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Shining Synchrotron Light on Supercritical Fluids

This study explores the use of synchrotron light and X-ray techniques to analyze supercritical fluids in the Hydrothermal Diamond Anvil Cell (HDAC). The research focuses on different diamond anvil configurations, sample chamber surface profilometry, and diamond anvil path of fluorescence X-rays to the detector. The study includes X-ray fluorescence imaging and quantitative analysis of Ta2O5 particles and Ta in HF solutions at varying temperatures, as well as time-resolved analysis of Pb in aqueous fluid during interaction with metamict zircon. Additional techniques such as Raman spectroscopy, X-ray absorption spectroscopy (XAS), and X-ray diffraction (XRD) are employed to study the local structure of aqueous metal complexes and the solubility of selected oxides.

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Shining Synchrotron Light on Supercritical Fluids

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  1. Shining Synchrotron Light on Supercritical Fluids Alan J. Anderson St. Francis Xavier University

  2. The Hydrothermal Diamond Anvil Cell HDAC

  3. Hydrothermal Diamond Anvil Cell (HDAC)

  4. Different Diamond Anvil Configurations Grooves Re Gasket Sample Chamber

  5. Surface Profilometry Average depth 47.48 μm Volume 3.55 X 106µm3 FIB Milling of Diamond Anvil

  6. HDAC Sample Chamber at 25 oC Aqueous solution Vapor bubble 0.2 mm

  7. ρ = 0.87 0.80 Isochores 0.71 0.58 0.32 Liquid Vapor

  8. Synchrotron X-ray Micro- and Nanoprobes

  9. Canadian Light Source Inc.

  10. Detector

  11. Solution in Sample Chamber @ 25 ºC Diamond Anvil Path of Fluorescence X-rays to the Detector Liquid Vapor Path of Incident X-rays 300 µm

  12. X-ray Fluorescence Imaging and Quantitative Analysis

  13. Map showing the distribution of Ta2O5 particles in 5% HF at 25 ºC (HDAC 116) Solid Ta2O5 Particles Map showing the distribution of Ta in 5% HF at 360°C (HDAC 116) 100 µm

  14. Ta Lα1 Ta2O5 Dissolved in 5% HF HDAC 116 @ 360°C (ρ = 0.566) 10,700 μg mL-1 Ta HDAC 110 @ 350°C (ρ = 0.575) 7,400 µg mL-1 Ta Intensity Ta Standard (1000 µg mL-1) HDAC 110 @ 360°C (ρ = 0.575) HDAC 116 @ 400°C (ρ = 0.504) Ta Lβ1 Fe Kα1 Fe Kβ1 Energy (keV)

  15. Time resolved analysis - Pb in aqueous fluid during interaction with partially metamict zircon (ZrSiO4) at 300 oC

  16. X-ray Absorption Spectroscopy XAS Resolving the local structure of metals in SCW

  17. X-ray Absorption Fine Structure (XAFS)

  18. Summary • Synchrotron – based techniques • Monitor SCW – material interaction • Resolve the local structure of aqueous metal complexes • Solubility of selected oxides

  19. Raman spectroscopy HDAC on the microscope Raman system

  20. Re L lines Ta L lines 7.0 7.5 8.0 8.5 9.0 9.5 10.0 10.5 11.0 11.5 12.0 12.5 Energy (keV) Interferences in X-ray Emission Spectra

  21. Counts Energy (keV) Sample Contamination from Re Gasket

  22. Sample Contamination from Gasket Reaction with Diamond CH4

  23. X-ray Diffraction

  24. In situ XRD Wu et al. (1997) Dehydration & Rehydration of Montmorillonite Reversible changes in lattice dimensions

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