In this project we studied the electrochemical mineralization of synthetic human urine contained in alkaline aqueous solution by means of Ni(II)cyclam-modified nanoparticulate TiO₂ films (OTE/TiO₂/Ni-cyclam, where an optically transparent electrode OTE was utilized as conductive substrate) and the simultaneous electrogeneration of H₂ via H₂O reduction on Pt cathodes; both inserted in an electrolytic cell. Comparative results were obtained from the same setup where an anode without TiO₂ (OTE/Ni-cyclam) was alternatively inserted in the electrolysis cell. Electrolysis experiments were carried out for 2h by applying 1.0V vs. NHE to the OTE/TiO₂/Ni-cyclam or OTE/Ni-cyclam anodes, where the urea oxidation was predominantly taking place, while the H₂ was continuously evolved from the Pt cathode. During this period of time, urine mineralization and H₂ production were followed by measuring at the same time: the decrement of the total organic carbon (TOC) in the electrolytic solution and the H₂ evolved from the cell. Our results revealed that the H₂ evolution proceeds on Pt cathode when the mineralization of urea contained in urine achieves efficiencies of 53 and 36% on OTE/TiO₂/Ni-cyclam and OTE/Ni-cyclam electrodes, respectively. Furthermore, it was also observed that urea electrolysis on the OTE/TiO₂/Ni-cyclam anodes occurs without interference of parasitic reactions, which could be promoted from other chemical components of the synthetic urine (i.e. chloride ions oxidation for producing hypochlorite ions); thus suggesting that the combination of Ni-cyclam with TiO₂ is essential for inhibiting secondary electron transfer processes. These results demonstrate that the OTE/TiO₂/Ni-cyclam electrodes could be considered as a promising electrochemical technology for aiding to the treatment of wastewaters containing real human urine, which can be accomplished by H₂ generation.