A novel microporous sorbent consisting of zirconium hydroxide impregnated with triethylenediamine (TEDA) was evaluated for the removal of cyanogen chloride. Breakthrough data were collected on packed beds, illustrating the efficacious nature of TEDA and the enhanced cyanogen chloride removal from the basic zirconium hydroxide structure. NMR and XPS analyses revealed the fate of cyanogen chloride, with inorganic chloride byproducts deposited on the surface of the material and polymerized urea condensates physically adsorbed in the pore structure. The zirconium hydroxide media were found to provide significantly enhanced removal capabilities as compared to traditionally impregnated activated carbons, allowing for the development of respirators with reduced encumbrance.