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The principal gaseous carbon-containing components identified in the first 400 m of sediment at Deep Sea Drilling Project Site 533, Leg 76, are methane (CH4) and carbon dioxide (CO2). Below a sub-bottom depth of about 25 m, sediment cores commonly contained pockets caused by the expansion of gas upon core recovery. The carbon isotopic composition (d13C per mil relative to PDB standard) of CH4 and CO2 in these gas pockets has been measured, resulting in the following observations: (1) d13C-CH4 values increase with depth from approximately -94 per mil in the uppermost sediment to about -66 per mil in the deepest sediment, reflecting a systematic but nonlinear depletion of 12C with depth. (2) d13C-CO2 values also increase with depth of sediment from about -25 per mil to about -4 per mil, snowing a depletion of 12C that closely parallels the trend of the isotopic composition of CH4. The magnitude and parallel distribution of d13C values for both CH4 and CO2 are consistent with the concept that the formation of the CH4 resulted from the microbiological reduction of CO2 from organic substances. These results imply that CH4 and CO2 incorporated in gas hydrates at this site are biogenic.