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SUMMARY— Organic acids precipitated as lead salts from water extracts of cocoa beans were converted to trimethylsilyl ethers. TMS ethers were then separated and identified using a combined gas chromatograph-mass spectrometer. Citric, phosphoric, lactic, oxalic, malic, tartaric, succinic and gluconic acids were present in every sample examined, irrespective of geographic origin. Five of the acids were quantitated using a GLC procedure which involved the preparation of methyl esters from freeze-dehydrated, water extracts. Concentration ranges found, g/100g beans, were: lactic, 0.11–0.71; oxalic, 0.24–0.43; succinic, 0.02–0.07; malic, 0.02–0.10; citric, 0.56–1.32. Concentrations of lactic acid were lowest and citric acid levels tended to be highest in commercial samples from countries where cocoa beans usually are not subjected to a planned fermentation. These trends were confirmed in an experiment involving beans from Trinidad which had undergone a carefully controlled fermentation. Only minor differences were found in organic acid concentrations between roasted and unroasted cocoa beans.