Identification of the iron oxidation state and coordination geometry in iron oxide- and zeolite-based catalysts using pre-edge XAS analysis

Journal of Synchrotron Radiation
Alexey BoubnovJan Dierk Grunwaldt

Abstract

Analysis of the oxidation state and coordination geometry using pre-edge analysis is attractive for heterogeneous catalysis and materials science, especially for in situ and time-resolved studies or highly diluted systems. In the present study, focus is laid on iron-based catalysts. First a systematic investigation of the pre-edge region of the Fe K-edge using staurolite, FePO4, FeO and α-Fe2O3 as reference compounds for tetrahedral Fe(2+), tetrahedral Fe(3+), octahedral Fe(2+) and octahedral Fe(3+), respectively, is reported. In particular, high-resolution and conventional X-ray absorption spectra are compared, considering that in heterogeneous catalysis and material science a compromise between high-quality spectroscopic data acquisition and simultaneous analysis of functional properties is required. Results, which were obtained from reference spectra acquired with different resolution and quality, demonstrate that this analysis is also applicable to conventionally recorded pre-edge data. For this purpose, subtraction of the edge onset is preferentially carried out using an arctangent and a first-degree polynomial, independent of the resolution and quality of the data. For both standard and high-resolution data, multiplet ana...Continue Reading

References

Aug 22, 2001·Journal of Synchrotron Radiation·M Newville
May 15, 2003·Angewandte Chemie·Robert Schlögl
Jun 22, 2005·Journal of Synchrotron Radiation·B Ravel, M Newville
Nov 9, 2007·Chemical Communications : Chem Comm·Jan-Dierk GrunwaldtAlfons Baiker
Feb 25, 2011·Chemical Communications : Chem Comm·Houhuan DongWeiping Ding
Mar 11, 2009·Journal of Physics. Condensed Matter : an Institute of Physics Journal·Frank de GrootPieter Glatzel

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Citations

Apr 23, 2019·Geophysical Research Letters·E BoulardG Fiquet
Sep 19, 2019·Faraday Discussions·Anke SchochMatthias Bauer
Jul 28, 2021·Journal of the American Chemical Society·Matthew C SimonsAditya Bhan
Dec 30, 2020·The Journal of Physical Chemistry. a·Nicholas J AndersonMary Jane Shultz

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