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Title: High-pressure magic angle spinning nuclear magnetic resonance

Abstract

A high-pressure magic angle spinning (MAS) NMR capability, consisting of a reusable high-pressure MAS rotor, a high-pressure rotor loading/reaction chamber for in situ sealing and re-opening of the high-pressure MAS rotor, and a MAS probe with a localized RF coil for background signal suppression, is reported. The unusual technical challenges associated with development of a reusable high-pressure MAS rotor are addressed in part by modifying standard ceramics for the rotor sleeve by abrading the internal surface at both ends of the cylinder. In this way, not only is the advantage of ceramic cylinders for withstanding very high-pressure utilized, but also plastic bushings can be glued tightly in place so that other removable plastic sealing mechanisms/components and O-rings can be mounted to create the desired high-pressure seal. Using this strategy, sealed internal pressures exceeding 150 bars have been achieved and sustained under ambient external pressure with minimal loss of pressure for 72 h. Finally, as an application example, in situ 13C MAS NMR studies of mineral carbonation reaction intermediates and final products of forsterite (Mg 2SiO 4) reacted with supercritical CO 2 and H 2O at 150 bar and 50 °C are reported, with relevance to geological sequestration of carbon dioxide.

Authors:
; ; ; ; ; ;
Publication Date:
Research Org.:
Pacific Northwest National Laboratory (PNNL), Richland, WA (US), Environmental Molecular Sciences Laboratory (EMSL)
Sponsoring Org.:
USDOE
OSTI Identifier:
1026593
Report Number(s):
PNNL-SA-80681
Journal ID: ISSN 1090-7807; 39937; 39924; KP1704020; TRN: US1105027
DOE Contract Number:  
AC05-76RL01830
Resource Type:
Journal Article
Journal Name:
Journal of Magnetic Resonance
Additional Journal Information:
Journal Volume: 212; Journal Issue: 2; Journal ID: ISSN 1090-7807
Publisher:
Elsevier
Country of Publication:
United States
Language:
English
Subject:
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND SUPERFLUIDITY; BUSHINGS; CARBON DIOXIDE; CERAMICS; GASKETS; NUCLEAR MAGNETIC RESONANCE; PLASTICS; PROBES; REACTION INTERMEDIATES; ROTORS; SLEEVES; Environmental Molecular Sciences Laboratory

Citation Formats

Hoyt, David W., Turcu, Romulus V. F., Sears, Jesse A., Rosso, Kevin M., Burton, Sarah D., Felmy, Andrew R., and Hu, Jian Zhi. High-pressure magic angle spinning nuclear magnetic resonance. United States: N. p., 2011. Web. doi:10.1016/j.jmr.2011.07.019.
Hoyt, David W., Turcu, Romulus V. F., Sears, Jesse A., Rosso, Kevin M., Burton, Sarah D., Felmy, Andrew R., & Hu, Jian Zhi. High-pressure magic angle spinning nuclear magnetic resonance. United States. doi:10.1016/j.jmr.2011.07.019.
Hoyt, David W., Turcu, Romulus V. F., Sears, Jesse A., Rosso, Kevin M., Burton, Sarah D., Felmy, Andrew R., and Hu, Jian Zhi. Sat . "High-pressure magic angle spinning nuclear magnetic resonance". United States. doi:10.1016/j.jmr.2011.07.019.
@article{osti_1026593,
title = {High-pressure magic angle spinning nuclear magnetic resonance},
author = {Hoyt, David W. and Turcu, Romulus V. F. and Sears, Jesse A. and Rosso, Kevin M. and Burton, Sarah D. and Felmy, Andrew R. and Hu, Jian Zhi},
abstractNote = {A high-pressure magic angle spinning (MAS) NMR capability, consisting of a reusable high-pressure MAS rotor, a high-pressure rotor loading/reaction chamber for in situ sealing and re-opening of the high-pressure MAS rotor, and a MAS probe with a localized RF coil for background signal suppression, is reported. The unusual technical challenges associated with development of a reusable high-pressure MAS rotor are addressed in part by modifying standard ceramics for the rotor sleeve by abrading the internal surface at both ends of the cylinder. In this way, not only is the advantage of ceramic cylinders for withstanding very high-pressure utilized, but also plastic bushings can be glued tightly in place so that other removable plastic sealing mechanisms/components and O-rings can be mounted to create the desired high-pressure seal. Using this strategy, sealed internal pressures exceeding 150 bars have been achieved and sustained under ambient external pressure with minimal loss of pressure for 72 h. Finally, as an application example, in situ13C MAS NMR studies of mineral carbonation reaction intermediates and final products of forsterite (Mg2SiO4) reacted with supercritical CO2 and H2O at 150 bar and 50 °C are reported, with relevance to geological sequestration of carbon dioxide.},
doi = {10.1016/j.jmr.2011.07.019},
journal = {Journal of Magnetic Resonance},
issn = {1090-7807},
number = 2,
volume = 212,
place = {United States},
year = {2011},
month = {10}
}