Abstract: The p-matrix method for simultaneous spectrofluorimetric determination of phenol and SDBS was studied.Fluorescence intensity was measured at an excitation wavelength of 230nm and three emission wavelengths in the range 290～310nm.The calibration was found linear in the range of 0～0.08mg/L of phenol and 0～0.14mg/L of SDBS.This method has been used satisfactorily for the determination of phenol and SDBS in environmental Water.