Abstract: Waste water sample was treated by self-made biphenyl-molecularly imprinted polymers, and GC was applied to the determination of biphenyl and 3,3-dichlorobiphenyl in the sample solution. The analytes were separated on ZB-624 capillary column (30 m×0.25 mm, 0.25 μm) and detected by FID. Linear relationships between values of peak area and mass concentration of biphenyl and 3,3-dichlorobiphenyl were kept in the same range of 0.20-20 mg·L-1, with detection limits (3S/N) of 20.0, 35.0 μg·L-1 respectively. Recovery of the method was tested by standard addition method, and values of recovery and RSD′s (n=5) found were in the ranges of 91.2%-98.5% and 4.7%-5.9% respectively.