Major and minor acids present in dried leaf tissue of Bryophyllum calycinum were identified or characterized using the combined methods of ion exchange chromatography, paper and thin-layer chromatography, gas chromatography, and infrared spectroscopy. After esterification of the acids in methanol containing H+ form cation exchange resin, their amounts were determined by gas chromatography. The acids identified and their approximate percentage amounts of the total acid content were: malic 32.5%, citric 10.1%, isocitric 46.5%, succinic 1.0%, fumaric 0.9%, pyruvic 1.0%, oxalacetic 0.4%, α-ketoglutaric 0.5%, glyoxylic 0.1%, lactic 0.2%, oxalic 0.2%, and cis-aconitic 1.6%. Tentative characteristics were proposed for previously undetermined acids present mainly in amounts from 0.05% to 0.6%. These were apparently mono-, di-, and tricarboxylic acids containing from three to seven carbons in the carbon chain. Most of these evidently had additional functional groups, including methyl, keto, and hydroxyl groups. The boiling points of the methyl esters of these acids ranged from 140° to 300°.