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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 2 papers using this protocol.
Procedure from a recent peer-reviewed implementation
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
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