Microgram quantities of manganese were determined using the extraction of the 8-hydroxyquinaldine (2-methyl8-quinolinol) complex with chloroform and the spectrophotometric measurement of the extract. The method is applied successfully to traces of manganese in uranium after most of the uranium is removed by tributyl phosphate extraction. This method, without preliminary separation of the metal, is used also for the determination of microgram quantities of manganese in aluminum. With both metals, the procedure is more sensitive, precise, and accurate than the usual permanganate method, and is useful for determining manganese down to the 1-ppm level.