Experiments were made to investigate the effect of temperature on the hydrolysis reaction in aqueous 6 N HCl with a view to developing a rapid hydrolysis procedure. The maximum yield for all of the protein amino acids was obtained at 145° ± 2° for the minimal time of 4 h. Essentially equivalent hydrolysis of ribonuclease was achieved at the two different hydrolysis conditions, i.e., 110° ± 1° for 26 h, or 145° ± 2° for 4 h. The yields obtained were in good agreement.