A new hydrogel that contains sulfur is prepared by radiation polymerization and its application for recovery of Hg2+, Pb2+, Cd2+, and Cu2+ ions is discussed. The metal hydrogel complexes are isolated and characterized by using different spectroscopic techniques (UV-visible, IR, NMR, and mass), thermal analysis (TGA and DSC) measurements, and SEM. Also, the mode of complexation is determined using IR and NMR spectroscopy. The scanning electron micrographs show that the hydrogel has a great ability to recover the metal ions in the following order: Hg2+ > Cd2+ > Pb2+ > Cu2+. TGA thermograms are used to investigate the mechanism of thermal decomposition.