decane (photomirex), were discovered in the whole body lipid of Herring Gulls from Pigeon Island, Lake Ontario. PCBs, which were evident in high concentrations, coeluted with Mirex and photomirex in residue cleanup procedures, and interfered with their determination by electron-capture gas chromatography (EC-GC) using standard analytical columns. Samples were perchlorinated to remove this interference, and structures were confirmed by gas chromatography /mass spectrometry (GC/MS). The Hall electrolytic conductivity detector was shown to be useful as a specific detector to monitor residues of Mirex and photomirex in the presence of high PCB interference. Eggs of Herring Gulls proved to be useful as indicators of these compounds in Lake Ontario.