A quantitative analysis method of halogen elements in volatile organohalogen compounds was established by the Wickbold combustion pretreatment in an enclosed system and ion chromatography. The sample pretreatment parameters of Wickbold combustion were experimentally optimized, and using the determined optimal pretreatment parameters, the reproducibility was estimated by ion chromatography. As a comparison for real samples, NIST certified reference materials (CRMs) were analyzed for the recovery efficiency and reproducibility.