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Gadolinium, and possibly praseodymium, are relatively enriched in the magnetic fractions of Class F fly ashes from Central Appalachian coal sources. Although the enrichment is evident in the inductively coupled plasma–atomic emission spectroscopy (ICP-AES) determinations of the rare earth content, transmission electron microscopy–energy dispersive x-ray spectroscopy (TEM-EDS) examination of the fly ash fails to show the sites of the Gd or Pr. This apparent lack of correlation could be due to the inability of the EDS to detect low concentrations of the rare earth elements definitively; interferences in the analytics, leading to false positives in the chemical analysis; or the overlap of the energies of Gd and/or Pr with more abundant elements, leading to inaccurate negative results.