Issue 5, 2023

A laboratory X-ray emission spectrometer for phosphorus Kα and Kβ study of air-sensitive samples

Abstract

The analytical chemistry of phosphorus-containing materials is often impeded by the long measurement times and relatively large sample masses needed for 31P NMR spectroscopy, by the scarcity and access limitations of synchrotron beamlines operating in the energy range of the P K-edge, by the challenges posed by species interconversion during liquid extraction, and by the considerable air-sensitivity typical of many phosphorus-containing materials and nanophases. To this end, we report the design and operation of a new laboratory-based spectrometer to simultaneously perform P Kα and Kβ X-ray emission spectroscopy (XES) while being housed in a research-grade controlled-atmosphere glovebox. Demonstration studies on nickel phosphide nanophases illustrate the importance of air-free XES and the value of simultaneous Kα and Kβ spectroscopy for identifying the P oxidation state and for investigating nanoscale influences on valence level electronic structures.

Graphical abstract: A laboratory X-ray emission spectrometer for phosphorus Kα and Kβ study of air-sensitive samples

Supplementary files

Article information

Article type
Paper
Submitted
21 feb 2023
Accepted
05 apr 2023
First published
06 apr 2023

J. Anal. At. Spectrom., 2023,38, 1125-1134

Author version available

A laboratory X-ray emission spectrometer for phosphorus Kα and Kβ study of air-sensitive samples

J. E. Abramson, W. M. Holden, R. A. Rivera-Maldonado, A. Velian, B. M. Cossairt and G. T. Seidler, J. Anal. At. Spectrom., 2023, 38, 1125 DOI: 10.1039/D3JA00053B

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