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A series of periphyton, sediment, and water samples has been collected from the Kolubara River and its tributaries at selected locations, characterized by heavy industrialization, and analysed for stable isotopes by X-ray-fluorescence spectrometry. The results of measurements for stable metals revealed that the anthropogenic contribution essentially overwhelms the natural system of the catchment. Thus, concentrations of heavy metals near points of industrial discharge were significantly higher than background concentrations. The existing primary and secondary waste water-treatment plants associated with heavy industry of the area must therefore be revived, and control should be instituted at the sources of pollution. The bioaccumulation factors (BF), and sediment distribution coefficients (K(D)), and concentration ratios (CR) for sixteen stable isotopes were calculated. It is shown that the concentration ratios of periphyton over sediment for Mn, Zn, As, Sb, I, Ba, and Pb exceeded unity. Furthermore, the recorded partition coefficients were indicative of the distribution and mobility of the stable metals in the Kolubara River environment.