AbstractHeating of intact cassava leaves causes liberation of hydrogen cyanide. This phenomenon appears to be caused by β‐glucosidase‐catalysed decomposition of the cyanogenic glycosides linamarin and lotaustralin. Because of these losses, many previously determined values for total nitrogen in cassava (and other cyanogenic plants) are probably in error as plant materials used for Kjeldahl determinations are often dried at 70–90°C. Liberation of cyanide from intact cassava leaves by heating at 80°C is more complete than liberation by the homogenisation methods commonly used. Homogenisation of cassava leaf tissues with liquid nitrogen or dry ice gives somewhat lower values, and these materials are often not readily available in areas where cassava is studied. The basis of a relatively simple procedure for the isolation of hydrogen cyanide from cassava leaves is suggested.