Toxic heavy metals and organic pollutants are simultaneously exist in the wastewater of some industries. This study explores reduction of poisonous divalent nickel ions from either nitrate or sulfate salts coupled with naphthalene (NA) degradation using titania photocatalyst in an efficient photo-sono reactor. A synergism appears when reduction and degradation treatments perform simultaneously in the media. With initial concentrations of [Ni(II)]0 = 5 mg/L and [NA]0 = 10 mg/L, under dominant mild conditions, removal efficiencies of 54.5% and 56.6% were correspnding to Ni(II) and NA when nickel nitrate was used, respectively. These efficiencies were enhanced to 59.2% and 57.5% with nickel sulfate source, all after 90 min operations. For evaluating the mechanism of reactions, reactive oxygen species analysis on solutions as well as FTIR, SEM and BET analysis on the titania nanoparticles, before and after usage, were conducted. The reaction kinetic was also followed for individual species in the mixed solution and accordingly, the energy consumption was evaluated for one order of magnitude decrease in pollutants concentration. The high performance of the used method was revealed in comparison to the similar reported reduction/degradation processes.