Two pyrolysis/microcoulometric titration methods for the determination of extractable organic halides in soils and oily waste are described. The first method involves the washing of soil sample in a column packed with granular activated carbon with a dilute nitrate solution to remove interfering inorganic halides. The organic halides are subsequently determined by pyrolysis/microcoulometric titration of the sample soil-activated carbon mixture. The second method involves the extraction of soil or oily waste samples with a mixture of octanol and 1 M sulfuric acid. The organic halides are extracted into the octanol phase and then analyzed by pyrolysis/microcoulometry. The inorganic halides are removed by extraction into the aqueous phase. The second method has the advantage of extending the technique to the analysis of a broader spectrum of organic halides including polar compounds such as chloroacetic acid