Microextraction has been developed for extracting trace polynuclear aromatic hydrocarbons (PAHs), i.e., acenaphthene, fluorene, phenanthrene, flouranthene and pyrene from water samples prior to the determination by gas chromatograph equipped with flame ionization detector (FID). The factors having the effect on % recovery, i.e., the extracting solvents, e.g., carbon disulfide, cyclohexane and methylene chloride, the sample to solvent ratios, e.g., 9:1, 5:5 and 2:8 and the salting out with sodium chloride and sodium sulfate were studied. The carbon disulfide, the sample to solvent ratio of 9:1 and salting out with sodium sulfate should be considered as suitable combination for microextraction of PAHs in water samples. The % recoveries obtained from this study ranged from 96.62-104.88% with % RSD 0.58-6.78%. The accuracy of this technique was studied and the results of % errors of PAHs were in the ranges of 0.22-1.72%. The aqueous samples contained as low as 20 ppb of these PAHs could be easily determined.