A polymeric decontaminant N,N-dichloropolystyrene sulfonamide was synthesized by different steps from starting material polystyrene and followed by sulfonation, chlorosulfonation, and amidification. Halogeno-sulfonamide was obtained by treatment of sodium hypochlorite with sulfonamide resin. It was characterized by FTIR, solubility, viscosity, DSC, and TGA techniques. Efficiency of this polymer as decontaminant was evaluated by reaction with 2-chloro ethyl pheny] sulfide, a simulant of sulfur mustard (SM) at room temperature. This decontamination reaction was monitored by gas chromatography (GC) and products were identified by gas chromatography-mass spectrometry (GC-MS). The positive chlorine content of this polymer was checked by standard iodometry titration. The synthesized positive chlorine compound is observed to be a promising decontaminant against simulant of sulfur mustard, chiefly in the situation where use of aqueous medium such as acetonitrile : water (2 : 1) is precluded. (c) 2007 Wiley Periodicals, Inc.