Cloud point extraction (CPE) has been used for the preconcentration and indirect quantification of cyanide after the formation of a ion-associate complex with 3-amino-7-diethylamino-8,9-benzo-2-phenoxazine chloride (Nile blue, NB+) in the presence of copper (II) ions, and later analysis by flame atomic absorption spectrometry (FAAS) using polyethyleneglycolmono-p-nonylphenylether (PONPE 7.5) as extracting surfactant. The chemical variables affecting the separation phase and the viscosity affecting the detection process were optimized. At pH 5.5, preconcentration of only 50 mL of sample in the presence of 0.04 % (w/v) PONPE 7.5 and 5.64 x 10(-5) mol L-1 Nile blue permitted the detection of 3.75 mu g L-1 cyanide. The enhancement factor was 64.7 for cyanide. The proposed method was successfully applied to the determination of free cyanide in environmental water samples. The method was compared with the pyridine-barbituric acid method and the paired t test was used to determine whether the results obtained by the two methods differ significantly.