Abstract: A method for simultaneous determination of phenol and resorcinol in mixtures using fluorimetry is developed by combining synchronous fluorescence technique with linear regression of multiwavelength data. The effect of solution pHand other mental variables was examined and the optimal condition for determination of phenol and resorcinol was established. The proposed method was applied to fluorescent assay of resocinol based on preparation with recoveries of 97.18 (± 2.42)% and 98.15(±2.70)% for phenol and resorcinol, respectively.