Abstract:Objective: A gas chromatographic (GC) method for ethylene glycol and diethylene glycol determination in glycerol samples was established. Method: 6% cyanopropyl-phenyl and 94% dimethyl polysiloxane capillary column (DB-624) was used. The internal standard method with temperature-programmed mode was used for quantitative analysis. Result: The sample peak area and the internal standard peak area ratio to the concentration of samples for both the ethylene glycol and the diethylene glycol had a good linear relation in the range of 20.00-160.00 mg·L-1. The linear equation of ethylene glycol was YEG=0.004X-0.025 (r=0.999 8). The average recovery was 101.80% and RSD was 1.6% (n=9).The linear equation of diethylene glycol was YDEG=0.004 2X-0.045 7 (r=0.999 8). The average recovery was 98.95% and RSD was 1.9% (n=9). Conclusion: The method has a short peak retention time, which can be used for quality control of the glycerol.