Amino acids have appreciable vapor pressures above 150 degrees C and will sublime under partial vacuum at elevated temperatures without any racemization or decomposition. The recoveries of several amino acids including aspartic acid, serine, glycine, alanine, alpha-aminoisobutyric acid, and valine were optimized by varying the temperature and duration of sublimation. Sublimation has been shown to be a rapid and effective technique for the isolation of amino acids from natural samples for enantiomeric analyses and a good substitute for conventional cation-exchange desalting techniques.