SummaryCombination of various GC detectors by using a Varian effluent splitter with glass capillatycolumns has been found to be a rapid procedure for profiling organicsextractedfromsludgesand river sediments. The selectivity and the increased sensitivity of the thermionic nitrogen-phosphorus detector (TSD), the electron capture detector (ECD), and the flame photometric detector (FPD) over the flame ionization detectors (FID) or mass spectrometersallow the detection of compounds present at trace levels without need for extensive sample cleanup. Furthermore, the combination of two selective detectors may supplement the information with regard to the chemical functionalities required for structure elucidation.