A scanning electron microscope is used to investigate techniques for performing microanalysis of highly radioactive material from the Three Mile Island Unit 2 reactor. Wavelength dispersive X-ray (WDX) spectrometer methods allow quantitative analysis of metallic and oxide phases in samples with radiation fields of up to 60 R/h (contact β-γ). It is found that sputtered gold provides an unexpectedly useful specimen coating for remote analysis, being easily applied and forming more uniform layers than evaporated carbon, and proving compatible with quantitative point analysis. Through a combination of electron imaging, shielded energy dispersive spectrometry, WDX dot mapping, and quantitative WDX point analysis, it is possible to obtain data on core metal oxidation, trace concentration fission product distribution, and phase composition for core temperature estimation.