Since the 1920's, there has been interest in determining polythionates in solution. The reaction of h2s with so2 in solution yields Wackenroder's Solution, which contains s2o3--, s3o6--, and s5o6--, but no other polythionates or s2o6--. Many methods have been developed for determining polythionates contained in this mixture, but there is no satisfactory way of separating and quantifying them that is not lengthy and time consuming. Because the time involved in these separations is long, the stability of the polythionates from the beginning to the end of analysis is in doubt. The method described in this paper will separate and quantify the above named polythionates in 15 minutes. The method depends on the adsorption and elution from activated carbon by high-speed liquid chromatography. The factors governing the separation are described.