Abstract: The chelate compound formed by terbium with dipic clinic acid (DPA) has been used as the basis for a selective spectrofluorimetric determination of microamounts of terbium. At pH5-12, [DPA]/[Tb]≥10, the chelate of terbium with DPA forms quickly. The composition of the chelate is Tb:DPA=l:3. The system absorbs the radiation characteristic of DPA at 280nm, and emits the band fluorescence of the dipicolinate of terbium with the emission characteristic of terbium at 542nm.A linear increase in 542nm emission intensity was obtained in solution containing 4-40ng/ml and 0.02-0.24/μg/ml of terbium. The interference of other metals was examined. When sufficient DPA was present to chelate the terbium, the remaining lanthanides and Ca, Mg, Cu, Zn, Al did not affect the fluorescence intensities. The interference of ferric ion can be masked by EDTA. Satisfactory results were obtained by the proposed method for the determination of terbium in LaOBr and La₂O₃ Samples.