A novel type of resin derived from calix[4]arene carboxylate was synthesized and adsorption behavior for lead(II), zinc(II), copper(II), nickel(II), and cobalt(II) was investigated. Further, column separation of lead(II) from zinc(II) was also carried out. Adsorption equilibria of metal ions showed following order of selectivity series among metal ions: Pb(II) >> Cu(II) > Zn(II) > Co(II) = Ni(II). Separation of lead and zinc using the packed column was sufficiently achieved.