Determinations of low atomic number elements in real uranium oxide samples using vacuum chamber total reflection x‐ray fluorescence

Conditions for the total reflection x‐ray fluorescence (TXRF) analysis of real uranium samples for low atomic number elements using vacuum chamber TXRF spectrometer were optimized. It was observed that for analysis of low atomic number elements, almost complete removal of uranium matrix is required. Two certified reference materials of uranium containing trace elements in different concentrations were dissolved in minimum amount of high purity nitric acid. The uranium matrix from these solutions was separated by solvent extraction using tri‐n‐butyl phosphate as extracting reagent. Low atomic number elements in TXRF spectrum of the aqueous phase could be seen only after six tri‐n‐butyl phosphate equilibrations in extraction. The TXRF determinations of the certified low atomic number elements Mg and Al were made in these aqueous solutions after addition of Sc as an internal standard. The TXRF determined values for Mg were in good agreement with the certified values, whereas TXRF determined Al values differed from the certified values appreciably, probably due to the interference of Al Kα peak with escape peak of U Mα and the neighboring Si Kα peak. Copyright © 2013 John Wiley & Sons, Ltd.