This study was performed : 1) to establish the experimental analysis conditions for the sorption and desorption of toxic organic contaminants to/from the activated sludge, sediment, and clay, and 2) to determine the sorption and desorption equilibrium coefficients of some representative halogenated aliphatic compounds. Through the preliminary sorption test using Azo dye, a setting of quantitative experimental conditions to determine the sorption and desorption characteristics was decided as follows; equilibration time of 180 minutes, centrifuge for 15 minutes at 5000×g, and 500㎎/ℓ of TOC concentration. The sorption and desorption characteristics of halogenated aliphatic compounds onto activated sludge, sediment and clay could be described very well using the Freundlich isotherm. The preference of the average sorption capacity of the overall compounds showed in the sequence sediment 0.26㎎/g, clay 0.23㎎/g, and activated sludge 0.11㎎/g. The desorption rate of the sorbed compounds onto activated sludge, sediment and clay was approximately 89.8%, 35.3%, and 66.4%, respectively.