Sulfur Speciation in Biochars by Very High Resolution Benchtop Kα X-ray Emission Spectroscopy

The Journal of Physical Chemistry. a
William M HoldenSingfoong Cheah

Abstract

The analytical chemistry of sulfur-containing materials poses substantial technical challenges, especially due to the limitations of 33S NMR and the time-intensive preparations required for wet-chemistry analyses. A number of prior studies have found that synchrotron-based X-ray absorption near edge structure (XANES) measurements can give detailed speciation of sulfur chemistry in such cases. However, due to the obvious access limitations, synchrotron XANES of sulfur cannot be part of routine analytical practice across the chemical sciences community. Here, in a study of the sulfur chemistry in biochars, we compare and contrast the chemical inferences available from synchrotron XANES with that given by benchtop, extremely high resolution wavelength-dispersive X-ray fluorescence (WD-XRF) spectroscopy, also often called X-ray emission spectroscopy (XES). While the XANES spectra have higher total information content, often giving differentiation between different moieties having the same oxidation state, the lower sensitivity of the S Kα XES to coordination and local structure provides pragmatic benefit for the more limited goal of quantifying the S oxidation state distribution. Within that constrained metric, we find good agreeme...Continue Reading

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Citations

Oct 4, 2018·The Review of Scientific Instruments·William M HoldenAnthony D DiChiara
Mar 11, 2020·Journal of Synchrotron Radiation·Alexander S DitterGerald T Seidler

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