Fe-57-Mossbauer spectroscopy is demonstrated to be a sensitive phase analysis tool for control of the ilmenite reduction process in a commercial rotary kiln. Knowledge of recoil-free fractions for each of the key Fe-bearing phases would further reduce the error of quantitative determination. In this case, the feed material is predominantly pseudorutile and rutile and the key phases are confirmed to evolve in two stages, namely the formation of ilmenite from pseudorutile (Fe3+ -> Fe2+) followed by the reduction of ilmenite into metallic iron and rutile (Fe2+ -> Fe) via ferrous pseudobrookite. (C) 2007 Elsevier B.V. All rights reserved.