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This paper proposes a method for determination of chemical oxygen demand (COD) in domestic wastewater. The proposed method is based on near-infrared reflectance (NIRR) measurements of seston collected from wastewater samples by filtration. The analysis does not require any special reagent, catalyst or solvent. Inherent baseline and noise features present in NIRR spectra are removed by a Savitzky-Golay derivative procedure followed by wavelet denoising. The resulting wavelet approximation coefficients are used for partial-least-squares modelling and subsequent prediction of COD values in new samples. The model is calibrated by using COD values obtained according to the American Public Health Association (APHA) reference method. The proposed method is applied to effluent samples from the anaerobic ponds of the Mangabeira municipal wastewater treatment plant in the city of João Pessoa (Paraíba, Brazil). By comparing the NIRR prediction results with the APHA reference values, a root-mean-square error of prediction (RMSEP) of 19 mg O2 L(-1) and a correlation of 0.97 were obtained. Such results are deemed adequate in view of the joint estimate of the standard error of the reference method, which was calculated as 21 mg O2 L(-1).