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Title: PRESTO polarization transfer to quadrupolar nuclei: Implications for dynamic nuclear polarization

Journal Article · · Physical Chemistry Chemical Physics. PCCP
DOI:https://doi.org/10.1039/c5cp04145g· OSTI ID:1221933
 [1];  [1];  [2]
  1. Ames Lab., Ames, IA (United States)
  2. Ames Lab., Ames, IA (United States); Iowa State Univ., Ames, IA (United States)

In this study, we show both experimentally and numerically on a series of model systems that in experiments involving transfer of magnetization from 1H to the quadrupolar nuclei under magic-angle-spinning (MAS), the PRESTO technique consistently outperforms traditionally used cross polarization (CP), affording more quantitative intensities, improved lineshapes, better overall sensitivity, and straightforward optimization. This advantage derives from the fact that PRESTO circumvents the convoluted and uncooperative spin dynamics during the CP transfer under MAS, by replacing the spin-locking of quadrupolar nuclei with a single central transition selective 90° pulse and using a symmetry-based recoupling sequence in the 1H channel. This is important in the context of dynamic nuclear polarization (DNP) NMR of quadrupolar nuclei, where the efficient transfer of enhanced 1H polarization is desired to obtain the highest sensitivity.

Research Organization:
Ames Laboratory (AMES), Ames, IA (United States)
Sponsoring Organization:
USDOE
Grant/Contract Number:
AC02-07CH11358
OSTI ID:
1221933
Report Number(s):
IS-J-8778; PPCPFQ; PII: S0965977399002603
Journal Information:
Physical Chemistry Chemical Physics. PCCP, Vol. 17, Issue 35; ISSN 1463-9076
Publisher:
Royal Society of ChemistryCopyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 28 works
Citation information provided by
Web of Science

References (58)

Probing Quadrupolar Nuclei by Solid-State NMR Spectroscopy: Recent Advances book January 2011
Distorted powder lineshapes in 27 Al CP / MAS NMR spectroscopy of solids journal June 1993
Theoretical Calculations of the CPMAS Spectral Lineshapes of Half-Integer Quadrupole Systems journal May 1995
Theoretical and experimental assessment of single- and multiple-quantum cross-polarization in solid state NMR journal May 2002
Line shapes in CP/MAS NMR spectra of half-integer quadrupolar nuclei journal February 1993
Increased Efficiency of Coherence Transfer in Cross-Polarization NMR from Quadrupolar Nuclei: Dynamic-Angle Cross-Polarization journal February 1994
Rapid Acquisition of 14 N Solid-State NMR Spectra with Broadband Cross Polarization journal October 2013
Signal enhancement in solid-state NMR of quadrupolar nuclei journal April 2013
Probing proximities between different quadrupolar isotopes using multi-pulse cross-polarization journal March 2013
Coherence transfer involving quadrupolar nuclei in solids: aluminum-27 .tautm. phosphorus-31 cross-polarization NMR in the molecular sieve VPI-5 journal July 1992
27 Al{ 1 H} Cross Polarization Triple-Quantum Magic Angle Spinning NMR journal July 1997
Multiple-Quantum Cross Polarization in Quadrupolar Spin Systems during Magic-Angle Spinning journal January 2000
High-Resolution Heteronuclear Correlation between Quadrupolar and Spin-12 Nuclei Using Multiple-Quantum Magic-Angle Spinning journal April 1997
A new sequence for the MQMAS/HETCOR experiment journal June 1998
Measurement of interatomic connectivities in molecular sieves using MQMAS-based methods journal March 1999
High resolution heteronuclear correlation NMR spectroscopy between quadrupolar nuclei and protons in the solid state journal August 2004
SPAM-MQ-HETCOR: an improved method for heteronuclear correlation spectroscopy between quadrupolar and spin-1/2 nuclei in solid-state NMR journal January 2006
13C/14N heteronuclear multiple-quantum correlation with rotary resonance and REDOR dipolar recoupling journal January 2007
3D 1H–13C–14N correlation solid-state NMR spectrum journal August 2008
Broadband excitation and indirect detection of nitrogen-14 in rotating solids using Delays Alternating with Nutation (DANTE) journal September 2011
Comparison of several hetero-nuclear dipolar recoupling NMR methods to be used in MAS HMQC/HSQC journal May 2008
Indirect high-resolution detection for quadrupolar spin-3/2 nuclei in dipolar HMQC solid-state NMR experiments journal August 2010
Population transfer HMQC for half-integer quadrupolar nuclei journal March 2015
Dynamic nuclear polarization at high magnetic fields journal February 2008
Dynamic Nuclear Polarization Surface Enhanced NMR Spectroscopy journal March 2013
Rapid Natural-Abundance 2D 13 C- 13 C Correlation Spectroscopy Using Dynamic Nuclear Polarization Enhanced Solid-State NMR and Matrix-Free Sample Preparation journal October 2012
Influences of Dilute Organic Adsorbates on the Hydration of Low-Surface-Area Silicates journal June 2015
Dynamic Nuclear Polarization of Oxygen-17 journal July 2012
High-Field 13 C Dynamic Nuclear Polarization with a Radical Mixture journal February 2013
Dynamic Nuclear Polarization of 17 O: Direct Polarization journal November 2013
Dynamic Nuclear Polarization NMR Spectroscopy of Microcrystalline Solids journal September 2012
Mesoporous Silica Nanoparticles Loaded with Surfactant: Low Temperature Magic Angle Spinning 13 C and 29 Si NMR Enhanced by Dynamic Nuclear Polarization journal January 2013
Dynamic nuclear polarization of quadrupolar nuclei using cross polarization from protons: surface-enhanced aluminium-27 NMR journal January 2012
Enhanced Solid-State NMR Correlation Spectroscopy of Quadrupolar Nuclei Using Dynamic Nuclear Polarization journal October 2012
Dynamic Nuclear Polarization Enhanced Natural Abundance 17 O Spectroscopy journal February 2013
Primostrato Solid-State NMR Enhanced by Dynamic Nuclear Polarization: Pentacoordinated Al 3+ Ions Are Only Located at the Surface of Hydrated γ-Alumina journal October 2014
Probing 27 Al– 13 C proximities in metal–organic frameworks using dynamic nuclear polarization enhanced NMR spectroscopy journal January 2014
Heteronuclear polarization transfer by symmetry-based recoupling sequences in solid-state NMR journal September 2004
Symmetry-based recoupling of 17O–1H spin pairs in magic-angle spinning NMR journal March 2006
14 N overtone NMR under MAS: signal enhancement using symmetry-based sequences and novel simulation strategies journal January 2015
Natural Abundance 17 O DNP Two-Dimensional and Surface-Enhanced NMR Spectroscopy journal June 2015
Structural investigation of aluminium doped ZnO nanoparticles by solid-state NMR spectroscopy journal January 2012
Measurement of through-space connectivities between spin-1/2 and quadrupolar nuclei in solid-state NMR: the TEDOR-MQMAS method journal December 2007
Through-space MP-CPMAS experiments between spin-1/2 and half-integer quadrupolar nuclei in solid-state NMR journal May 2008
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
Efficient dipolar recoupling in the NMR of rotating solids. A sevenfold symmetric radiofrequency pulse sequence journal August 1995
Measurement of NH Bond Lengths by Fast Magic-Angle Spinning Solid-State NMR Spectroscopy:  A New Method for the Quantification of Hydrogen Bonds journal November 2001
SIMPSON: A General Simulation Program for Solid-State NMR Spectroscopy journal December 2000
Computer-intensive simulation of solid-state NMR experiments using SIMPSON journal September 2014
Obtaining accurate chemical shifts for all magnetic nuclei ( 1 H, 13 C, 17 O, and 27 Al) in tris(2,4-pentanedionato- O , O ′)aluminium(III) — A solid-state NMR case study journal September 2011
Isomerization of the Prenucleation Building Unit during Crystallization of AlPO 4 -CJ2:  An MQMAS, CP-MQMAS, and HETCOR NMR Study journal December 1999
11 B Chemical Shift Anisotropies in Borates from 11 B MAS, MQMAS, and Single-Crystal NMR Spectroscopy journal January 2004
Oxyfluorinated Microporous Compounds. II. Solid State NMR of (NH4)0.88(H3O)0.12AlPO4(OH)0.33F0.67 journal July 1993
Combining Multinuclear High-Resolution Solid-State MAS NMR and Computational Methods for Resonance Assignment of Glutathione Tripeptide journal May 2012
Large Molecular Weight Nitroxide Biradicals Providing Efficient Dynamic Nuclear Polarization at Temperatures up to 200 K journal August 2013
Heteronuclear NMR Spectroscopy as a Surface-Selective Technique: A Unique Look at the Hydroxyl Groups of γ-Alumina. journal March 2014
REPULSION, A Novel Approach to Efficient Powder Averaging in Solid-State NMR journal March 1997
Composite-180° pulse-based symmetry sequences to recouple proton chemical shift anisotropy tensors under ultrafast MAS solid-state NMR spectroscopy journal January 2015

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