ShimCap-InoWax capillary column and FID hydrogen flame ionization detector were used to separate and detect the components of heavy diol.By setting chromatographic conditions,various alcohol components were successfully separated and good detection results were obtained.The heavy diol actually produced by Yulin Chemical Co.,Ltd.was compared with the customer sample.The results showed that under the selected chromatographic conditions,the mass concentration of heavy diol had a good linear relationship with the measurement results,and the measurement range was 0~100.003%.The diethylene glycol and triethylene glycol components also showed a good linear relationship,and the measurement ranges were 0~3.10%and 0~0.03%respectively.The relative standard deviation was less than 2%,meeting the requirements.The recovery rate of heavy diol was 99.78%~100.05%,and the coefficient of variation was 0.44%.The recoveries of diethylene glycol and triethylene glycol were 99.48%~100.11%and 98.13%~100.96%respectively,and the coefficients of variation were 1.07%and 0.75%respectively.The relative error of the two samples was less than 4%,and the results were reliable.