This paper considers the fluorescent behavior of the compounds formed by terbium and dysprosium with nalidixic acid, which has been used in a highsensitivity method for the selective and rapid determination of these elements. The fluorescence intensities from the terbium and dysprosium complexes were recorded, and the content of the terbium in the sample was calculated from the heights of the fluorescence peaks for the sample alone and with additives. The accuracy and reliability were checked under laboratory conditions in analyzing specimens of lanthanide oxides for terbium and dysprosium by the method of addition.