We describe a new technique for sample preparation, accelerated solvent extraction (ASE), that combines elevated temperatures and pressures with liquid solvents. The effects of various operational parameters (i.e., temperature, pressure, and volume of solvent used) on the performance of ASE were investigated. The solvents used are those normally used for standard liquid extraction techniques like Soxhlet or sonication. We found the recoveries of polycyclic aromatic hydrocarbons, polychlorinated biphenyls, and total petroleum hydrocarbons from reference materials using ASE to be quantitative. The extraction time for 1-30-g samples is less than 15 min, and the volume of solvent is 1.2-1.5 times that of the extraction cell containing the sample. No evidence was seen for thermal degradation during the extraction of temperature-sensitive compounds.