Results are presented from a study of the preparation and characterization of Wyodak subbituminous coal impregnated with iron and iron-molybdenum salts by the incipient wetness (IW) technique. X-ray photoelectron spectroscopy (XPS) was used to examine the surface composition and chemistry of coals impregnated with 0.7-2.0 wt % Fe and 500-1000 ppmw Mo. Various salts were used in preparing the impregnated coals including ferric nitrate, ferric sulfate, ferrous sulfate, and ammonium molybdate. The surface concentration of Fe increased as the amount of added Fe increased, with higher concentrations being observed for the nitrate-impregnated coals. The anions of the impregnating salts were readily removed from the samples that were treated with ammonium hydroxide solution. For samples impregnated with sulfate salts, which were not treated with base, higher sulfur concentrations were observed on the surface of the coal. The Fe-2p32 and Fe-3p peak positions in the base treated coals correspond with alpha-FeOOH while the positions in the non-base-treated sulfate-impregnated coals are consistent with the Fe sulfate salts. The added Fe on the surface of the impregnated coals has a direct impact on the position of the O-1s peak shifting it to a lower energy position. Overlap of the Mo-3d doublet by the S-2s peak required deconvolution based upon peak positions in reference materials. The liquefaction performance of the impregnated samples is directly related to the amount of added Fe with THF conversion and oil yield increasing as Fe concentration on the surface increased. The liquefaction results with the Fe-Mo co-impregnated coals were better than the other coals prepared in this study.