The quantitative determination of chlorinated-insecticide residues in treated foodstuffs by total chlorine methods is expedited and simplified by the exploitation of an unusually sensitive direct potentiometric method for chloride ion. This method uses a pH meter and a silver-silver chloride vs. calomel electrode system, and responds reproducibly to as little as 0.02 p.p.m. of chloride ion. With the equipment and procedures recommended, the useful range, without concentration or dilution stages, appears to be from 0.02 p.p.m. to 10,000 p.p.m.