Macroreticular type crosslinked polystyrene useful for a chelate resin matrix and gel extraction chromatography was prepared. The effect of the external appearance of resin matrix on the polymeric reaction was also examined by chloromethylation of crosslinked macroreticular type polystyrene. In preparation of macroreticular type crosslinked polystyrene, the influence of the amount of diluent on the surface area of resin matrix and polymeric reactivity was studied.