1. An attempt to determine small quantities of iron by reduction with silver followed by titration with eerie sulfate revealed an error attributable to the formation of hydrogen peroxide in the reductor. 2. By conducting the reduction in an atmosphere of hydrogen, thereby decreasing the reductor correction, and applying a correction for the indicator, it was possible to determine quantities of iron of the order of 1.5 mg. with a high degree of accuracy. 3. The method was found to be relatively rapid and not to require the use of large platinum dishes, thus possessing advantages of practical value.