Abstract: Perdeuterated acetaldehyde is one of the intermediates for the synthesis of perdeuterated polystyrene which is the material of inertial confinement fusion (ICF) solid targets. Calcium carbide and heavy water are used as the main reactants, through a series of liquid solid and gas liquid reactions, perdeuterated acetaldehyde (the deuterium isotopic content is more than 99 %) has been synthesized. This paper describes the synthesis procedures and deuterium isotopic content characterization method,some of the process parameters have been discussed also.