The structure of a series of Fe/Al2O3 catalysts containing from 1 to 24 weight percent iron has been examined by XRD, EXAFS, Mössbauer, ESCA, and gravimetric analysis. Two iron phases, Fe2O3 and Fe+3 in solid solution in the alumina support, are characterized as a function of iron loading. The combination of ESCA H2 titration and gravimetric analysis allows both quantitative and qualitative measurement of the two species. The amount of Fe2O3 phase increases with increasing iron loading for Fe1 to Fe24, whereas the amount of Fe+3 solid-solution phase increases with increasing iron loading for Fe1 to Fe6 and then levels off to approximately 2.2 wt % Fe for Fe8 to Fe24. The particle size of the Fe2O3 phase, determined from ESCA measurements, increases with increasing iron loading.
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