Photocatalytic hydrogen generation by water splitting ($H_2O_{(1)}{ ightarrow}H_2_{(g)}+1/2O_2_{(g)}$) has been studied on photocatalysts based on Zn, Cd, Fe and Cu, synthesized by coprecipitation. Iron and copper nanoparticles were incorporated as cocatalysts to enhance the photocatalytic activity of the ZnCd solid solution. The effect of the different synthesis parameters (temperature, elemental atomic ratios, amount of Cu and Fe incorporated in the catalyst and calcination temperature) on the photocatalytic production of hydrogen has been studied in order to determine the best experimental synthesis conditions. The catalysts have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and BET. The experiments of photocatalytic water splitting were performed in aqueous solution of the photocatalysts previously dispersed in a soft ultrasound bath. The photocatalysts were irradiated under different lights ranging from 220 to 700 nm. The photocatalytic activity was found to be clearly dependent on the specific area of the photocatalyst.