Abstract: A method was developed for the determination of total glycerine in biodiescl.The free glycerin was determined separatly after extraced.The sample was derivated for determination of bounded glycerin.Acapillary column of high temperatare tolerance was used for separation.The sample was detected by the flame ionization detector,without cool on-column injector .The internal standard method was used for quantification.The method can eliminate the interference of C10~C12 fatty acid methyl esters to free glycerin.Suitable content of free glycerin can be obtained by adjusting the amount of sample and extract reagent.The method is accurate.