To prevent an environmental pollution by hazardous heavy metals, in the present study, a simulatenous decrease of the concentration of Pb((II) and Cu(II) in the solution by photo-Fenton method has been systematically studied. Photo-Fenton process proceeded in a close reactor by batch technique. The process was conducted by exposure solutions containing Pb(II) and Cu(II) ions, and Fenton’s reagent (Fe2+ and H2O2) under UV-A lamp. In this study, the initial concentations of Pb(II) and Cu(II), and the exposure time were optimized. The synergyc effect that may be appeared on the decrease of Pb(II) and Cu(II) ion concentrations simultaneously through photo-Fenton process was also addressed. The concentrations of Pb(II) and Cu(II) in the solution were determined by AAS. The research results exhibited that photo-Fenton process could decrease Pb(II) and Cu(II) concentrations, and the maximum decreases, 46.12 % dan 16.86% for Pb(II) and for Cu(II) respecticely, were found by applying both initial concentration of Pb(II) and Cu(II) as much 35 mg/L, and 60 min of the time. The concentration decreases of Pb (II) and Cu(II) were results of oxidation by OH and by electron to form PbO2 and Cu particles respectively as probed by EDX data. Furthermore, photo-Fenton process toward a solution containing Pb(II) and Cu(II) ions allowed oxidation of Pb(II) and reduction of Cu(II) simultaneously and showed a synergic effect. Such effect was demonstrated by the fact that the presence of Cu(II) ion in the photo-Fenton process of Pb(II) solution could improve the Pb(II) oxidation and the highest improvement of Pb(II) oxidation (81.06%) was shown by 35 mg/L of the Cu(II) concentration. Similarly, the presence of Pb(II) in the photo-Fenton process of Cu(II) solution could enhance the reduction of Cu(II), and the highest effect on the Cu(II) reduction enhancement was exhibited by 35 mg/L of the Pb(II) concentration.