Extraction of Cd, Pb, Zn, Ni, and Cu from aq. solutions with kerosenic 10% di-(2-ethylhexyl)-phosphoric acid was the more efficient, the higher was the pH (0.68 to 4.54) of the aq. phase. At pH 2.5, Pb and Zn were nearly 100% extracted; so were Cd and Cu at pH 3.5; at pH 4.5, Ni was extracted only in 76.6%. Separation of Pb from Zn and Cd from Cu was judged impracticable. Three pairs were studied, Pb-Cd, Cd-Ni, and Pb-Ni, to re-extract the metals from the org. phase with oxalic acid + ammonium oxalate at the pH considered most advisable from the extraction step. Single-stage re-extraction at fixed pH and three-stage re-extraction at varying pH values of the re-extractant were studied. The former gave better recoveries and better selectivities than the latter, except for the Pb-Cd pair which could not be fully separated.