A new chemiluminescence method was presented for the determination of phenol based on its sensitization on the luminol-K3Fe (CN)(6) system. The linear range for phenol is 0.01 similar to 10 mg/L. with a detection limit (3sigma).of 4 x 10(-3) mg/L, and the relative standard deviation (3sigma) for 1 mg/L phenol is 1.06% (n = 11). The proposed method has been applied to the determination of phenol in river waters and industrial waste waters with satisfactory results.