Non-sulfide lead flotation tailings draw attention in terms of their valuable contents. Dissolution studies have been carried out with strong inorganic acids, especially in ore form, but these acids have been unfavorable in removal in the context of metal recovery processes. Organic acids, on the other hand, are notable for their environmentally friendly properties and selective metal recovery opportunities. In this study, the effects of acetic acid on metal recovery from oxidized waste were investigated with different experimental parameters at a laboratory scale. Optimal conditions were determined depending on the increase in acetic acid concentration. At 0.75-1.0 M acid concentrations, 49-55% Pb and 49-54% Zn recovery efficiencies were obtained with grades of 7.0-7.2% and 19.5-19.7%, respectively. The recovery of Pb/Zn by the leaching process with acetic acid and the selective non-recovery of iron were also observed through characterization studies. With the Rietveld XRD method, an increase in iron minerals such as goethite and a decrease in smithsonite-hydrozincite minerals were determined. These changes were seen as a decrease in the contents of these minerals in SEM/EDX analysis and as a decrease in smithsonite mineral bond structures in the FT-IR analysis. This study showed that acetic acid has many advantages in the utilization of zinc-lead-containing oxide flotation tailings, which have high economic value, such as selective metal recovery, easy biodegradability, environmental friendliness, and non-corrosiveness.