SPME device was applied to determine the THM in an aqueous solution. The 6 kinds of THM was quantitatively detemined by using GC-ECD which has the sample extracted on the SPME fiber from an aqueous solution for 10 min. The THM components were well separated from CHCl_3 to the last CHBr_3 within 13 mans at the condition. 6 kinds of the volatile halogenated organic compounds: CHCl_3, CHBrCl_2, CHBr_2Cl, CHCl_3, C_2Cl_4, and CHBr_3, showed well defined calibration graph with good linearity from a few ppb level up to several tens of ppb concentration. CHBr_2Cl and C_2Cl_4, were detected from a few samples among the 10 of river samples. CHCl_3, however, was detected in 4 sea water samples with the highest of 10 ppb among the polluted 6 positions. Trace level of CHBr_2Cl and few ppb level of CHBr_3 were also detected at the other two sample stations. Most of the 13 rain water samples collected from 6 sampling stations were contained ppb level of CHCl_3, and also CHBr_2Cl, and C_2Cl_4 were only detected at trace level at a few rain samples among them. We could recognize the fact that our air and water environment has already been contaminated by certain volatile halogenated organic compounds through this study.