Abstract: GC method was applied to determine acidolysis hydrecarbond in high carbonate soil samples. 10 g of sample was mixed with acid and was then degassed for 35 min. Acidolysis hydrocarbons were collected, separated by HP-PLOT capillary column, and detected with FID. The detection limits (3σ) were in the range of 0.007-0.715 μL·kg-1 and RSD were all less than 10%. The method was applied to analyze the standard sample consisting of standard gas, with relative error between measured values and certified values less than 5%.