The fluorescence excitation-emission matrices (FEEM) of domestic waste water, treated effluent of a waste water treatment plant and receiving river water were analyzed to select wavelengths for the monitoring of organic contents as COD. Excitation/emission wavelengths of 220/350 nm and 270/350 nm for protein-like fluorescence and 240/450 nm and 340/450 nm for humic-like fluorescence were suggested as fluorescence peak emitting wavelength pairs, respectively. Without any pre-treatment, the protein-like fluorescence peaks showed better correlation between COD values and fluorescence intensities than the humic-like fluorescence peaks. No enhanced correlation was observed by removing the suspended solids from the samples using filtration. However, statistical multiple regression methods, using the fluorescence intensities from each peak and the light scattering intensity at 633 nm as variables, resulted in an enhanced correlation, with r2 > 0.9 for the measured and predicted COD values.