Novel resins have been prepared by crosslinking calix[4]arene tetracarboxylate units each other by methylene groups to investigate their solubility to some organic solvents and basic solutions, and their adsorption behavior for lead(II), zinc(II), copper(II), nickel(II), and cobalt(II). The present resins exhibit high selectivity to lead due to the special complexation nature of calix[4]arene tetracarboxrylate. The sequence of adsorptive selectivity for metal ions is as follows: Pb(II)•¬Cu(II)>Zn(II)•¬Co(II)•¬Ni(II). The resin prepared by crosslinking calix[4]arene units using trioxane as the crosslinking reagent with the molar ratio 1:1 (calix[4]arene unit:trioxane) exhibit the highest loading capacity for lead ion, 2.10 mol kg-1.