Improved precision in As speciation analysis with HERFD-XANES at the As K -edge: the case of As speciation in mine waste

Saurette, Emily M.; Frinfrock, Y. Zou; Verbuyst, Brent; Blowes, David W.; McBeth, Joyce M.; Ptacek, Carol J.

doi:10.1107/S1600577522007068

Title: Improved precision in As speciation analysis with HERFD-XANES at the As K -edge: the case of As speciation in mine waste

Journal Article · Thu Aug 11 00:00:00 EDT 2022 · Journal of Synchrotron Radiation (Online)

DOI:https://doi.org/10.1107/S1600577522007068· OSTI ID:1881046

; Frinfrock, Y. Zou; Verbuyst, Brent; Blowes, David W.; McBeth, Joyce M.; Ptacek, Carol J.

High-energy-resolution fluorescence-detected (HERFD) X-ray absorption near-edge spectroscopy (XANES) is a spectroscopic method that allows for increased spectral feature resolution, and greater selectivity to decrease complex matrix effects compared with conventional XANES. XANES is an ideal tool for speciation of elements in solid-phase environmental samples. Accurate speciation of As in mine waste materials is important for understanding the mobility and toxicity of As in near-surface environments. In this study, linear combination fitting (LCF) was performed on synthetic spectra generated from mixtures of eight measured reference compounds for both HERFD-XANES and transmission-detected XANES to evaluate the improvement in quantitative speciation with HERFD-XANES spectra. The reference compounds arsenolite (As ₂ O ₃ ), orpiment (As ₂ S ₃ ), getchellite (AsSbS ₃ ), arsenopyrite (FeAsS), kaňkite (FeAsO ₄ ·3.5H ₂ O), scorodite (FeAsO ₄ ·2H ₂ O), sodium arsenate (Na ₃ AsO ₄ ), and realgar (As ₄ S ₄ ) were selected for their importance in mine waste systems. Statistical methods of principal component analysis and target transformation were employed to determine whether HERFD improves identification of the components in a dataset of mixtures of reference compounds. LCF was performed on HERFD- and total fluorescence yield (TFY)-XANES spectra collected from mine waste samples. Arsenopyrite, arsenolite, orpiment, and sodium arsenate were more accurately identified in the synthetic HERFD-XANES spectra compared with the transmission-XANES spectra. In mine waste samples containing arsenopyrite and either scorodite or kaňkite, LCF with HERFD-XANES measurements resulted in fits with smaller R -factors than concurrently collected TFY measurements. The improved accuracy of HERFD-XANES analysis may provide enhanced delineation of As phases controlling biogeochemical reactions in mine wastes, contaminated soils, and remediation systems.

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Research Organization:: Argonne National Laboratory (ANL), Argonne, IL (United States)

Sponsoring Organization:: USDOE Office of Science (SC); Canadian Light Source, Inc.; Canada Foundation for Innovation (CFI); Natural Sciences and Engineering Research Council of Canada (NSERC); National Research Council (Canada); Canadian Institutes of Health Research (CIHR)

Grant/Contract Number:: AC02-06CH11357

OSTI ID:: 1881046

Alternate ID(s):: OSTI ID: 1988621

Journal Information:: Journal of Synchrotron Radiation (Online), Journal Name: Journal of Synchrotron Radiation (Online) Vol. 29 Journal Issue: 5; ISSN 1600-5775

Publisher:: International Union of Crystallography (IUCr)Copyright Statement

Country of Publication:: Denmark

Language:: English

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58 GEOSCIENCES
HERFD-XANES
geochemistry
mine waste
arsenic
linear combination fitting

Title: Improved precision in As speciation analysis with HERFD-XANES at the As K -edge: the case of As speciation in mine waste

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References (79)

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