Sealed rotors for in situ high temperature high pressure MAS NMR

Hu, Jian Z.; Hu, Mary Y.; Zhao, Zhenchao; Xu, Souchang; Vjunov, Aleksei; Shi, Hui; Camaioni, Donald M.; Peden, Charles H. F.; Lercher, Johannes A.

doi:10.1039/c5cc03910j

Title: Sealed rotors for in situ high temperature high pressure MAS NMR

Journal Article · Mon Jul 06 00:00:00 EDT 2015 · ChemComm

DOI:https://doi.org/10.1039/c5cc03910j· OSTI ID:1212233

Hu, Jian Z. ^[1]; Hu, Mary Y. ^[1]; Zhao, Zhenchao ^[1]; Xu, Souchang ^[1]; Vjunov, Aleksei ^[1]; Shi, Hui ^[1]; Camaioni, Donald M. ^[1]; Peden, Charles H. F. ^[1]; Lercher, Johannes A. ^[1]

Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

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.

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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)

Grant/Contract Number:: AC05-76RL01830; AC06-76RL01830; NIEHS R01ES022176

OSTI ID:: 1212233

Report Number(s):: PNNL-SA-110035; CHCOFS; 47841; KC0302010

Journal Information:: ChemComm, Vol. 51, Issue 70; ISSN 1359-7345

Publisher:: Royal Society of ChemistryCopyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 40 works

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Nuclear Magnetic Resonance Spectroscopy for In Situ Monitoring of Porous Materials Formation under Hydrothermal Conditions Haouas, Mohamed Materials, Vol. 11, Issue 8 https://doi.org/10.3390/ma11081416	journal	August 2018
Development and Application of In Situ High-Temperature, High-Pressure Magic Angle Spinning NMR Jaegers, Nicholas R.; Hu, Mary Y.; Hoyt, David W. Modern Magnetic Resonance https://doi.org/10.1007/978-3-319-28388-3_93	book	January 2018

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