Results of experiments on the adsorption of plutonium (IV) on alumina and their application to the recovery of plutonium from analytical waste solutions containing phosphoric-nitric acid are reported. Distribution ratios of plutonium (IV) between alumina and solutions containing varying concentrations of phosphoric acid and nitric acid are determined. The influence of various ions like UO22+, Fe3+, MoO42–, VO2+ and SO42– on the distribution ratio is evaluated. Saturation values of adsorption of plutonium (IV) on alumina and optimum conditions for loading and elution of plutonium on a column packed with alumina are described.