The presented thesis deals with the possibility of the application of mechanically activated metal mixtures (aluminum and nickel) for the removal of halogenated aromatic compounds from an aqueous environment. Mechanical activation is a process, in which the compounds are activated by milling, mainly due to an increase in a specific surface area and the formation of various defects in their crystal structure. Thermally treated activated Al-Ni mixtures may lead to a decrease in the total costs of reductive dehalogenation process for selected analytes in comparison with commercially available Raney type Al-Ni alloys; such as the 50:50 wt.% Al-Ni alloy