Monomers of diacylated amine were synthesized by the reaction of acryloyl chloride or methacryloyl chloride with p-phenylenediamine. Heating DMF solution of these monomers at 75 degrees C in the presence of AIBN as an initiator gave the corresponding polymer. The solid metal-lopolymer complexes with different metal salts were isolated either by the in situ addition of the monomer, metal salt, and initiator at 75 degrees C or by the reaction of the isolated polymer with the metal salt at 150 degrees C. The monomers, polymers, and their metallopolymer compounds were characterized using elemental analysis, IR, NMR (H-1 and C-13), and MS spectral measurements in addition to thermal analysis. The IR data showed that the coordinating atoms of the polymer are dependent on the reaction temperature. The ion selectivity of the isolated polymers toward different metal ions either for a single metal ion or in a mixture as aqueous solutions are studied by the batch techniques. Energy dispersive spectroscopy (EDS) measurements showed that both polymers are more selective to Hg2+ and Pb2+. The morphology of the polymers and their metallopolymer complexes at different temperature was also studied. (c) 2006 Wiley Periodicals, Inc.