Ethyl chloroacetate (EGA) is a valuable chemical used in the preparation of crop protection agents and pharmaceutical intermediates. It is generally prepared by the reaction of monochloroacetic acid(MCA) and ethanol. Selective, accurate and rapid analytical methods are essential for monitoring the reaction pathway and quantitative estimation of the products during the process development of EGA. A gas chromatographic (GC) method has been developed for the separation and quantitative determination of carbontetrachloride, ethanol, water and ECA using pentyl acetate as an internal standard. The method has been successfully applied for the determination of the components of reaction mixtures of EGA.