A technique to determine a trace amount of hydrogen in carbon materials heat-treated above 1000°C was developed. Three types of carbons prepared from poly(furfulyl alcohol), poly(vinyl chloride) and mesophase carbon microbeads were heat-treated at various temperatures ranging from 1000 to 1800°C. Then they were gasified by O2 in a fixed bed flow reactor, and the H2O gases formed during the gasification processes were carefully monitored with a Karl Fischer moisture analyzer. As a result, this method makes it possible to determine the hydrogen contents in the carbons down to three places of decimals as a weight percent and can detect even a trace amount of hydrogen as low as 0.002wt.%. A possible chemical structure of carbon edge sites was also discussed based on the experimentally determined hydrogen contents.