It has been acknowledged by WHO that styrene is a carcinogen which does great harm to human’s health and natural environment. In recent years, given the frequency of the leakage accidents of styrene that has given rise to potential safety hazard to drinking water, the fast detection of styrene pollutant in water and treatment of accidental release are of great significance for supplying safe drinking water. Total scanning fluorescence technique was used to unravel the 3D fluorescence feature of styrene by scanning its aqueous solution. A distinct fluorescence peak of styrene located at Ex255/Em305 was detected. There was a significant linear correlation between the concentration of styrene and the value of fluorescence peak, the correlation index being 0.995 7. The color of the fluorescence peak got darker with the raise of styrene concentration. There were four conjugated double bonds existing in the structure of styrene, among which a cyclic hydrocarbon with a continuous pi bond exists in benzene ring, the other one is in vinyl. All carbon atoms that makes up the structure of styrene were in the same plane, thus styrene molecules were completely planar with certain rigidity, which is the feature of fluorescent substances. Therefore, the concentration of styrene and the pollution of water by the leakage of styrene could be easily detected with the 3D fluorescence spectra. Powdered activated carbon (PAC) had a good effect on the absorption of styrene dissolved in water. Adding PAC(180 mesh) at a dosage of 15 mg·L-1 into source water with the concentration of styrene was 0.02 mg·L-1, which is the limited value in sanitary standard for drinking water, the concentration could be reduced to 0.001 mg·L-1 and the removal rate of styrene was as high as 95.5% .