Triethylene glycol dimethacrylate (TGD3) crosslinked macroreticular type polyacrylonitril (PAN) was synthesized. Toluene added as diluent lowered the polymerization capability of acrylonitril (AN) monomer, especially in low degree of crosslinking. Maximum surface area of crosslinked PAN was obtained at 60~90% dilution over all the experimenal range of 5~20% degree of crosslinking. Amidoximated-PAN(Ami-PAN) chelate resin has an excellent adsorption capability for Cr+2, UO2+2 regardless of pH and concentration of metal ion. Adsorption of metal ion was not governed by surface area of Ami-PAN resin matrix.