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t1-noise elimination by continuous chemical shift anisotropy refocusing

Journal Article · · Solid State Nuclear Magnetic Resonance
 [1];  [2];  [2]
  1. Ames Lab., Ames, IA (United States)
  2. Ames Lab., and Iowa State Univ., Ames, IA (United States)

We report that due to their high gyromagnetic ratio, there is considerable interest in measuring distances and correlations involving protons, but such measurements are compounded by the simultaneous recoupling of chemical shift anisotropy (CSA). This secondary recoupling adds additional modulations to the signal intensities that ultimately lead to t1-noise and signal decay. Recently, Venkatesh et al. demonstrated that the addition of CSA refocusing periods during 1H-X dipolar recoupling led to sequences with far higher stability and performance. Herein, we describe a related effort and develop a symmetry-based recoupling sequence that continually refocuses the 1H CSA. This sequence shows superior performance to the regular and t1-noise eliminated D-HMQC sequences in the case of spin-1/2 nuclei and comparable performance to the later for half-integer quadrupoles.

Research Organization:
Ames Laboratory (AMES), Ames, IA (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES). Materials Sciences & Engineering Division
Grant/Contract Number:
AC02-07CH11358
OSTI ID:
1873414
Alternate ID(s):
OSTI ID: 1960939
Report Number(s):
IS-J-10,826
Journal Information:
Solid State Nuclear Magnetic Resonance, Journal Name: Solid State Nuclear Magnetic Resonance Vol. 120; ISSN 0926-2040
Publisher:
ElsevierCopyright Statement
Country of Publication:
United States
Language:
English

References (60)

Heteronuclear NMR Spectroscopy as a Surface-Selective Technique: A Unique Look at the Hydroxyl Groups of γ-Alumina. journal March 2014
Indirectly Detected DNP‐Enhanced 17 O NMR Spectroscopy: Observation of Non‐Protonated Near‐Surface Oxygen at Naturally Abundant Silica and Silica‐Alumina journal June 2021
SpinDynamica: Symbolic and numerical magnetic resonance in a Mathematica environment: SpinDynamica journal September 2017
35 Cl– 1 H Heteronuclear correlation magic‐angle spinning nuclear magnetic resonance experiments for probing pharmaceutical salts journal July 2021
Theoretical Calculations of the CPMAS Spectral Lineshapes of Half-Integer Quadrupole Systems journal May 1995
Sensitivity Enhancement in Solid State 15N NMR by Indirect Detection with High-Speed Magic Angle Spinning journal January 2000
SIMPSON: A General Simulation Program for Solid-State NMR Spectroscopy journal December 2000
Homonuclear Zero-Quantum Recoupling in Fast Magic-Angle Spinning Nuclear Magnetic Resonance journal May 2002
Good lattice points, discrepancy, and numerical integration journal December 1966
The importance of precise timing in pulsed, rotor-synchronous MAS NMR journal April 1992
Distorted powder lineshapes in 27 Al CP / MAS NMR spectroscopy of solids journal June 1993
of quadrupolar nuclei journal February 1992
The D-HMQC MAS-NMR Technique: An Efficient Tool for the Editing of Through-Space Correlation Spectra Between Quadrupolar and Spin-1/2 (31P, 29Si, 1H, 13C) Nuclei book January 2014
Symmetry principles for the design of radiofrequency pulse sequences in the nuclear magnetic resonance of rotating solids journal April 2000
Order-selective multiple-quantum excitation in magic-angle spinning NMR: creating triple-quantum coherences with a trilinear Hamiltonian journal December 2002
Indirect high-resolution detection for quadrupolar spin-3/2 nuclei in dipolar HMQC solid-state NMR experiments journal August 2010
Measurements of motionally averaged heteronuclear dipolar couplings in MAS NMR using R-type recoupling journal June 2004
A phase cycle scheme that significantly suppresses offset-dependent artifacts in the R2-CPMG 15N relaxation experiment journal November 2004
13C/14N heteronuclear multiple-quantum correlation with rotary resonance and REDOR dipolar recoupling journal January 2007
Broadband adiabatic inversion pulses for cross polarization in wideline solid-state NMR spectroscopy journal November 2012
Finite-pulse radio frequency driven recoupling with phase cycling for 2D 1H/1H correlation at ultrafast MAS frequencies journal June 2014
Computer-intensive simulation of solid-state NMR experiments using SIMPSON journal September 2014
Genetic algorithm optimized triply compensated pulses in NMR spectroscopy journal November 2015
Indirect detection of infinite-speed MAS solid-state NMR spectra journal March 2017
Using the heteronuclear Bloch-Siegert shift of protons for B1 calibration of insensitive nuclei not present in the sample journal January 2020
Proton-detected solid-state NMR spectroscopy of spin-1/2 nuclei with large chemical shift anisotropy journal June 2021
Double echo symmetry-based REDOR and RESPDOR pulse sequences for proton detected measurements of heteronuclear dipolar coupling constants journal March 2022
Heteronuclear polarization transfer by symmetry-based recoupling sequences in solid-state NMR journal September 2004
Proton detection of MAS solid-state NMR spectra of half-integer quadrupolar nuclei journal July 2017
γ-Independent through-space hetero-nuclear correlation between spin-1/2 and quadrupolar nuclei in solids journal July 2017
Enhanced 1H-X D-HMQC performance through improved 1H homonuclear decoupling journal April 2019
Frequency-Swept Ultra-Wideline Magic-Angle Spinning NMR Spectroscopy journal June 2021
High-Resolution NMR of S = 3/2 Quadrupole Nuclei by Detection of Double-Quantum Satellite Transitions via Protons journal May 2020
A Series of (6,6)-Connected Porous Lanthanide−Organic Framework Enantiomers with High Thermostability and Exposed Metal Sites: Scalable Syntheses, Structures, and Sorption Properties journal November 2010
Rod Packings and Metal−Organic Frameworks Constructed from Rod-Shaped Secondary Building Units journal February 2005
Proton-Selective 17 O− 1 H Distance Measurements in Fast Magic-Angle-Spinning Solid-State NMR Spectroscopy for the Determination of Hydrogen Bond Lengths journal November 2006
Chemical Shift Correlation NMR Spectroscopy with Indirect Detection in Fast Rotating Solids:  Studies of Organically Functionalized Mesoporous Silicas
  • Wiench, Jerzy W.; Bronnimann, Charles E.; Lin, Victor S. -Y
  • Journal of the American Chemical Society, Vol. 129, Issue 40, p. 12076-12077 https://doi.org/10.1021/ja074746+
journal September 2007
Hydrogen Adsorption in a Highly Stable Porous Rare-Earth Metal-Organic Framework: Sorption Properties and Neutron Diffraction Studies journal July 2008
The Structure of Molecular and Surface Platinum Sites Determined by DNP-SENS and Fast MAS 195 Pt Solid-State NMR Spectroscopy journal October 2020
Natural Abundance 17 O DNP Two-Dimensional and Surface-Enhanced NMR Spectroscopy journal June 2015
Observation of Low-γ Quadrupolar Nuclei by Surface-Enhanced NMR Spectroscopy journal May 2020
Sensitivity Enhancement and Heteronuclear Distance Measurements in Biological 17 O Solid-State NMR journal August 2006
Indirect Detection via Spin-1/2 Nuclei in Solid State NMR Spectroscopy: Application to the Observation of Proximities between Protons and Quadrupolar Nuclei journal November 2009
Probing Hydrogen Bonding in Cocrystals and Amorphous Dispersions Using 14 N– 1 H HMQC Solid-State NMR journal February 2013
PRESTO polarization transfer to quadrupolar nuclei: implications for dynamic nuclear polarization journal January 2015
Rapid acquisition of wideline MAS solid-state NMR spectra with fast MAS, proton detection, and dipolar HMQC pulse sequences journal January 2016
t 1 -Noise eliminated dipolar heteronuclear multiple-quantum coherence solid-state NMR spectroscopy journal January 2020
High-resolution through-space correlations between spin-1/2 and half-integer quadrupolar nuclei using the MQ-D-R-INEPT NMR experiment journal January 2012
Symmetry principles in the nuclear magnetic resonance of spinning solids: Heteronuclear recoupling by generalized Hartmann–Hahn sequences journal July 2001
Proton‐enhanced NMR of dilute spins in solids journal July 1973
Investigations of a nonrandom numerical method for multidimensional integration journal October 1973
Molecular Schrödinger Equation. VIII. A New Method for the Evaluation of Multidimensional Integrals journal December 1967
Second order average Hamiltonian theory of symmetry-based pulse schemes in the nuclear magnetic resonance of rotating solids: Application to triple-quantum dipolar recoupling journal June 2004
Theory and applications of supercycled symmetry-based recoupling sequences in solid-state nuclear magnetic resonance journal June 2006
Synchronous helical pulse sequences in magic-angle spinning nuclear magnetic resonance: Double quantum recoupling of multiple-spin systems journal May 2000
Accurate measurement of heteronuclear dipolar couplings by phase-alternating R-symmetry (PARS) sequences in magic angle spinning NMR spectroscopy journal September 2014
Population transfer HMQC for half-integer quadrupolar nuclei journal March 2015
Indirect NMR detection via proton of nuclei subject to large anisotropic interactions, such as 14 N, 195 Pt, and 35 Cl, using the T-HMQC sequence journal February 2022
Natural abundance O 17 and S 33 nuclear magnetic resonance spectroscopy in solids achieved through extended coherence lifetimes journal October 2019
Selective 1H-14N Distance Measurements by 14N Overtone Solid-State NMR Spectroscopy at Fast MAS journal April 2021

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