An experimental study has been made on the recovery, separation and concentration of some metals from electroplating solutions and sludge. Two membrane methods, i.e., the Donnan dialysis (DD) and the pertraction in a multimembrane hybrid system (MHS) were used and compared. Related ionic fluxes and separation coefficients for uni- and divalent cations were measured and discussed. It was found that the DD as a simple membrane technique can be used to permeate Zn²⁺ and Cu²⁺ with high fluxes associated with fluxes of other cations (Na⁺, Ca²⁺, Mg²⁺). The selective recovery of Zn²⁺ at the presence of Mg²⁺, K⁺, and Na⁺ was reached in the MHS composed of cation-exchange membranes and a liquid membrane containing di-(2-ethylhexyl) phosphoric acid (D2EHPA) or bis(2,4,4-trimethylpentyl) thiophosphinic acid (Cyanex 302) as a selective carrier. In the case of solutions remaining after zinc electroplating, the Zn²⁺ flux was 1.6x10^-11 mol/cm²s, and separation coefficients a^Zn_S gained the value of 8-10. The use of the MHS for processing dissolved and acidified sludge (pH~1) allowed to recover Zn²⁺ with the transport stationary rate equal to 3.2x10^-11 mol/cm²s. According to the D2EHPA properties, other cations as Cr³⁺, Fe³⁺, Cu²⁺, Mg²⁺, and Na⁺ have not been transported to the stripping solution (1 M H₂SO₄). The use of Cyanex 302 instead of D2EHPA considerably lowers the flux of calcium and leads to the effective separation Zn²⁺ over Ca²⁺.