The present invention discloses a preparation apparatus and an oxidative combustion method of an organic tritium carbon sample. The preparation apparatus comprises a reaction working pipe, an oxidative combustion furnace and an absorption device, wherein the reaction working pipe comprises a pipe body, a first gas inlet hole, a second gas inlet hole and a gas outlet hole, a heating zone is arranged in the oxidative combustion furnace and is sequentially divided into a catalytic reaction zone, a sample stacking zone and a sample recovery zone, the lower portions are respectively provided with a temperature controller, the reaction working pipe is horizontally arranged in the oxidative combustion furnace, the pipe body penetrates through the heating zone, the gas outlet hole is connected to the absorption device, the absorption device comprises a collection bottle and a low temperature cold trap, the collection bottle is arranged in the low temperature cold trap, and the gas outlet hole is connected to the collection bottle. According to the present invention, the structure is simple, the problems of open fire production caused by combustion, quartz pipe bursting, incomplete sample combustion and the like during the sample treatment process are effectively prevented, the generated water has the clear color, the sample treatment capacity is high, the sample absorption rate of the combustible materials such as tritium and carbon-14 is substantially improved, and the sample measurement requirements in the modern industry are met.