The main purpose of the paper is to share the results and experience from processing soil extracts containing a high concentration of both anionic surfactant and polychlorinated biphenyls (PCBs) by use of method the called adsorptive micellar flocculation. The method is similar to coagulation, but the mechanism is more complicated. The flocculants examined in the laboratory section involved ferric chloride, aluminium chloride, ferric sulfate, and aluminum sulfate. It was observed that ferric chloride provides the best PCB removal efficiency from the extract. Subsequently, two extracts obtained from the pilot-scale demonstration of the PCBs leaching from the soils by the surfactant solution were processed by this method. The volume of the extracts processed was several hundred liters. The method proved it can remove PCBs from all extracts with a very high efficiency (greater than 99.99%). The residual PCB concentrations in solution were less than 1 microg/L.