A high energy resolution x-ray absorption near-edge structure ͑XANES͒ spectroscopy study on U 4+ ͑UO 2 ͒, U 5+ ͓͑UO 2 Py 5 ͔͓KI 2 Py 2 ͔͒, and U 6+ ͓UO 2 ͑NO 3 ͒ 2 ͑H 2 O͒ 6 ͔ demonstrates the potential of this experimental technique for qualitative/semiqualitative and quantitative actinide speciation investigations. We observe a pre-edge feature with quadrupole nature in a U L 3 edge partial fluorescence yield-XANES spectrum. This feature is a tool for characterizing the participation of 5f orbitals in U-O bonding. The feature origin is explained by performing calculations with the finite difference method near-edge structure code based on the multiplescattering theory and the finite difference method.
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