The paper provides the physicochemical analysis of galvanic sludge to determine the presence and concentration of toxic metals. Two sludges sampled from the same factory, but from different technological processes, alkaline galvanic sludge obtained from galvanizing process and acidic sludge generated from the chromium plating process were analyzed. Inductively Coupled Plasma - Optical Emission Spectrometry (ICP-OES) revealed increased concentrations of toxic heavy metal ions Zn2+, Cr3+, Ni2+ and Pb2+ in the sludge from the galvanizing process and Cr3+, Cu2+, Ni2+, Pb2+, Cd2+ and Zn2+ from the chroming process. Moreover, the sludges were further physicochemically characterized by Reflectance Fourier Transform InfraRed Spectrometry (FTIR), Scanning Electron Microscopy with Energy-dispersive X-ray Spectroscopy Analysis (SEM-EDX) and X-ray diffraction (XRD). The results of ICP-OES were corroborated by FTIR. Analysis of FTIR spectra revealed the specific bands indicating the existence of metal oxides in the analyzed sludges, as well as the presence of organic substances, i.e. solvents and surfactants, used in the electroplating process. The analysis was accomplished following international norms and confirmed the increased concentrations of heavy metal ions from both sludges. In line with the regulations of the Environmental Protection Agency (EPA), the results proved the hypothesis that galvanic sludge is hazardous waste.