X-ray Absorption Near Edge Structure spectroscopy

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Method synopsis

Sulfur K-edge X-ray Absorption Near Edge Structure spectroscopy was used to determine sulfur speciation in solid samples including bedrock, soils, and sediments. Linear combination fitting was used to quantify different sulfur forms including pyrite, elemental sulfur, sulfate, and organic sulfur.

Synthesized from method descriptions across 4 papers using this protocol.

Procedure from a recent peer-reviewed implementation

Steps below were extracted from the most recent peer-reviewed implementation of this protocol in the corpus — Sulfur Biogeochemical Cycling and Redox Dynamics in a Shale-Dominated Mountainous Watershed (2022), Journal of Geophysical Research: Biogeosciences. Implementations in other papers (listed below) may differ.

1. Perform sulfur K-edge XANES analysis
   All samples were analyzed at sulfur K-edge by XANES at Canadian Light Source (CLS), Stanford Synchrotron Radiation Laboratory (SSRL), and Advanced Light Source (ALS). Spectra were recorded in fluorescence mode with absolute energy calibrated to 2481.8 eV using calcium sulfate white line.
   Quantities: 2 scans per sample at CLS, 14-19 scans per sample at SSRLDuration: Multiple beamtime allocationsConditions: Synchrotron radiation facilities with specific beamline configurations
   Equipment: CLS SXRMB beamline with 7-element silicon drift detector, SSRL beamline 14-3 with 4-element Vortex detector, ALS beamline 10.3.2 with 1-element silicon drift fluorescence detector
2. Perform microscale XANES and XRF mapping
   Microscale X-ray fluorescence imaging and XANES analysis of hillslope shale were performed at ALS beamline 10.3.2. Low energy maps were collected at 2700 eV for S, Ca, Si at 20 x 20 μm and 5 x 5 μm spot sizes for lower and higher resolution maps.
   Quantities: Multiple maps at different resolutions on fracture surfacesDuration: Not specifiedConditions: ALS beamline 10.3.2 with energy resolution of 0.3 eV
   Equipment: 1-element silicon drift fluorescence detector, low energy maps capability

Typical Equipment

• synchrotron X-ray sources
• XANES spectroscopy equipment
• ATHENA software for data analysis

Output Measurements

• sulfur speciation percentages
• elemental sulfur content
• pyrite content
• organic sulfur content

Papers Using This Protocol (4)

Species Studied With This Protocol

Places Where Used