An integrated analytical approach, which combines elemental [scanning elect
ron microscopy with energy-dispersive X-ray spectroscopy (SEM/EDS)] and mol
ecular (Raman) chemical imaging techniques, has been utilized for the chara
cterization of a residual phase of gallium in mixed oxide (MOX) surrogate m
aterial. Surrogate MOX materials are comprised of CeO2 in place of PuO2. In
real MOX materials, PuO2 is mixed with UO2 as a commercial fuel source. A
Ga phase remains in the surrogate sample following reductive heating experi
ments designed to explore the removal of gallium from weapons-grade plutoni
um. The SEM/EDS data reveal the concentration of Ga within the grain bounda
ries of the sample and a distribution of Ce and O throughout the sample mat
rix. Molecular analysis provided by Raman chemical matrix imaging correlate
s with the SEM/EDS elemental imaging results. Specifically, the Raman data
suggest that the matrix is comprised of CeO2 and grain boundaries are a mix
ed phase comprised of CeO2 with a form of Ga, most likely a CeGaO3 perovski
te phase ha,iug a cubic structure.