A method is described for the determination of several pesticides containing bromine and chlorine by molecular emission cavity analysis (MECA). The pesticides were decomposed in an oxygen flask and the combustion products dissolved in aqueous ammonia. The ammonium halides were separated by TLC using microcrystalline cellulose adsorbent. After scraping from the TLC plates and dissolving in water the separated components were quantitated by MECA using either the InBr (Λmax= 376 nm) or the InCl (Λmax= 360 nm) emission bands. Recoveries of over 96% were obtained. Soils fortified with l, 2-dibromo-3-chloropropane at levels of 5–25 ppm were extracted using shaking and distillation procedures. Subsequent analysis showed that the shaking extraction gave a recovery of 92% compared to 85% from acid refluxing.