Abstract: Dioxane has been frequently detected in river water,especially in ground water polluted by volatile halogenated hydrocarbons.Wastewater samples were passed through the Self-made activated carbon cartridge and PS-2 cartridge connected in a series.The desorbed and concentrated solution of 1,4-Dioxane was analyzed by GC/MS. The results showed that only small amount of samples were needed in this method.Simple sample pretreatment and high recovery were proved.