In this paper, two major interests, -i.e., synthesis of chloromethylstyrene, and transformation of crosslinked chlormethylpolystyrene into chelating resin-were extensively dealt. first of all, newer method for the preparation of pure o-, m- and p-chloromethylstyrene was investigated. Bromoethylbenzene was chloromethylated by conventional chloromethylation technique yielding mixture of isomers of o-, m-, and p-chloromethylbromoethylbenzene, then this mixture was fractionated preparatively as o-, and p-chloromethylbromoethylbenzene by silica fraction analysis method. This obtained o-, and p-isomers were dehydrobrominated respectively yielding o-, and p-chlormethylstyrene. Then this isomeric chloromethyl-styrene was analyzed by HPLC respectively. In the second place, crosslinked chloromethylpolystyrene beads were prepared directly from the polymerization of chloromethylpolystyrene were transformed into polyethyleneimine ligand type chelate resin by the cationic ring-opening graft copolymerization of 2-methyl-2-oxazoline on to chloromethylpolystyrene. Chelating abilities and capacities of these resins for various metals were extensively discussed and the structural effect of the resin bead on chelating capacities were detailed.