A synchronous fluorescence method for simultaneous determination of catechol and hydroquinone has been established.In pure aquo-medium,by fixing the wavelength interval(ΔA) as 19 nm,the sychronous fluorescence scanning for catechol and hydroquinone is performed fo get the maximum peaks at 298 nm and 315 nm,respectively.On the basis of the fact,the content of both is determined.The concentrations of catechol and hydroquinone are linear with the intensity of synchronous fluorescence in the concentration range of 1.0×10-6-9.0×10-5 mol/L and 1.0×10-6-1.0×10-4 mol/L,with correlation coefficients of 0.998 6 and 0.999 1 and detection limits of 8.2×10-7 mol/L and 5.4×10-7 mol/L.The recoveries of catechol and hydroquinone are found in the range of 83%-107% and 92%-100%,respectively.