Sphalerite concentrates prepared during processing of Missouri lead ores contain small percentages of cobalt and nickel which adversely affect zinc electrolysis. The Bureau of Mines has evaluated solvent extraction and precipitation techniques to remove and recover cobalt and nickel from zinc sulfate solution prior to zinc electrolysis. Prepared zinc sulfate solutions containing about 190 gpl of zinc and 50 ppm of both cobalt and nickel were treated using various combinations of complexing reagents, solvent, ph, concentration, time, and temperature. The following complexing reagents gave the best results: a-nitroso-b-naphthol, b-nitroso-a-naphthol, 1,2 cyclohexane dione dioxime (nioxime), di-2-pyridyl ketone oxime, and dimethylglyoxime. These reagents in suitable solvents lowered the cobalt and nickel levels to less than 0.1 Ppm. Stripping the complexed reagents from the solvents was not possible except for nioxime. Direct addition of the appropriate reagent to the prepared zinc sulfate solution resulted in the precipitation of cobalt and nickel. Several possible flowsheets are presented for the removal and recovery of cobalt and nickel. Good zinc deposits were successfully electrowon from zinc sulfate solutions purified by solvent extraction and precipitation.