Moessbauer spectroscopy has been proven to be a valuable tool in physical metallurgy. The Moessbauer effect has been successfully applied in the qualitative and quantitative identification of various alloying phases, the determination of the solid-solution limit, the study of martensite transformation, precipitation, texture and amorphous alloys. Phase formation in rapidly solidified Al-Fe alloys has been extensively investigated by using Moessbauer spectroscopy in the past years. The phases, such as the solid solution of Fe in Al, the metastable Al[sub 6]Fe as well as the stable Al[sub 13]Fe[sub 4], have been identified. The Moessbauer parameters of these phases have also been well established. In mechanically alloyed Al-Fe alloys, the Moessbauer effect was successfully employed to study the formation of amorphous structures. There are very few reports in the literature of Moessbauer studies of the solid-state reactions in mechanically alloyed Fe-containing Al alloys. In the present work, the solid-state reactions occurring in mechanically alloyed Al-Fe and Al-Fe-Mn powders are analyzed and characterized by Moessbauer spectroscopy.