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Title: High temperature/pressure MAS-NMR for the study of dynamic processes in mixed phase systems

Abstract

Here, a new MAS-NMR rotor (the WHiMS rotor) has been developed which can reach pressures of 400 bar at 20 °C or 225 bar at 250 °C. These rotors are ideal for mixed phase systems such as a reaction using a solid catalyst with a liquid/supercritical solvent topped with high pressure gas in the head space. After solid and liquid portions of the sample are loaded, the rotor is capped with an o-ring equipped polymer bushing that snaps into a mating groove in the rotor. The bushings incorporate a check valve into the sealing mechanism which allows for pressurization without mechanical manipulation – they will allow gas to flow in but not out. This WHiMS rotor design has enabled experiments on a wide variety of biotic and abiotic mixed-phase systems. Geochemical systems have also been studied, for example, adsorption and confinement studies of supercritical methane/CO 2 in clays and other minerals which display pressure dependent 13C chemical shifts. Example data from other mixed-phase chemical and microbial systems are reported. These include monitoring metabolite conversion of extremophilic bacteria found in subsurface systems at elevated pressures and real-time operando reactions in catalysis systems - with liquid-quality resolution for 1H and 13C NMRmore » spectra.« less

Authors:
 [1];  [2];  [3];  [3];  [1];  [3]; ORCiD logo [3]
  1. Univ. of California, Santa Barbara, CA (United States)
  2. Ames Lab., Ames, IA (United States)
  3. Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
Publication Date:
Research Org.:
Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1479148
Alternate Identifier(s):
OSTI ID: 1482210
Report Number(s):
PNNL-SA-138048
Journal ID: ISSN 0730-725X; PII: S0730725X18304259
Grant/Contract Number:  
CBET-1512228; CBET-1604095; AC05-76RL01830
Resource Type:
Journal Article: Published Article
Journal Name:
Magnetic Resonance Imaging
Additional Journal Information:
Journal Volume: 56; Journal ID: ISSN 0730-725X
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY

Citation Formats

Chamas, Ali, Qi, Long, Mehta, Hardeep S., Sears, Jesse A., Scott, Susannah L., Walter, Eric D., and Hoyt, David W. High temperature/pressure MAS-NMR for the study of dynamic processes in mixed phase systems. United States: N. p., 2018. Web. doi:10.1016/j.mri.2018.09.026.
Chamas, Ali, Qi, Long, Mehta, Hardeep S., Sears, Jesse A., Scott, Susannah L., Walter, Eric D., & Hoyt, David W. High temperature/pressure MAS-NMR for the study of dynamic processes in mixed phase systems. United States. doi:10.1016/j.mri.2018.09.026.
Chamas, Ali, Qi, Long, Mehta, Hardeep S., Sears, Jesse A., Scott, Susannah L., Walter, Eric D., and Hoyt, David W. Thu . "High temperature/pressure MAS-NMR for the study of dynamic processes in mixed phase systems". United States. doi:10.1016/j.mri.2018.09.026.
@article{osti_1479148,
title = {High temperature/pressure MAS-NMR for the study of dynamic processes in mixed phase systems},
author = {Chamas, Ali and Qi, Long and Mehta, Hardeep S. and Sears, Jesse A. and Scott, Susannah L. and Walter, Eric D. and Hoyt, David W.},
abstractNote = {Here, a new MAS-NMR rotor (the WHiMS rotor) has been developed which can reach pressures of 400 bar at 20 °C or 225 bar at 250 °C. These rotors are ideal for mixed phase systems such as a reaction using a solid catalyst with a liquid/supercritical solvent topped with high pressure gas in the head space. After solid and liquid portions of the sample are loaded, the rotor is capped with an o-ring equipped polymer bushing that snaps into a mating groove in the rotor. The bushings incorporate a check valve into the sealing mechanism which allows for pressurization without mechanical manipulation – they will allow gas to flow in but not out. This WHiMS rotor design has enabled experiments on a wide variety of biotic and abiotic mixed-phase systems. Geochemical systems have also been studied, for example, adsorption and confinement studies of supercritical methane/CO2 in clays and other minerals which display pressure dependent 13C chemical shifts. Example data from other mixed-phase chemical and microbial systems are reported. These include monitoring metabolite conversion of extremophilic bacteria found in subsurface systems at elevated pressures and real-time operando reactions in catalysis systems - with liquid-quality resolution for 1H and 13C NMR spectra.},
doi = {10.1016/j.mri.2018.09.026},
journal = {Magnetic Resonance Imaging},
issn = {0730-725X},
number = ,
volume = 56,
place = {United States},
year = {2018},
month = {10}
}

Journal Article:
Free Publicly Available Full Text
Publisher's Version of Record at 10.1016/j.mri.2018.09.026

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