This study was carried out in a technogenic landfill of sludge from the Taiaçupeba Water Treatment Station, Suzano, Brazil. The availability of this residue is a problem, since the presence of heavy metals in the sludge increases the risk of contamination of the physical environment, especially the soils and groundwater. The metal dosage methodologies in the samples took into account the presence of organic matter, and the use of technologies based on Advanced Oxidative Processes (AOPs) were applied to lead to the complete mineralization of metallic chemical elements. The results indicated that the irradiated samples presented higher metals dosages in relation to the non irradiated samples. The application of water analysis techniques through advanced oxidation processes (AOP) such as radiolysis indicated that contents found in environments containing high organic matter concentration, such as the samples collected in the technogenic landfill where the sludge was deposited, presented different values from those analyzed through conventional techniques.