A kinetic method of analysis is outlined for the determination of two-component mixtures of ethane-diol, propane-1,2-diol and butane-2,3-diol, based on the measurement of reaction rates with lead tetraacetate in acetic acid solution. The method is of limited application only for ethane- and propane-diol mixtures but should prove useful for the analysis of butane-diol/propane-diol and butanediol/ethane-diol systems, the lower limit of concentration ratio being 1:100 and 1:1000 respectively.