A new cationic poly[acrylamide/N, N-diallyl morpholinium bromide/N, N-diallyl piperidinium bromide] super absorbent hydrogels (H1-H7) were prepared via microwave irradiated free radical cyclopolymerization using different composition. By the swelling study, hydrogel H1 is found to bear good swelling properties amongst all prepared hydrogels. The hydrogel H1 has been characterized by Fourier transform infrared (FTIR) spectroscopy, scanning electron microscope (SEM), and TGA analysis. A batch system was applied to study the adsorption of Ni(II) and Cu(II) from aqueous solutions by hydrogel H1. The effect of treatment time, pH of the medium, amount of adsorbent doses, and initial feed concentration of metal ion on adsorption of Ni(II) and Cu(II) from their solution were also investigated. Adsorption of Ni(II) and Cu(II) increases with the increase in treatment time, adsorbent doses, and initial feed concentration and decreases with the increase in pH of the medium. The desorption of metal ions were carried out using 1N HCl and 0.5N H2SO4. (C) 2010 Wiley Periodicals, Inc. J Appl Polym Sci 119: 2485-2493, 2011