Building a Cost-Efficient High-Pressure Cell for Online High-Field NMR and MRI Using Standard Static Probe Heads: An In Situ Demonstration on Clathrate Hydrate Formation

Surface modification of mesostructured cellular foam to enhance hydrogen storage in binary THF/H2 clathrate hydrate

“…In order to minimize the 1 H background signal of the host material and facilitate identification of all components in spectra, the MCF (f-1) material was rinsed 3 times with D 2 O and subsequently dried at 363 K under vacuum. Approximately 30 mg of dried D-exchanged MCF (f-1) sample was packed in a 5 mm high-pressure NMR cell built according to the design by Houlleberghs et al 70 before adding 60 μL of a 5.56 mol% THF-D 2 O mixture to the system. The tube was pressurized to 7 MPa with H 2 gas before transferring to a pre-cooled (265 K) NMR probe head and allowing the system to equilibrate for 10 h. Following shimming, 48 transients were recorded for each 1 H NMR spectrum using a 30° pulse with 18 kHz RF strength and a repetition delay of 10 s. Chemical shift referencing was carried out with respect to TMS, using ethylbenzene (10% in chloroform-d) as a secondary reference with δ ( 1 H) = 1.22 ppm.…”

Noncontact In Situ Multidiagnostic NMR/Dielectric Spectroscopy

“…Characterization of interfacial interactions is, however, extremely tedious, especially in 3D porous materials such as zeolites, mesoporous silicates, metal–organic frameworks (MOFs), and covalent organic frameworks (COFs). Such materials are nevertheless abundantly implemented in chemical applications, − in molecular water research, , and for energy storage applications. − Specifically for zeolites, solvent (e.g., water, alcohol) pore wall interactions impact catalysis and adsorption processes. , …”