The chemical and biochemical oxygen demand values of a number of synthetic and wastewater samples were determined using fluorescence spectroscopy. Treated and untreated sewage samples were obtained from a local sewage treatment works while synthetic samples were analysed before, during, and after treatment via a rotating biodisc contactor. Fluorescence intensities were normalised using the water Raman signal as an internal standard and corrections applied to take into account the attenuation effects caused by the sample matrix. The fluorescence emission spectra (lambda(exc) = 280nm) of synthetic and sewage samples were very similar in that two main fluorescence bands centred around 350nm and 440nm were observed in all samples. Normalised fluorescence data, centred at 350nm, correlate well with corresponding BOD, COD and TOC values (R-2 values ranging between 0.93 and 0.98). Using BOD, COD and TOC data the fluorescence at 350nm and 440nm can be apportioned to biodegradable and non-biodegradable dissolved organic matter respectively. The findings of this research show that fluorescence data can be used to quantify oxygen demand values (chemical and biochemical) and total organic carbon values. Furthermore, the fluorescence spectral response can be apportioned to biodegradable (BOD) and non-biodegradable (COD -BOD) dissolved organic matter. The potential of using fluorescence spectroscopy as a possible tool for real-time monitoring of sewage wastes is discussed.