These studies describe an efficient preparative method of separating and purifying polar mixtures of low molecular weight (mol wt) sulfonic acid derivatives containing one to six sulfonic acid moieties and possessing mol wt differences ranging from less than 100 and up to 650. This gel permeation chromatography procedure successfully separates materials with similar charges, requires no prepurification step, uses inexpensive apparatus, and employs water as the eluant. This technique has quantitative recovery and is potentially applicable to other anionic separations.