The atomic variations occurring in cathode/electrolyte interface regions of La{sub 1-x}Sr{sub x}Co{sub y}Fe{sub 1-y}O{sub 3-?} (LSCF) cathodes and other SOFC related materials have been investigated and characterized using soft X-ray Absorption Spectroscopy (XAS) and diffuse soft X-ray Resonant Scattering (XRS). X-ray Absorption Spectroscopy in the soft X-ray region (soft XAS) is shown to be a sensitive technique to quantify the disruption that occurs and can be used to suggest a concrete mechanism for the degradation. For LSC, LSF, and LSCF films, a significant degradation mechanism is shown to be Sr out-diffusion. By using the XAS spectra of hexavalent Cr in SrCrO4 and trivalent Cr in Cr2O3, the driving factor for Sr segregation was identified to be the oxygen vacancy concentration at the anode and cathode side of of symmetric LSCF/GDC/LSCF heterostructures. This is direct evidence of vacancy induced cation diffusion and is shown to be a significant indicator of cathode/electrolyte interfacial degradation. X-ray absorption spectroscopy is used to identify the occupation of the A-sites and B-sites for LSC, LSF, and LSCF cathodes doped with other transition metals, including doping induced migration of Sr to the anti-site for Sr, a significant cathode degradation indicator. By using spatially resolved valence mapping of Co, a complete picture of the surface electrochemistry can be determined. This is especially important in identifying degradation phenomena where the degradation is spatially localized to the extremities of the electrochemistry and not the average. For samples that have electrochemical parameters that are measured to be spatially uniform, the Co valence modifications were correlated to the effects of current density, overpotential, and humidity.