Tetraethyleneglycol-dimethacrylate (TGD) and ethyleneglycol-d imethacrylate (IGD) crosslinked polyacrylonitrile(PAN) was polymerized gel and macroreticular type crosslinked PAN was synthesized to investigate the effect of external resin appearance on the adsorption capacity for metal ions. As the side reaction, cyclization reaction between introduced amidoxime group was accompanied in the course of amidoximation of PAM. Cyclization was modelized from the nitrogen content analysis of amidoximated PAN (Ami-PAN). Ami-PAN amidoximated in water medium shows higher adsorption capacity than that amidoximated in methanol. Ami-PAN has an excellent adsorption capacity for Cu+2, Cr+2, Cd+2.