Solid energy calibration standards for P K-edge XANES: electronic structure analysis of PPh4 Br

Journal of Synchrotron Radiation
Anastasia V BlakeScott R Daly

Abstract

P K-edge X-ray absorption near-edge structure (XANES) spectroscopy is a powerful method for analyzing the electronic structure of organic and inorganic phosphorus compounds. Like all XANES experiments, P K-edge XANES requires well defined and readily accessible calibration standards for energy referencing so that spectra collected at different beamlines or under different conditions can be compared. This is especially true for ligand K-edge X-ray absorption spectroscopy, which has well established energy calibration standards for Cl (Cs2CuCl4) and S (Na2S2O3·5H2O), but not neighboring P. This paper presents a review of common P K-edge XANES energy calibration standards and analysis of PPh4Br as a potential alternative. The P K-edge XANES region of commercially available PPh4Br revealed a single, highly resolved pre-edge feature with a maximum at 2146.96 eV. PPh4Br also showed no evidence of photodecomposition when repeatedly scanned over the course of several days. In contrast, we found that PPh3 rapidly decomposes under identical conditions. Density functional theory calculations performed on PPh3 and PPh4+ revealed large differences in the molecular orbital energies that were ascribed to differences in the phosphorus oxidatio...Continue Reading

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Citations

Sep 17, 2020·Dalton Transactions : an International Journal of Inorganic Chemistry·Nicholas A PhillipsStefan G Minasian
Apr 7, 2019·Journal of Colloid and Interface Science·Annaleise R KleinLudmilla Aristilde

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