In the field of air pollution, awareness of the pollution potential of vehicular exhaust has resulted in studies aimed at measuring levels of exhaust components. Since excessive exposure to lead has long been recognized as a serious public health problem, a significant portion of this work is directed currently toward the measurement of lead concentrations in urban atmospheres. A variety of chemical procedures are available for the determination of lead. A need was recognized for an evaluation of methods now in use in terms of accuracy and precision. This study was therefore undertaken to provide such comparative information to those who have responsibilities or interest in the measurement of lead in the atmosphere.