A synchronous fluorimetry for simultaneous determination of dissolved anthracene and pyrene in aqueous solution has been established. The linear ranges for determination of dissolved anthracene and pyrene were 1.00x10(-8) to 4.50x10(-7)molL(-1) and 5.00x10(-9) to 6.50x10(-7)molL(-1), and the limits of detection (LOD) for anthracene and pyrene were 2.23x10(-9) and 8.24x10(-10)molL(-1) with relative standard deviations (R.S.D.) of 2.90 and 2.34% (n=5), respectively. Satisfactory results were obtained when the established method was used to simultaneously determine anthracene and pyrene in spiked water samples.