Slovakia has a long and distinguished tradition in the field of mining and in the processing of raw materials such as gold, silver, copper, and iron ores. In medieval times, the area that is today’s Slovakia was one of the most important producers and processors of sulfide ore, which was processed specifically by flotation. Flotation waste is the remains of fine-grained materials that are deposited in sludge beds after mining and mineral processing activities. Flotation waste also contains residues of heavy metals, which can pose a potential risk to the surrounding environment. The areas with this deposited material (heaps and sludge beds) have been classified as an environmental threat and require regular monitoring by government bodies. The Slovinky sludge bed is one of these areas. The aim of the work was therefore to investigate the selected physico-chemical properties of sludge flotation waste using spectroscopic methods (XPS, XRF, and AAS). Our findings showed that the concentrations of Cu, Zn, and Ni exceeded the limits set by the relevant legislation by several fold even two decades after the end of mining and processing activities. Although the sludge bed material is alkaline, our results showed that the sludge bed material could be a potential source of selected heavy metals. The obtained data could help in the protection and restoration of areas affected by the mining and processing of sulfide ore.