A 47-year-old man was found dead in a factory where dichloromethane (DCM) tanks were stocked. He was making an inventory of the annual stock of DCM contained in several tanks (5- to 8000-L capacity) by transferring the solvent into an additional tank with the help of compressed air. During this operation, one of the tanks overflowed and the man, who was not wearing any protection, was intoxicated. Autopsy showed digestive, suprarenal, and liver bleeding. Blood was also found in the trachea. DCM was identified by headspace gas chromatography-mass spectrometry (GC-MS). A headspace gas chromatography-flame ionization detection technique (GC-HS-FID) optimized for quantitation in biological fluids, organs and viscera was established at autopsy. The following concentrations of DCM were found: blood (150 mg/L), urine (2.0 mg/L), gastric content (5.6 mg/L), brain (122 mg/kg), fat (99 mg/kg), liver (44 mg/kg), lung (20 mg/kg), and kidney (15 mg/kg). A study of the storage stability of DCM was carried out on these samples. Ethanol production was measured in some organs. The results are discussed in light of the rarity of existing literature.