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Title: Magic angle spinning nuclear magnetic resonance apparatus and process for high-resolution in situ investigations

A continuous-flow (CF) magic angle sample spinning (CF-MAS) NMR rotor and probe are described for investigating reaction dynamics, stable intermediates/transition states, and mechanisms of catalytic reactions in situ. The rotor includes a sample chamber of a flow-through design with a large sample volume that delivers a flow of reactants through a catalyst bed contained within the sample cell allowing in-situ investigations of reactants and products. Flow through the sample chamber improves diffusion of reactants and products through the catalyst. The large volume of the sample chamber enhances sensitivity permitting in situ .sup.13C CF-MAS studies at natural abundance.
Inventors:
; ; ; ;
Issue Date:
OSTI Identifier:
1226816
Assignee:
Battelle Memorial Institute (Richland, WA) PNNL
Patent Number(s):
9,194,920
Application Number:
13/648,751
Contract Number:
AC05-76RL01830
Resource Relation:
Patent File Date: 2012 Oct 10
Research Org:
Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
Sponsoring Org:
USDOE
Country of Publication:
United States
Language:
English
Subject:
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND SUPERFLUIDITY

Works referenced in this record:

In situ flow MAS NMR spectroscopy: State of the art and applications in heterogeneous catalysis
journal, October 2008

In situ MAS NMR spectroscopy of surface compounds formed from methanol and from a toluene/methanol mixture on basic zeolite X
journal, May 2000
  • Hunger, Michael; Schenk, Udo; Seiler, Michael
  • Journal of Molecular Catalysis A: Chemical, Vol. 156, Issue 1-2, p. 153-161
  • DOI: 10.1016/S1381-1169(99)00404-5

Application of in situ MAS NMR for elucidation of reaction mechanisms in heterogeneous catalysis
journal, November 1999
  • Ivanova, Irina I.
  • Colloids and Surfaces A: Physicochemical and Engineering Aspects, Vol. 158, Issue 1-2, p. 189-200
  • DOI: 10.1016/S0927-7757(99)00145-4

In Situ NMR Investigations of Heterogeneous Catalysis with Samples Prepared under Standard Reaction Conditions
journal, April 1998

Sealed capsules for convenient acquisition of variable-temperature controlled-atmosphere magic-angle-spinning NMR spectra of solids
journal, July 1986
  • Adrian Carpenter, T.; Klinowski, Jacek; Tilak, D.
  • Journal of Magnetic Resonance (1969), Vol. 68, Issue 3, p. 561-563
  • DOI: 10.1016/0022-2364(86)90347-1

Chemistry with ADF
journal, January 2001
  • te Velde, G.; Bickelhaupt, F. M.; Baerends, E. J.
  • Journal of Computational Chemistry, Vol. 22, Issue 9, p. 931-967
  • DOI: 10.1002/jcc.1056

NMR spectra of the BnAA′Bn′ type: Studies of but-2-ene and related compounds
journal, October 1968

The Nuclear Magnetic Resonance Spectrum of 2-Butanol
journal, December 1966
  • Jackman, L. M.; Bowman, N. S.
  • Journal of the American Chemical Society, Vol. 88, Issue 23, p. 5565-5570
  • DOI: 10.1021/ja00975a040