The degree of chemical treatment in terms of removal of organic matter from different wastewaters has been investigated by employing potassium ferrate (K2FeO4) and ozone in various combinations. The study was performed in both the batch and the continuous flow systems. The treatment efficiency was determined through three different methods, i.e., chemical oxygen demand (COD), fluorescence and ultraviolet (UV) absorption. Fluorescence and UV absorption techniques were employed due to their specificity in measurement of humic substances, aromatic compounds and heterocyclic systems, whereas COD is a general parameter for the estimation of total organic matter. Fluorescence and UV absorbance values were correlated with respective COD values.