A procedure has been devised for the isolation of dicoumarol from spoiled sweetclover (Melilotus alba). Using this procedure a method has been developed for the quantitative determination of dicoumarol in sweetclover, which involves an isotope dilution technique, and utilizes methylene-14C-dicoumarol. A colorimetric method for dicoumarol measurement has also been studied, which although not quantitatively reliable, provides a rapid qualitative determination of whether or not spoilage has rendered sweetclover hay unsafe for use as fodder. The results of analyses of a variety of forage samples are reported and discussed.