SummarySimultaneous detection with a 700-A Hall@ and an NPD detector is an effective technique for characterizing chloro-and chloronitroanilines in highly complex Publicly Owned Water Treatment Works ( P O W sludges. The utilization of a modified Varian effluent splitter and a SE-54 fused silica capillary column permitted the detection of mid-picogram quantities of the polar chloroanilines without sacrificing peak shape. The response of the Hall @ detector in the halogen modewas roughly proportional to the number of chlorine atoms present, while the response of the Hall@ in the nitrogen mode and the NPD was less predictably influenced by the presence of one or more nitro groups. When combined with retention timedata, theratioof theNPD response to the Hall@ response has been found to substantiate the presence of chloro-and chloronitroanilines in sludge extracts.