Removal of lead and zinc from binary aqueous solutions with total initial concentrations co ≈ 1 mmol/l, at different ratios of co(Pb)/co(Zn) from 0,18 to 2,15 has been examined using the column method. Experiments were carried out isothermally in glass columns filled with natural zeolite up to bed depths of 4, 8 and 12 cm. Service and regeneration cycles were studied by monitoring of the Pb and Zn concentrations and pH values in the effluent and regenerate solutions. The measurement of pH values allows efficient determination of the breakthrough point and the end of regeneration. The results are shown by breakthrough curves and regeneration curves and the following characteristic parameters have been calculated: breakthrough and exhaustion capacities, removal efficiency, symmetry of breakthrough curves, height of the mass transfer zone, empty bed contact time, quantity of eluted ions, degree of regeneration, and the concentration factor. Twelve successful service and regeneration cycles were carried out without reducing zeolite capacity. Up to breakthrough, Pb and Zn ions were bound simultaneously according to their concentrations in the influent, while at the exhaustion point the quantity of bound Pb was higher. This is due to the displacement of bound Zn by Pb from the feeding solution. This effect has been confirmed by regeneration of zeolite where the ratio of quantities of eluted ions nR(Pb)/nR(Zn) was much higher than the Pb/Zn ratio in the influent. The displacement effect has also been confirmed by SEM images of zeolite particles and elemental EDS analysis. The regeneration of zeolite provides for complete elution of bound ions and the volumes of regenerates were up to 10 times lower compared to the volume of solutions in service cycles. This contributes to the application of natural zeolites in wastewater treatment processes. The experimentally obtained breakthrough curves have been tested according to the Thomas and the ADR models. The modelled curves showed very good agreement with the experimental ones, and were helpful in estimation of kinetic parameters and mechanisms of mass transfer during the overall process.