Discrete magic angle turning system, apparatus, and process for in situ magnetic resonance spectroscopy and imaging

Hu, Jian Zhi; Hoyt, David W; Wind, Robert A

Discrete magic angle turning system, apparatus, and process for in situ magnetic resonance spectroscopy and imaging

Patent · Tue May 19 00:00:00 EDT 2009

OSTI ID:963818

Hu, Jian Zhi ^[1]; Hoyt, David W ^[1]; Wind, Robert A ^[2]

Richland, WA
Kennewick, WA

Described are a "Discrete Magic Angle Turning" (DMAT) system, devices, and processes that combine advantages of both magic angle turning (MAT) and magic angle hopping (MAH) suitable, e.g., for in situ magnetic resonance spectroscopy and/or imaging. In an exemplary system, device, and process, samples are rotated in a clockwise direction followed by an anticlockwise direction of exactly the same amount. Rotation proceeds through an angle that is typically greater than about 240 degrees but less than or equal to about 360 degrees at constant speed for a time applicable to the evolution dimension. Back and forth rotation can be synchronized and repeated with a special radio frequency (RF) pulse sequence to produce an isotropic-anisotropic shift 2D correlation spectrum. The design permits tubes to be inserted into the sample container without introducing plumbing interferences, further allowing control over such conditions as temperature, pressure, flow conditions, and feed compositions, thus permitting true in-situ investigations to be carried out.

View Patent

Research Organization:: Pacific Northwest National Laboratory (PNNL), Richland, WA

Sponsoring Organization:: United States Department of Energy

DOE Contract Number:: AC06-76RL01830

Assignee:: RLO

Patent Number(s):: 7,535,224

Application Number:: 11/754,660

OSTI ID:: 963818

Country of Publication:: United States

Language:: English

References (41)

Solid-State ¹³ C NMR Measurements in Methoxynaphthalenes: Determination of the Substituent Chemical Shift Effects in the Principal Values Orendt, Anita M.; Hu, Jian Zhi; Jiang, Yi-Jin The Journal of Physical Chemistry A, Vol. 101, Issue 48 https://doi.org/10.1021/jp972212x	journal	November 1997
Metabonomics: Metabolic processes studied by NMR spectroscopy of biofluids Lindon, John C.; Nicholson, Jeremy K.; Holmes, Elaine Concepts in Magnetic Resonance, Vol. 12, Issue 5 https://doi.org/10.1002/1099-0534(2000)12:5<289::AID-CMR3>3.0.CO;2-W	journal	January 2000
Solid-State 13C NMR, X-ray, and Quantum Mechanical Studies of the Carbon Chemical Shifts Tensors of p-Tolyl Ether Facelli, Julio C.; Hu, Jian Zhi; Orendt, Anita M. The Journal of Physical Chemistry, Vol. 98, Issue 47 https://doi.org/10.1021/j100098a011	journal	November 1994
Removal of Dipolar Broadening of Nuclear Magnetic Resonance Spectra of Solids by Specimen Rotation Andrew, E. R.; Bradbury, A.; Eades, R. G. Nature, Vol. 183, Issue 4678 https://doi.org/10.1038/1831802a0	journal	June 1959
Measurement of 13C chemical shift tensor principal values with a magic-angle turning experiment Hu, Jian Zhi; Orendt, Anita M.; Alderman, D. W. Solid State Nuclear Magnetic Resonance, Vol. 3, Issue 4 https://doi.org/10.1016/0926-2040(94)90039-6	journal	August 1994
An Isotropic Chemical Shift-Chemical Shift Anisotropy Magic-Angle Slow-Spinning 2D NMR Experiment Hu, J. Z.; Alderman, D. W.; Ye, C. H. Journal of Magnetic Resonance, Series A, Vol. 105, Issue 1 https://doi.org/10.1006/jmra.1993.1252	journal	October 1993
High-resolution1H NMR spectroscopy in rat liver using magic angle turning at a 1 Hz spinning rate Hu, Jian Zhi; Rommereim, Donald N.; Wind, Robert A. Magnetic Resonance in Medicine, Vol. 47, Issue 5 https://doi.org/10.1002/mrm.10139	journal	April 2002
Two-dimensional switched-speed spinning NMR Kolbert, A. C.; de Groot, H. J. M.; Griffin, R. G. Journal of Magnetic Resonance (1969), Vol. 85, Issue 1 https://doi.org/10.1016/0022-2364(89)90320-X	journal	October 1989
High-resolution1H NMR spectroscopy in a live mouse subjected to 1.5 Hz magic angle spinning Wind, Robert A.; Hu, Jian Zhi; Rommereim, Donald N. Magnetic Resonance in Medicine, Vol. 50, Issue 6 https://doi.org/10.1002/mrm.10650	journal	November 2003
NMR-based metabonomic approaches for evaluating physiological influences on biofluid composition Bollard, Mary E.; Stanley, Elizabeth G.; Lindon, John C. NMR in Biomedicine, Vol. 18, Issue 3 https://doi.org/10.1002/nbm.935	journal	January 2005
Correlation of isotropic shifts and chemical shift anisotropies by two-dimensional fourier-transform magic-angle hopping nmr spectroscopy Bax, Ad; Szeverenyi, Nikolaus M.; Maciel, Gary E. Journal of Magnetic Resonance (1969), Vol. 52, Issue 1 https://doi.org/10.1016/0022-2364(83)90267-6	journal	March 1983
Resolution Enhancement in13C and15N Magic-Angle Turning Experiments with TPPM Decoupling McGeorge, Gary; Alderman, D. W.; Grant, David M. Journal of Magnetic Resonance, Vol. 137, Issue 1 https://doi.org/10.1006/jmre.1998.1664	journal	March 1999
Metabolic profiles to define the genome: can we hear the phenotypes? Griffin, Julian L. Philosophical Transactions of the Royal Society of London. Series B: Biological Sciences, Vol. 359, Issue 1446 https://doi.org/10.1098/rstb.2003.1411	journal	June 2004
Variable‐angle correlation spectroscopy in solid‐state nuclear magnetic resonance ^a) Frydman, Lucio; Chingas, Gerard C.; Lee, Young K. The Journal of Chemical Physics, Vol. 97, Issue 7 https://doi.org/10.1063/1.463860	journal	October 1992
Switching-angle sample-spinning NMR spectroscopy for obtaining powder-pattern-resolved 2D spectra: Measurements of 13C chemical-shift anisotropies in powdered 3,4-dimethoxybenzaldehyde Terao, T.; Fujii, T.; Onodera, T. Chemical Physics Letters, Vol. 107, Issue 2 https://doi.org/10.1016/0009-2614(84)85689-4	journal	May 1984
An Improved 2D Magic-Angle-Turning Pulse Sequence for the Measurement of Chemical-Shift Anisotropy Gan, Zhehong; Ernst, R. R. Journal of Magnetic Resonance, Series A, Vol. 123, Issue 1 https://doi.org/10.1006/jmra.1996.0227	journal	November 1996
Spinning-Sideband Suppression Using a Pseudo-Two-Dimensional Experiment Gan, Z. H. Journal of Magnetic Resonance, Series A, Vol. 109, Issue 2 https://doi.org/10.1006/jmra.1994.1164	journal	August 1994
Magic-angle hopping as an alternative to magic-angle spinning for solid state NMR Szeverenyi, Nikolaus M.; Bax, Ad; Maciel, Gary E. Journal of Magnetic Resonance (1969), Vol. 61, Issue 3 https://doi.org/10.1016/0022-2364(85)90184-2	journal	February 1985
Localized in vivo isotropic-anisotropic correlation1H NMR spectroscopy using ultraslow magic angle spinning Wind, Robert A.; Hu, Jian Z.; Majors, Paul D. Magnetic Resonance in Medicine, Vol. 55, Issue 1 https://doi.org/10.1002/mrm.20740	journal	January 2005
Sensitivity-enhanced phase-corrected ultra-slow magic angle turning using multiple-echo data acquisition Hu, Jian Zhi; Wind, Robert A. Journal of Magnetic Resonance, Vol. 163, Issue 1 https://doi.org/10.1016/S1090-7807(03)00103-4	journal	July 2003
A new MAS NMR probe for in situ investigations of hydrocarbon conversion on solid catalysts under continuous-flow conditions Hunger, Michael; Horvath, Thomas Journal of the Chemical Society, Chemical Communications, Issue 14 https://doi.org/10.1039/c39950001423	journal	January 1995
Improvements to the magic angle hopping experiment Hu, Jian Zhi; Orendt, Anita M.; Alderman, Donald W. Solid State Nuclear Magnetic Resonance, Vol. 2, Issue 5 https://doi.org/10.1016/0926-2040(93)90003-6	journal	October 1993
A new in situ chemical reactor for studying heterogeneous catalysis by NMR: The GRASSHopper Keeler, Camille; Xiong, Jincheng; Lock, Herman Catalysis Today, Vol. 49, Issue 4 https://doi.org/10.1016/S0920-5861(98)00451-9	journal	March 1999
A fast two-dimensional switching-angle sample-spinning method for separating chemical-shift powder patterns Nakai, Toshihito; McDowell, Charles A. Journal of Magnetic Resonance (1969), Vol. 93, Issue 3 https://doi.org/10.1016/0022-2364(91)90090-G	journal	July 1991
Two-Dimensional Sideband Separation in Magic-Angle-Spinning NMR Antzutkin, O. N.; Shekar, S. C.; Levitt, M. H. Journal of Magnetic Resonance, Series A, Vol. 115, Issue 1 https://doi.org/10.1006/jmra.1995.1142	journal	July 1995
Slow-MAS NMR: A new technology for in vivo metabolomic studies Wind, Robert A.; Hu, Jian Z.; Majors, Paul D. Drug Discovery Today: Technologies, Vol. 2, Issue 3 https://doi.org/10.1016/j.ddtec.2005.08.009	journal	September 2005
Chemical shift anisotropy in powdered solids studied by 2D FT NMR with flipping of the spinning axis Bax, Ad; Szeverenyi, Nikolaus M.; Maciel, Gary E. Journal of Magnetic Resonance (1969), Vol. 55, Issue 3 https://doi.org/10.1016/0022-2364(83)90134-8	journal	December 1983
Quantitative neuropathology by high resolution magic angle spinning proton magnetic resonance spectroscopy Cheng, L. L.; Ma, M. J.; Becerra, L. Proceedings of the National Academy of Sciences, Vol. 94, Issue 12 https://doi.org/10.1073/pnas.94.12.6408	journal	June 1997
A sensitive, high resolution magic angle turning experiment for measuring chemical shift tensor principal values Alderman, D. W.; McGEORGE, Gary; Hu, Jian Zhi Molecular Physics, Vol. 95, Issue 6 https://doi.org/10.1080/00268979809483243	journal	December 1998
Gradient, high-resolution, magic angle spinning1H nuclear magnetic resonance spectroscopy of intact cells Weybright, Patrick; Millis, Kevin; Campbell, Natalee Magnetic Resonance in Medicine, Vol. 39, Issue 3 https://doi.org/10.1002/mrm.1910390302	journal	March 1998
Two-dimensional resolution of isotropic and anisotropic chemical shifts in magic angle spinning NMR Kolbert, A. C.; Griffin, R. G. Chemical Physics Letters, Vol. 166, Issue 1 https://doi.org/10.1016/0009-2614(90)87055-V	journal	February 1990
High-resolution magic angle spinning proton NMR analysis of human prostate tissue with slow spinning rates Taylor, Jennifer L.; Wu, Chin-Lee; Cory, David Magnetic Resonance in Medicine, Vol. 50, Issue 3 https://doi.org/10.1002/mrm.10562	journal	August 2003
High resolution proton magnetic resonance spectroscopy of biological fluids Nicholson, Jeremy K.; Wilson, Ian D. Progress in Nuclear Magnetic Resonance Spectroscopy, Vol. 21, Issue 4-5 https://doi.org/10.1016/0079-6565(89)80008-1	journal	January 1989
High-resolution chemical shift and chemical shift anisotropy correlation in solids using slow magic angle spinning Gan, Zhehong Journal of the American Chemical Society, Vol. 114, Issue 21 https://doi.org/10.1021/ja00047a062	journal	October 1992
Biochemical Analysis Using High-Resolution Magic Angle Spinning NMR Spectroscopy Distinguishes Lipoma-Like Well-Differentiated Liposarcoma from Normal Fat Chen, Jin-Hong; Enloe, Brian M.; Fletcher, Christopher D. Journal of the American Chemical Society, Vol. 123, Issue 37 https://doi.org/10.1021/ja016182u	journal	September 2001
Structural Determination in Carbonaceous Solids Using Advanced Solid State NMR Techniques Hu, Jian Zhi; Solum, Mark S.; Taylor, Craig M. V. Energy & Fuels, Vol. 15, Issue 1 https://doi.org/10.1021/ef0001888	journal	January 2001
Anin SituNMR Probe with Reagent Flow and Magic Angle Spinning Goguen, Patrick; Haw, James F. Journal of Catalysis, Vol. 161, Issue 2 https://doi.org/10.1006/jcat.1996.0250	journal	July 1996
Magic-Angle-Turning Experiments for Measuring Chemical-Shift-Tensor Principal Values in Powdered Solids Hu, J. Z.; Wang, W.; Liu, F. Journal of Magnetic Resonance, Series A, Vol. 113, Issue 2 https://doi.org/10.1006/jmra.1995.1082	journal	April 1995
The stop-and-go spinning technique in MAS experiments Zeigler, Robert C.; Wind, Robert A.; Maciel, Gary E. Journal of Magnetic Resonance (1969), Vol. 79, Issue 2 https://doi.org/10.1016/0022-2364(88)90221-1	journal	September 1988
High-resolution1H NMR and magic angle spinning NMR spectroscopic investigation of the biochemical effects of 2-bromoethanamine in intact renal and hepatic tissue Garrod, S.; Humpher, E.; Connor, S. C. Magnetic Resonance in Medicine, Vol. 45, Issue 5 https://doi.org/10.1002/mrm.1106	journal	January 2001
Chemical-shift-anisotropy powder patterns by the two-dimensional angle-flipping approach. Effects of crystallite packing Maciel, Gary E.; Szeverenyi, Nikolaus M.; Sardashti, Maziar Journal of Magnetic Resonance (1969), Vol. 64, Issue 3 https://doi.org/10.1016/0022-2364(85)90098-8	journal	October 1985

Similar Records

An Isotropic Chemical Shift-Chemical Shift Anisotropic Correlation Experiment Using Discrete Magic Angle Turning

Journal Article · Fri May 01 00:00:00 EDT 2009 · Journal of Magnetic Resonance, 198(1):105-110 · OSTI ID:957352

Applications of the {sup 13}C NMR magic angle turning experiment to coal studies

Conference · Sat Dec 30 23:00:00 EST 1995 · OSTI ID:214680

Method for high resolution magnetic resonance analysis using magic angle technique

Patent · Mon Dec 29 23:00:00 EST 2003 · OSTI ID:1174657

Related Subjects

47 OTHER INSTRUMENTATION

Discrete magic angle turning system, apparatus, and process for in situ magnetic resonance spectroscopy and imaging

Citation Formats

References (41)

Similar Records

Related Subjects