Pb 2+ and NO 3 − are major water pollutants with severe environmental effects. Several methods were used for treating them, but most of the intended solutions failed to treat these ions simultaneously. Electrodialysis (ED) may be able to treat them, particularly after the recent progress in membrane manufacture that has led to significant improvements in the performance. In this paper, we investigated the effect of pH on ED separation of Pb 2+ and NO 3 − in terms of concentration ratio (CR), concentration polarization (i lim ), current efficiency (η), and energy consumption (EC). The results showed that, pH between 3 and 5 was the most effective for removal of these ions. Additionally, the distribution of ions among the charged sites on the membrane surfaces was governed by pH. At low electric potentials (<10V), ion exchange/adsorption was the prevalent phenomenon occurring on the membrane surfaces, while at voltages over 25V the membranes were regenerated. Consequently, cation and anion exchange membranes could be used for water treatment at low voltages, then regenerated at higher voltages.