Abstract: Glycerol carbonate and residual glycerin in the crude product of glycerol carbonate were determined by GC with HP 1701 capillary column. Gradient elevation of column temperature and using of tetraethylene glycol as internal standard were adopted in the analysis. Clear separation between glycerol carbonate and glycerin was attained under the optimized conditions. Linearity ranges of glycerol carbonate and glycerin were kept in the ranges of 23.30-116.6 g·L-1 and 3.70-18.40 g·L-1. Values of recovery and RSD′s (n=6) found were in the ranges of 99.1%-100.9% and 0.61%-1.93%, respectively.