The use of sodium hexametaphosphate in the spectrofluorometric determination of trace amounts of cerium(III) ions is described. Sodium hexametaphosphate acts as a specific reagent for enhancing the fluorescence intensity of cerium(III) in aqueous solutions. The apparent excitation and fluorescence wavelength used are 304 and 344 nm, respectively. Maximum fluorescence intensity is obtained by irradiating Ce(III) dissolved in 5.346 g/l sodium hexametaphosphate solution at room temperature. The fluorescence varies linearly with the concentration of cerium(III) in the range of 0.001-60 mu g/ml. The coefficient of variation for 45 mu g/ml Ce(III) in 5.346 g/l sodium hexametaphosphate solution is 1. The quenching effects of other lanthanides and some inorganic anions are given. This technique permits a direct and rapid determination of cerium(III) in rare earth mixtures and cerium concentrates.