Acidic organophosphorous extractants were screened for the mutual separation of Mn(II) and Zn(II), in a leach solution of waste Zn–C cell powder. This was done using a 2mol/L H2SO4 solution containing 2g/L glucose. Extraction characteristics of both metal ions in this mixture have been examined as functions of equilibrium pH. Although tech. and anal. grade D2EHPA are not so effective for the separation, PC88A, Cyanex 272, Cyanex 302 and Cyanex 301 are all promising for this purpose. Strippings of Mn(II) and Zn(II) from the extracted organic phases have been examined, using 0.25, 0.50 and 1mol/L H2SO4; and 1mol/L HCl, HNO3 and HClO4 at different phase ratios. H2SO4 appears to be the best stripping agent. A 1mol/L H2SO4 solution strips almost 100% of target metal ions in 10min, regardless of the extractant used. As ΔpH1/2 =2.75 and as the max. separation factor (β)=1793 for Cyanex 302 at pH(eq) =4.0, a flow sheet has been developed for their mutual separations. Finally, classical precipitation methods have been adopted to obtain MnS and ZnS, which can be easily oxidized to MnO2 and ZnO, respectively.