A simple, fast and accurate method has been develop ed for the determination of Benzene in Toluene by Gas Chromatography. The analysis was car ried out on Shimadzu GC-2010 Gas Chromatograph. The column used was 30mx 0.32 mm Id fused silica analytical column ZB-624, 1.80 μ m. (6% cyanopropylphenyl: 94% dimethylpolysiloxane as a stationary phase). The detector used was FID detector. The validation of p roposed method was also carried out.