Db. Hunter et Pm. Bertsch, IN-SITU EXAMINATION OF URANIUM CONTAMINATED SOIL PARTICLES BY MICRO-X-RAY ABSORPTION AND MICRO-FLUORESCENCE SPECTROSCOPIES, Journal of radioanalytical and nuclear chemistry, 234(1-2), 1998, pp. 237-242
Two complimentary spectroscopic techniques, X-ray absorption and fluor
escence spectroscopy have been conducted at spatial scales of 1 to 25
mu m on uranium contaminated soil sediments collected from two former
nuclear materials processing facilities of the DOE: Fernald, OH and Sa
vannah River Site, SC. A method of imbedding particles in a non-reacti
ve Si polymer was developed such that individual particles could be ex
amined before and after extraction with a wide range of chemicals typi
cally used in sequential extraction techniques and others proposed for
ex situ chemical intervention technologies. Using both the micro-X-ra
y fluorescence (XRF) and micro-X-ray Absorption Near Edge Structure (X
ANES) techniques, both elemental and oxidation state distribution maps
were generated on individual particles before and following chemical
extraction. XANES can determine the relative proportion of U(VI) and U
(IV) in phases comprising individual particles before and after extrac
tion and showed that greater than 85% of the uranium existed as hexava
lent U(VI). Fluorescence spectra of contaminated particles containing
mainly U(VI) revealed populations of uranyl hydroxide phases and demon
strated the relative efficacy and specificity of each extraction metho
d. Correlation of XAS and fluorescence data at micron scales provides
information of U oxidation state as well as chemical form in heterogen
eous samples.