PCBs have been measured using GC-ECD, GC-MS, GC-ELCD, HPLC, TLC, NMR and Immunoassay. The analysis of PCBs using GC- ECD include the peak pattern method as none derivatization and the perchlorination method as derivatization. This study was conducted to establish the perchlorination method with SbCl_5 from PCBs to decachlorinated biphenyl(DCB). The aroclor 1242 of PCBs was chlorinated and then, converted into the DCB which showed a single peak in GC-ECD chromatogram. The detection limit of DCB was 2pg. The quantification detection concentration of PCBs extracted with soxhlet was 0.5ng/g in the soil. PCBs were not detected in the suburban soil, but 174ng/g in the soil of industrial complex. Mean PCBs concentration of Shinchun stream at Kumho river and Jinchun stream at Nakdong river was calculated average 88ng/g in the sediment. PCBs concentration in the sediment of Kumho river near 2-7㎞ from conjunction with Nakdong river was average 154ng/g. PCBs concentration in the sediment of Nakdong river near conjunction with Kumho river was average 159ng/g.