Abstract;A solid phase extraction-GC/MS method was applied to determination of N,N-dimethylformamide(DMF) in water and sediment. Five hundred milliliters of water samples, spiked with DMF-d7, are passed through a C18 cartridge and two active carbon cartridges in series. DMF absorbed on the active carbon cartridges is eluted with 3ml of methanol. The eluate is concentrated to 0.5ml and then added 4.5ml of ethyl acetate. After dehydration with anhydrous sodium sulfate, the eluent is concentrated to 1ml and determined by GC/MS. Sediment samples are spiked with DMF-d7 and extracted three times by 20ml portions of purified water. The subsequent procedure is the same as water samples. The overall recoveries were 88.5% to 112% from water samples and 94.5% from sediment samples. The detection limits were 0.065.MU.g/l in water samples and 1.9.MU.g/kg in sediment samples. (author abst.)