To selectively separate arsenic from arsenic-containing copper dust, this paper reports a new method of treating the dust by carbothermal reduction and roasting it with coke powder at low temperatures. The effects of different roasting temperatures, coke powder additions and roasting times are discussed. Optimum conditions were obtained to selectively separate arsenic from other valuable metals. The volatilization rate of arsenic was 97.02% and the content of arsenic in the slag was 0.31%. Other valuable metals were not volatile under the conditions of a 350?C roasting temperature, coke powder addition of 30%wt, coke powder particle size of 0.15?1 mm, and a roasting time of 150?min.