A sensitive spectrofluorimetric procedure was described for the determination of dysprosium in mixed rare earths,which was based on the fluorescence of the dysprosium-4-chlorsalicylic acid(CSA)-EDTA-cetyltrimethylammonium bromide(CTMAB) complex.The effect of the experimental conditions on the fluorescence intensity was defined.Under the optimum conditions selected,the fluorescence intensity was linear with dysprosium concentration in the range of 1.5×10-7 ~ 1.4×10-5 mol/L.The detection limits(S/N=3) was 4×10-9 mol/L for dysprosium.With this method,the contents of dysprosium in two rare earths oxides were successfully determined.