The determination of chlorine, bromine and iodine present as non-polar, hydrophobic hydrocarbons in environmental samples is reported. The organohalogen compounds are seprated from water into an organic phase by on-site liquid-liquid extraction, and form biological material by procedures based on lipid phase extraction and codistillation. After removal of inorganic halides by washing with water and concentration of the sample by evaporation of the solvent, the resulting extracts are analyzed for their chlorine, bromine and iodine contents by instrumental neutron activation analysus. Strict attention is paid to the possibility of contamination in every step of the procedure. Background values in routine analysis are approximately 100-200 ng of chlorine, <5 ng of bromine and <3 ng of iodine.