Solutions, obtained from the mixture of different mole ratios of N-vinyl 2-pyrrolidone and acrylonitrile, were irradiated in a Co-60-gamma source to produce copolymers. The swelling percentage curves were formed, and a diffusion exponent was calculated. For the uranyl ion adsorption, these copolymers were reacted with hydroxylamine hydrochloride to convert C=N groups to -C=N-OH (amidoxime) groups. The optimum amidoximation time was determined by uranyl ion adsorption. The structure of copolymers, before and after amidoximation, was analyzed with spectroscopic and thermal methods.