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Sealed rotors for in situ high temperature high pressure MAS NMR

Journal Article · · ChemComm
DOI:https://doi.org/10.1039/c5cc03910j· OSTI ID:1212233
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  1. Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
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Magic angle spinning (MAS) nuclear magnetic resonance (NMR) investigations on heterogeneous samples containing solids, semi-solids, liquid and gases or a mixture of them under non-conventional conditions of a combined high pressure and high temperature, or cold temperature suffer from the unavailability of a perfectly sealed rotor. Here, we report the design of reusable and perfectly-sealed all-zircornia MAS rotors. The rotors are easy to use and are suitable for operation temperatures from below 0 to 250 °C and pressures up to 100 bar. As an example of potential applications we performed in situ MAS NMR investigations of AlPO₄-5 molecular sieve crystallization, a kinetic study of the cyclohexanol dehydration reaction using 13C MAS NMR, and an investigation of the metabolomics of intact biological tissue at low temperature using 1H HR-MAS NMR spectroscopy. The in situ MAS NMR experiments performed using the reported rotors allowed reproduction of the results from traditional batch reactions, while offering more detailed quantitative information at the molecular level, as demonstrated for the molecular sieve synthesis and activation energy measurements for cyclohexanol dehydration. The perfectly sealed rotor also shows promising application for metabolomics studies using 1H HR-MAS NMR.

Research Organization:
Pacific Northwest National Laboratory (PNNL), Richland, WA (United States). Environmental Molecular Sciences Laboratory (EMSL).
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)
Grant/Contract Number:
AC05-76RL01830; AC06-76RL01830
OSTI ID:
1212233
Report Number(s):
PNNL-SA--110035; 47841; KC0302010
Journal Information:
ChemComm, Journal Name: ChemComm Journal Issue: 70 Vol. 51; ISSN CHCOFS; ISSN 1359-7345
Publisher:
Royal Society of ChemistryCopyright Statement
Country of Publication:
United States
Language:
English

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Cited By (4)

Nuclear Magnetic Resonance Spectroscopy for In Situ Monitoring of Porous Materials Formation under Hydrothermal Conditions journal August 2018
Unraveling Structure and Dynamics in Porous Frameworks via Advanced In Situ Characterization Techniques journal January 2020
Development and Application of In Situ High-Temperature, High-Pressure Magic Angle Spinning NMR book January 2018
The Progress of Metabolomics Study in Traditional Chinese Medicine Research journal January 2015

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Environmental Molecular Sciences Laboratory