Empirical Identification of Uranium Oxides and Fluorides Using Electron Energy-loss Spectroscopy in the Transmission Electron Microscope.

: A set of uranium compound particles relevant to contaminated soils and other environmental concerns surrounding uranium bioavailability were studied by electron energy-loss spectroscopy (EELS). Core-loss EELS results suggest that uranium 4(+) compounds have an energy loss resolvable from 6(+) compounds. Shoulders on the uranium O(4,5) edge further distinguish UO(2) from UF(4). Low-loss characteristics distinguish carbon-free uranium oxide specimens on holey substrates. In the presence of carbon, correction techniques must be applied. Uranium oxides, fluorides, and minerals show a tendency toward reduction of uranium toward 4(+) under the beam. The electron dose required to achieve the transformation from 6(+) to 4(+) is more severe than that usually required to obtain satisfactory spectra, but the possibility for reduction should be considered. The conditions for low-loss analysis need not be as vigorous as those for core losses, and can be done without altering the valence of most oxides.