In this study, separation of silver(I) and zinc(II) from nitrate leach solution of spent silver oxide batteries were carried out by extraction and selective stripping. Di-(2-ethylhexyl) phosphoric acid (D2EHPA) was used to extract Zn(II) and Ag(I) in the equilibrium pH range of 0.991.34. The extraction of Zn(II) was more affected by the pH value than that of Ag(I). Zn(II) and Ag(I) loaded in D2EHPA was separated by selective stripping with a mixture of 0.01 mol/dm 3 nitric acid and 1 mol/dm 3 thiourea and 0.5 mol/dm 3 nitric acid for Ag(I) and Zn(II), sequentially. A process flowsheet for the separation and recovery of Zn(II) and Ag(I) from the nitrate leach solution of spent silver oxide batteries was proposed.where c a,s is metal ion concentration in the aqueous phase