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

Abstract

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.

Authors:
 [1];  [1];  [1];  [1];  [1];  [1];  [1];  [1];  [1]
  1. Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
Publication Date:
Research Org.:
Pacific Northwest National Lab. (PNNL), Richland, WA (United States). Environmental Molecular Sciences Lab. (EMSL)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
OSTI Identifier:
1212233
Report Number(s):
PNNL-SA-110035
Journal ID: ISSN 1359-7345; CHCOFS; 47841; KC0302010
Grant/Contract Number:  
AC05-76RL01830; AC06-76RL01830; NIEHS R01ES022176
Resource Type:
Journal Article: Accepted Manuscript
Journal Name:
ChemComm
Additional Journal Information:
Journal Volume: 51; Journal Issue: 70; Journal ID: ISSN 1359-7345
Publisher:
Royal Society of Chemistry
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; 42 ENGINEERING; Environmental Molecular Sciences Laboratory

Citation Formats

Hu, Jian Z., Hu, Mary Y., Zhao, Zhenchao, Xu, Souchang, Vjunov, Aleksei, Shi, Hui, Camaioni, Donald M., Peden, Charles H. F., and Lercher, Johannes A. Sealed rotors for in situ high temperature high pressure MAS NMR. United States: N. p., 2015. Web. doi:10.1039/c5cc03910j.
Hu, Jian Z., Hu, Mary Y., Zhao, Zhenchao, Xu, Souchang, Vjunov, Aleksei, Shi, Hui, Camaioni, Donald M., Peden, Charles H. F., & Lercher, Johannes A. Sealed rotors for in situ high temperature high pressure MAS NMR. United States. doi:10.1039/c5cc03910j.
Hu, Jian Z., Hu, Mary Y., Zhao, Zhenchao, Xu, Souchang, Vjunov, Aleksei, Shi, Hui, Camaioni, Donald M., Peden, Charles H. F., and Lercher, Johannes A. Mon . "Sealed rotors for in situ high temperature high pressure MAS NMR". United States. doi:10.1039/c5cc03910j. https://www.osti.gov/servlets/purl/1212233.
@article{osti_1212233,
title = {Sealed rotors for in situ high temperature high pressure MAS NMR},
author = {Hu, Jian Z. and Hu, Mary Y. and Zhao, Zhenchao and Xu, Souchang and Vjunov, Aleksei and Shi, Hui and Camaioni, Donald M. and Peden, Charles H. F. and Lercher, Johannes A.},
abstractNote = {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.},
doi = {10.1039/c5cc03910j},
journal = {ChemComm},
issn = {1359-7345},
number = 70,
volume = 51,
place = {United States},
year = {2015},
month = {7}
}

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