Vibrational spectroscopy as a probe of heterogeneities within geochemical thin films on macro, micro, and nanoscales

Kim, Deborah; Townsley, Samantha; Grassian, Vicki H.

doi:10.1039/d3ra05179j

Cited by 3 publications

(1 citation statement)

References 100 publications

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“…For AFM measurements, the EF Shale sample was adhered to a stainless-steel disc that was magnetically secured to the sample holder that fit into the instrument. The sample was analyzed with the nanoIR2 microscopy system (Bruker, Anasys-Santa Barbara, CA). − AFM images were collected at a scan rate of 0.1–0.6 Hz, depending on the roughness of the sample, for both pre- and post-exposure with tip radii of ∼30 nm. Tapping mode probes were purchased from Bruker and had a spring constant of 1 to 7 N/m and a resonant frequency of 75 kHz.…”

Section: Materials and Experimental Methodsmentioning

confidence: 99%

Initial Laboratory Measurements Probing Hydrogen Interactions with Eagle Ford Shale and Pyrite: Potential Implications for Subsurface Hydrogen Storage

Kim,

Townsley,

Kutchko

et al. 2024

J. Phys. Chem. C

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Hydrogen (H 2 ) has the potential to be a transformative technology as an enabler of a low-carbon future and a promoter of renewable energy. When H 2 is injected and stored in the subsurface, it has the potential to interact with the caprock (usually shale), which overlies and seals the storage reservoir. This study examines the geochemical reactions or changes in surface morphology of Eagle Ford Shale, a proxy for caprock, upon exposure to H 2 at 50 °C and 10.3 MPa. Exposures were also performed with N 2 to provide an experimental control. Scanning electron microscopy with energy dispersive spectroscopy, atomic force microscopy, and optical photothermal-infrared spectroscopy were applied to quantify surface changes on the microscale and nanoscale level. Fluid chemistry changes were monitored by ion chromatography and inductively coupled plasma mass spectrometry. Exposure of Eagle Ford Shale to H 2 gas alone did not result in any chemical alterations to the shale or any changes in the surface morphology. Exposure of Eagle Ford Shale to both H 2 and water as well as N 2 and water resulted in changes to the surface morphology because of gypsum dissolution and reprecipitation, thus indicating that H 2 is not necessary to promote changes. Pure pyrite was the most reactive with H 2 possibly resulting in a reduction to pyrrhotite. These initial studies suggest that the extent of reactions activated by hydrogen with caprock is minor under the temperature and pressure conditions that would represent underground hydrogen storage.

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Section: Materials and Experimental Methodsmentioning

confidence: 99%

Initial Laboratory Measurements Probing Hydrogen Interactions with Eagle Ford Shale and Pyrite: Potential Implications for Subsurface Hydrogen Storage

Kim,

Townsley,

Kutchko

et al. 2024

J. Phys. Chem. C

Self Cite

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Emerging technologies for the evaluation of spatio-temporal polymerisation changes in flowable vs. sculptable dental resin-based composites

Marovic,

Haugen,

Par

et al. 2024

Dental Materials

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Probing Mineral-Organic Interfaces in Soils and Sediments Using Optical Photothermal Infrared Microscopy

Jamoteau,

Kansiz,

Unger

et al. 2024

Environ. Sci. Technol.

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Interactions among microbes, minerals, and organic matter are key controls on carbon, nutrient, and contaminant dynamics in soils and sediments. However, probing these interactions at relevant scales and through time remains an analytical challenge due to both their complex nature and the need for tools permitting nondestructive and real-time analysis at sufficient spatial resolution. Here, we demonstrate the ability and provide analytical recommendations for the submicronscale characterization of complex mineral-organic microstructures using optical photothermal infrared (O-PTIR) microscopy. Compared to conventional infrared techniques, O-PTIR spectra collected at submicron resolution of environmentally relevant mineral and organic reference compounds demonstrated similar spectral quality and sensitivity. O-PTIR detection sensitivity was greatest for highly crystalline minerals and potentially for low molecular weight organic compounds. Due to photothermal effects, O-PTIR was more sensitive toward organics than minerals compared to conventional IR approaches, even when organics were mineral-bound. Moreover, O-PTIR resolved mineral-bound and unbound organics in a complex mixture at submicron (<500 nm) resolution. Finally, we provide best practices for artifact-free analysis of organic and mineral samples by determining the appropriate laser power using damage thresholds. Our results highlight the potential of O-PTIR microscopy for nondestructive and time-resolved analysis of dynamic microbe-mineral-organic matter interactions in soils and sediments.

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Vibrational spectroscopy as a probe of heterogeneities within geochemical thin films on macro, micro, and nanoscales

Abstract: Geochemical thin films of different minerals and mineral samples were analyzed using several vibrational probes including microspectroscopic photothermal IR probes to uncover heterogeneity in these samples on micro and nanoscales.

Cited by 3 publications

References 100 publications

Initial Laboratory Measurements Probing Hydrogen Interactions with Eagle Ford Shale and Pyrite: Potential Implications for Subsurface Hydrogen Storage

Initial Laboratory Measurements Probing Hydrogen Interactions with Eagle Ford Shale and Pyrite: Potential Implications for Subsurface Hydrogen Storage

Emerging technologies for the evaluation of spatio-temporal polymerisation changes in flowable vs. sculptable dental resin-based composites

Probing Mineral-Organic Interfaces in Soils and Sediments Using Optical Photothermal Infrared Microscopy

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