two different wet synthesis methods: polymeric precursor (PP) and sol-gel (SG). This study aimed to shed a light on how the synthesis method affects the photocatalytic activity of these oxides. Rhodamine B (RhB) degradation was used as a probe reaction to test the as-synthesized TiO 2 and ZnO photoactivity. It was observed that surface availability, which is related to the presence of synthesis residue, is the key parameter to determine photoactivity. ZnO PP and ZnO SG presented degradation of 88% to RhB. Both samples presented synthesis residue on the surface. On the other hand, TiO 2 PP presented a better performance than TiO 2 SG, once 90% of RhB was degraded, while TiO 2 SG degraded 80% of the dye. In this case, TiO 2 PP was free of synthesis residue on the surface, while TiO 2 SG presented residues.