||Some of the priority pollutants, e.g., aromatic hydrocarbons, halogenated aromatic hydrocarbons and halogenated alkanes and alkenes have been studied by a microextraction technique. The compounds studied were benzene, toluene, and ethylbenzene for aromatic hydrocarbons; chlorobenzene, m-dichlorobenzene, p-dichlorobenzene, and o-dichlorobenzene for halogenated aromatic hydrocarbons; and trans-1,2-dichloroethylene, 1,1-dichloroethane, 1,1,2,2-tetrachloroethane, chloroform, ethylene chloride, 1,1,1-trichloroethane, carbon tetrachloride, methylene chloride, bromodichloromethane, 1,2-dichloropropane, trichloroethylene and bromoform for halogenated alkanes and alkenes. The organic solvent-to-water sample ratios of study were 1:9, 5:5 and 8:2, respectively. Solvent extractability effect of carbon disulfide, methylene chloride and hexane or iso-octane and the effect of salts, e.g., saturated sodium chloride solution, saturated sodium sulfate solution, 2.00 g of sodium chloride and 2.00 g of sodium sulfate on the percent recovery were investigated in this study. This technique is based on the extraction into an organic solvent phase followed by the measurement of the peak area by a flame ionization detector. Gas chromatography and the internal standard technique were used throughout the study. The gas chromatographic conditions for each system of study were reported. The standard deviation of this study ranged from 1-16%. The distribution constant, K(,D), and the results of percent recovery for each compound are discussed.