The recent discovery of the pollution of the environment with Kepone has resulted in a tremendous interest in the development of residue methodology for the compound. Current multiresidue methods for the determination of the common organochlorinated pesticides do not yield good quantitative analytical results for Kepone. The extracting solvents are usually of insufficient polarity to extract Kepone from the various media. This article describes some of the recently developed methodology for Kepone in air filters, finfish, finfish livers and entrails, shellfish, and archival oyster samples. The finfish and archival oyster samples were Soxhlet extracted using diethyl ether/petroleum and ether (1:1 v/v) as the extracting solvent. The finfish livers and entrails were macerated in a Duall tissue grinder containing acetonitrile followed by partitioning of the Kepone into benzene. Shellfish samples were analyzed after extracting the sample with acetonitrile and partitioning the Kepone into benzene. The Hi-Vol air samples were extracted with methanol/benzene (1:1 v/v). The coextracting contaminants were removed by micro-Florisil column chromatography and/or acid digestion. The procedural recovery of Kepone from fortified samples averaged 82%.