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Title: Rotor Design for High Pressure Magic Angle Spinning Nuclear Magnetic Resonance

Abstract

High pressure magic angle spinning (MAS) nuclear magnetic resonance (NMR) with a sample spinning rate exceeding 2.1 kHz and pressure greater than 165 bar has never been realized. In this work, a new sample cell design is reported, suitable for constructing cells of different sizes. Using a 7.5 mm high pressure MAS rotor as an example, internal pressure as high as 200 bar at a sample spinning rate of 6 kHz is achieved. The new high pressure MAS rotor is re-usable and compatible with most commercial NMR set-ups, exhibiting low 1H and 13C NMR background and offering maximal NMR sensitivity. As an example of its many possible applications, this new capability is applied to determine reaction products associated with the carbonation reaction of a natural mineral, antigorite ((Mg,Fe2+)3Si2O5(OH)4), in contact with liquid water in water-saturated supercritical CO2 (scCO2) at 150 bar and 50 deg C. This mineral is relevant to the deep geologic disposal of CO2, but its iron content results in too many sample spinning sidebands at low spinning rate. Hence, this chemical system is a good case study to demonstrate the utility of the higher sample spinning rates that can be achieved by our new rotor design. Wemore » expect this new capability will be useful for exploring solid-state, including interfacial, chemistry at new levels of high-pressure in a wide variety of fields.« less

Authors:
; ; ; ; ; ;
Publication Date:
Research Org.:
Pacific Northwest National Laboratory (PNNL), Richland, WA (US), Environmental Molecular Sciences Laboratory (EMSL)
Sponsoring Org.:
USDOE
OSTI Identifier:
1059184
Report Number(s):
PNNL-SA-88703
Journal ID: ISSN 1090-7807; 47427; 39937; TRN: US1400315
DOE Contract Number:  
AC05-76RL01830
Resource Type:
Journal Article
Journal Name:
Journal of Magnetic Resonance
Additional Journal Information:
Journal Volume: 226; Journal ID: ISSN 1090-7807
Publisher:
Elsevier
Country of Publication:
United States
Language:
English
Subject:
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND SUPERFLUIDITY; MAS; sample cell; MAS rotor; Environmental Molecular Sciences Laboratory; NUCLEAR MAGNETIC RESONANCE; PRESSURE RANGE MEGA PA 10-100

Citation Formats

Turcu, Romulus V.F., Hoyt, David W., Rosso, Kevin M., Sears, Jesse A., Loring, John S., Felmy, Andrew R., and Hu, Jian Z. Rotor Design for High Pressure Magic Angle Spinning Nuclear Magnetic Resonance. United States: N. p., 2013. Web. doi:10.1016/j.jmr.2012.08.009.
Turcu, Romulus V.F., Hoyt, David W., Rosso, Kevin M., Sears, Jesse A., Loring, John S., Felmy, Andrew R., & Hu, Jian Z. Rotor Design for High Pressure Magic Angle Spinning Nuclear Magnetic Resonance. United States. doi:10.1016/j.jmr.2012.08.009.
Turcu, Romulus V.F., Hoyt, David W., Rosso, Kevin M., Sears, Jesse A., Loring, John S., Felmy, Andrew R., and Hu, Jian Z. Tue . "Rotor Design for High Pressure Magic Angle Spinning Nuclear Magnetic Resonance". United States. doi:10.1016/j.jmr.2012.08.009.
@article{osti_1059184,
title = {Rotor Design for High Pressure Magic Angle Spinning Nuclear Magnetic Resonance},
author = {Turcu, Romulus V.F. and Hoyt, David W. and Rosso, Kevin M. and Sears, Jesse A. and Loring, John S. and Felmy, Andrew R. and Hu, Jian Z.},
abstractNote = {High pressure magic angle spinning (MAS) nuclear magnetic resonance (NMR) with a sample spinning rate exceeding 2.1 kHz and pressure greater than 165 bar has never been realized. In this work, a new sample cell design is reported, suitable for constructing cells of different sizes. Using a 7.5 mm high pressure MAS rotor as an example, internal pressure as high as 200 bar at a sample spinning rate of 6 kHz is achieved. The new high pressure MAS rotor is re-usable and compatible with most commercial NMR set-ups, exhibiting low 1H and 13C NMR background and offering maximal NMR sensitivity. As an example of its many possible applications, this new capability is applied to determine reaction products associated with the carbonation reaction of a natural mineral, antigorite ((Mg,Fe2+)3Si2O5(OH)4), in contact with liquid water in water-saturated supercritical CO2 (scCO2) at 150 bar and 50 deg C. This mineral is relevant to the deep geologic disposal of CO2, but its iron content results in too many sample spinning sidebands at low spinning rate. Hence, this chemical system is a good case study to demonstrate the utility of the higher sample spinning rates that can be achieved by our new rotor design. We expect this new capability will be useful for exploring solid-state, including interfacial, chemistry at new levels of high-pressure in a wide variety of fields.},
doi = {10.1016/j.jmr.2012.08.009},
journal = {Journal of Magnetic Resonance},
issn = {1090-7807},
number = ,
volume = 226,
place = {United States},
year = {2013},
month = {1}
}