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Natural bearing (raw and calcined at 500 °C) and iron-enriched (impregnation and pillaring) montmorillonitic clay samples were prepared. The obtained samples were characterized (X-ray diffraction, Fourier Transformed Infrared Spectroscopy, Scanning Electron Microscopy, and Energy Dispersive X-ray Spectroscopy) and evaluated as catalysts in catalytic wet oxidation of Brilliant Green and Crystal Violet. Experiments were conducted in the same conditions (0.5 g catalysts, 300 mL air/min or 0.5 mL H2O2, 25 mL of dye solution, 25 °C, initial solution pH = 6.0, for 3 h) in thermostated batch reaction tubes. Process evolution was followed using UV-Vis spectrometry (200–1100 cm−1) and total organic carbon. Dye removal efficiencies (decolorization) between 98 and 99% were determined, while total organic carbon removal efficiencies were calculated to be in the 53–98% range. Iron leakage investigation showed that iron is lost in higher amounts for the catalysts prepared using the impregnation method by comparison with the pillared sample.
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Implementation of simultaneous ultraviolet/visible and x-ray absorption spectroscopy with microfluidics
X-ray spectroscopies are uniquely poised to describe the geometric and electronic structure of metalloenzyme active sites under a wide variety of sample conditions. UV/Vis (ultraviolet/visible) spectroscopy is a similarly well-established technique that can identify and quantify catalytic intermediates. The work described here reports the first simultaneous collection of full in situ UV/Vis and high-energy resolution fluorescence detected x-ray absorption spectra. Implementation of a fiber optic UV/Vis spectrometer and parabolic mirror setup inside the dual array valence emission spectrometer allowing for simultaneous measurement of microfluidic flow and mixing samples at the Photon-In Photon-Out X-ray Spectroscopy beamline is described, and initial results on ferricyanide and a dilute iron protein are presented. In conjunction with advanced microfluidic mixing techniques, this will allow for the measurement and quantification of highly reactive catalytic intermediates at reaction-relevant temperatures on the millisecond timescale while avoiding potential complications induced by freeze quenching samples.
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- Award ID(s):
- 1231306
- PAR ID:
- 10588808
- Publisher / Repository:
- Review of Scientific Instruments
- Date Published:
- Journal Name:
- Review of Scientific Instruments
- Volume:
- 96
- Issue:
- 1
- ISSN:
- 0034-6748
- Format(s):
- Medium: X
- Sponsoring Org:
- National Science Foundation
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- Free Publicly Accessible Full Text
-
Accepted Manuscript
- Journal Article:
- https://doi.org/10.1063/5.0218572
