skip to main content
OSTI.GOV title logo U.S. Department of Energy
Office of Scientific and Technical Information

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

Patent ·
OSTI ID:1226816

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.

Research Organization:
Pacific Northwest National Laboratory (PNNL), Richland, WA (United States)
Sponsoring Organization:
USDOE
DOE Contract Number:
AC05-76RL01830
Assignee:
Battelle Memorial Institute (Richland, WA)
Patent Number(s):
9,194,920
Application Number:
13/648,751
OSTI ID:
1226816
Resource Relation:
Patent File Date: 2012 Oct 10
Country of Publication:
United States
Language:
English

References (21)

NMR probe for heterogeneous catalysis with isolated reagent flow and magic-angle spinning journal March 1999
A combined MAS nuclear magnetic resonance spectroscopy, in situ FT infrared spectroscopy and catalytic study of the conversion of allyl alcohol over zeolite catalysts journal January 1995
Sequential Steps of Ammoniation of the Microporous Silicoaluminophosphates H-SAPO-34 and H-SAPO-37 Investigated by In Situ CF MAS NMR Spectroscopy journal March 2004
In situ MAS NMR investigations of molecular sieves and zeolite-catalyzed reactions journal January 1999
In situ flow MAS NMR spectroscopy: State of the art and applications in heterogeneous catalysis journal October 2008
A new MAS NMR probe for in situ investigations of hydrocarbon conversion on solid catalysts under continuous-flow conditions journal January 1995
Conversion of Propan-2-ol on Zeolites LaNaY and HY Investigated by Gas Chromatography andin SituMAS NMR Spectroscopy under Continuous-Flow Conditions journal April 1997
In situ MAS NMR spectroscopy of surface compounds formed from methanol and from a toluene/methanol mixture on basic zeolite X journal May 2000
Alkali Metal Oxides, Peroxides, and Superoxides:  A Multinuclear MAS NMR Study journal November 1998
Conversion of methanol to hydrocarbons on zeolite HZSM‐5 investigated by in situ MAS NMR spectroscopy under flow conditions and on‐line gas chromatography journal January 1999
Application of in situ MAS NMR for elucidation of reaction mechanisms in heterogeneous catalysis journal November 1999
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
The development and applications of CAVERN methods for in situ NMR studies of reactions on solid acids journal January 1997
Characterization of Dispersed Heteropoly Acid on Mesoporous Zeolite Using Solid-State 31 P NMR Spin−Lattice Relaxation journal July 2009
Solid-state lead-207 NMR of lead(II) nitrate: Localized heating effects at high magic angle spinning speeds journal October 1995
Chemistry with ADF journal January 2001
Synthesis, characterization, and catalytic function of novel highly dispersed tungsten oxide catalysts on mesoporous silica journal April 2006
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
Evaluation of various DFT protocols for computing 1 H and 13 C chemical shifts to distinguish stereoisomers: diastereomeric 2-, 3-, and 4-methylcyclohexanols as a test set journal May 2007

Similar Records

A Large Sample Volume Magic Angle Spinning Nuclear Magnetic Resonance Probe for In-Situ Investigations with Constant Flow of Reactants
Journal Article · Tue Feb 21 00:00:00 EST 2012 · Physical Chemistry Chemical Physics · OSTI ID:1226816

Rotor Design for High Pressure Magic Angle Spinning Nuclear Magnetic Resonance
Journal Article · Tue Jan 01 00:00:00 EST 2013 · Journal of Magnetic Resonance · OSTI ID:1226816

High-pressure magic angle spinning nuclear magnetic resonance
Journal Article · Sat Oct 01 00:00:00 EDT 2011 · Journal of Magnetic Resonance · OSTI ID:1226816