Abstract: Sixteen polycyclic aromatic hydrocarbons (PAH′s) were separated from water sediment by ultrasonic extraction with CH2Cl2, and the extract was purified and concentrated to about 0.5 mL. Rtx-5MS capillary column was used for separation. The identification of the 16 PAH′s was performed by comparing spectra obtained by MS detector with NIST05 atlas database; and quantification was performed by GC using external standard method with hydrogen flame ionization detector (FID). Values of detection limit (3S/N) of the method found were in the range of 0.27-6.0 μg·kg-1. Values of recovery found by the standard addition method, were ranged from 56% to 96% with RSD′s (n=5) ranged from 1.2% to 8.3%.