A m ethod is described for d etermi nin g s mall a mounts of a luminum (0.01 to 0.3 percent) in tainless a nd carbon s teels. A p erchlorie-sulfmic acid solution of th e steel is electrolyzed ill a m ercury catll ode cell to remov e most of the iroll , and an extraction with chloro form is m ade to remove elements such as alumi num, residu al iron , a nd titan iu m a s cupferrates from a solut. ion buffered at pH 3.5. These elements are conv erted from cupferrate to perchlorates; a ll excep t aluminum are t hen extracted as cupferrates with chloroform from 4 N hydrochlori c acid . Aluminum in t he acid solution is d eter.min ecl photo met ricall y wi t h a luminon (ammonium a urintricarboxylate) at a wave leng t h of approximately 540 millimicrons. An acc uracy of ± 0.005 percent a luminum is indi catecl .