A tissue extraction procedure was developed which minimized loss of readily volatilizable compounds for subsequent quantification by headspace gas chromatography, and evaluated for perchloroethylene (PER), 1,1,1-trichloroethane, 1,1,2,2-tetrachloroethane, and 1,1,2-trichloroethylene. Of the procedures evaluated, joint isooctane and saline tissue homogenization had the most efficient recovery, ranging from 73 to 104% for the four halocarbons from seven different rat tissues. PER concentrations were also determined in tissues of rats following in vivo halocarbon administration. Recovery did not appear to be tissue-dependent, but did vary somewhat with test chemical, with the least volatile, most lipophilic compounds exhibiting the highest recovery.