Pentachlorophenol (PCP) is a herbicide, defoliant, and antimicrobic chemical used throughout the United States as a preservative agent for many products. The ubiquity of human exposure to this potentially dangerous compound has prompted concern in the field of public health. This interest has been stimulated by several recent industrial and public intoxications which resulted in fatalities. This report describes a simple and rapid method for the determination of PCP based upon its conversion to any one or more of seven possible alkyl ethers. PCP ethers are detected and quantitated by electron capture gas chromatography and their identity is confirmed by p-values. Data are presented for seven GLC columns and three p-value solvent systems.