This study demonstrated a full evaporation (FE) headspace gas chromatographic technique for the determination of residual monomer in methyl methacrylate (MMA) polymer latex. A very small amount (～10–30 mg) of latex was added to a sealed headspace sample vial (20ml). A near-complete monomer mass transfer from both liquid (aqueous phase) and solid phase (polymer particles) to the vapor phase (headspace) is achieved within 5min at a temperature of 110℃. The method eliminates sample pretreatment procedures such as the solvent extraction. Thus, it avoids the risk of polymer deposition on the GC system caused by a directly injection of extraction solvent in the conventional GC monomer analysis. The present method is simple, rapid, and accurate.