Сhemical monitoring of phenols in natural, waste and tap waters has been completed. Phenols extraction concentration has been carried out by butyl acetate without organic solvent in water — antipyrine — naphthalene-2-sulphonic acid system. Combined analytical techniques — extraction-fluorometric and extraction-photometric — techniques should be combined with hybrid chromatographic one during chemical monitoring. The technique of phenols extraction from waters is statistically significant for the resulting analytical procedure of detecting phenols in water. Two combined extracting-fluorimetric techniques with and without organic solvent (butyl acetate) have been tested in practise. The features and advantages of bottom systems water — pyrazolone derivative — naphthalene-2-sulfonic acid have been discussed. The results of waters chemical monitoring give evidence to the complete discordance of the tested samples to the existing fishery standards for phenols — 1 μg/dm³.