A procedure has been developed for the speciation of aluminum in urine samples of four normal subjects fed required diet on two dates. Three fractions of aluminum species, i.e., labile monomeric ions, non-labile monomeric ions along with labile complexes, and non-labile complexes were classified and determined by the combination of ion-exchange (IE), fluorometric spectrometry and graphite-furnace atomic absorption spectrometry (GF-AAS) techniques. The results showed that the aluminum in urine was mainly in non-labile complex forms.