A possibility of using clay waste rocks (shales) from coal mines in the removal of heavy metals from industrial wastewaters is considered in this paper. Raw and calcined (600 °C) shales accompanying the coal beds in two Polish coal mines were examined with respect to their adsorptive capabilities for Pb, Ni and Cu ions. The mineralogical composition of the shales was determined and the TG/DTG analysis was carried out. The granulometric compositions of raw and calcined shales were compared. Tests of adsorption for various Pb(II), Ni(II) and Cu(II) concentrations were conducted and the pH before and after adsorption was analyzed. The results indicate that the shales from both coal mines differ in adsorptive capabilities for particular metal ions. The calcination improved the adsorptive capabilities for lead, but worsened them for nickel. The examined shales have good adsorptive capabilities, and could be used as inexpensive adsorbents of heavy metal ions, especially in the regions where resources of shale are easy accessible in the form of spoil tips.