Laboratory scale experiments with anion and cation exchange resins aiming to separate arsenic from highly acidic, sulphate-containing solutions were carried out. The data obtained proved that the use of strong acid cation exchangers in the Na form gives the opportunity for arsenic/acid separation in two stages. During the period of sulphuric acid accumulation (a period in which the resin is converted from Na form to its H form), the residual sulphuric acid concentration within 3 BV is below 0.1 g/l. The arsenic concentration in the effluent remains unchanged. The acid obtained, during the period of sulphuric acid recovery by stripping with Na 2SO 4 has a higher concentration than the initial concentration in the waste acidic solution. The recovered acid has levels of As, Cu, Pb and Fe low enough to be used in the sulphuric acid production industry. As a net result, the implementation of the strong acid ion-exchange method leads to two streams: (1) low acidity water in which all the arsenic is concentrated; (2) sulphuric acid free of arsenic.