Peat, D.T., et al., Achievement of high nuclear spin polarization using lanthanides as low-temperature NMR relaxation agents. Phys. Chem. Chem. Phys., 2013. 15(20): p. 7586-7591.
Many approaches are now available for achieving high levels of nuclear spin polarization. One of these methods is based on the notion that as the temperature is reduced, the equilibrium nuclear polarization will increase, according to the Boltzmann distribution. The main problem with this approach is the length of time it may take to approach thermal equilibrium at low temperatures, since nuclear relaxation times (characterized by the spin-lattice relaxation time T1) can become very long. Here, we show, by means of relaxation time measurements of frozen solutions, that selected lanthanide ions, in the form of their chelates with DTPA, can act as effective relaxation agents at low temperatures. Differential effects are seen with the different lanthanides that were tested, holmium and dysprosium showing highest relaxivity, while gadolinium is ineffective at temperatures of 20 K and below. These observations are consistent with the known electron-spin relaxation time characteristics of these lanthanides. The maximum relaxivity occurs at around 10 K for Ho-DTPA and 20 K for Dy-DTPA. Moreover, these two agents show only modest relaxivity at room temperature, and can thus be regarded as relaxation switches. We conclude that these agents can speed up solid state NMR experiments by reducing the T1 values of the relevant nuclei, and hence increasing the rate at which data can be acquired. They could also be of value in the context of a simple low-cost method of achieving several-hundred-fold improvements in polarization for experiments in which samples are pre-polarized at low temperatures, then rewarmed and dissolved immediately prior to analysis.
High Frequency Dynamic Nuclear Polarization
From The DNP-NMR Blog:
High Frequency Dynamic Nuclear Polarization
Ni, Q.Z., et al., High Frequency Dynamic Nuclear Polarization. Acc Chem Res, 2013.
http://www.ncbi.nlm.nih.gov/pubmed/23597038
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06-07-2013 10:42 PM
Temperature Dependence of Electron Spin Relaxation of 2,2-Diphenyl-1-Picrylhydrazyl in Polystyrene
From The DNP-NMR Blog:
Temperature Dependence of Electron Spin Relaxation of 2,2-Diphenyl-1-Picrylhydrazyl in Polystyrene
Meyer, V., S. Eaton, and G. Eaton, Temperature Dependence of Electron Spin Relaxation of 2,2-Diphenyl-1-Picrylhydrazyl in Polystyrene. Appl. Magn. Reson., 2013. 44(4): p. 509-517.
http://dx.doi.org/10.1007/s00723-012-0417-7
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04-15-2013 10:32 PM
High-Field (13)C Dynamic Nuclear Polarization with a Radical Mixture
From the The DNP-NMR Blog:
High-Field (13)C Dynamic Nuclear Polarization with a Radical Mixture
Michaelis, V.K., et al., High-Field (13)C Dynamic Nuclear Polarization with a Radical Mixture. J Am Chem Soc, 2013.
http://www.ncbi.nlm.nih.gov/pubmed/23373472
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04-15-2013 08:52 AM
[NMR paper] Electron Spin Density on the Axial His Ligand of High-Spin and Low-Spin Nitrophorin 2 Probed by Heteronuclear NMR Spectroscopy.
Electron Spin Density on the Axial His Ligand of High-Spin and Low-Spin Nitrophorin 2 Probed by Heteronuclear NMR Spectroscopy.
http://www.ncbi.nlm.nih.gov/corehtml/query/egifs/http:--pubs.acs.org-images-pubmed-acspubs.jpg Related Articles Electron Spin Density on the Axial His Ligand of High-Spin and Low-Spin Nitrophorin 2 Probed by Heteronuclear NMR Spectroscopy.
Inorg Chem. 2013 Jan 17;
Authors: Abriata LA, Zaballa ME, Berry RE, Yang F, Zhang H, Walker FA, Vila AJ
Abstract
The electronic structure of heme proteins is exquisitely tuned...
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02-03-2013 10:19 AM
Dynamic nuclear polarization at high magnetic fields in liquids
Dynamic nuclear polarization at high magnetic fields in liquids
July 2012
Publication year: 2012
Source:Progress in Nuclear Magnetic Resonance Spectroscopy, Volume 64</br>
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Graphical abstract
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12-15-2012 09:51 AM
Dynamic nuclear polarization at high magnetic fields in liquids
Dynamic nuclear polarization at high magnetic fields in liquids
Publication year: 2011
Source:Progress in Nuclear Magnetic Resonance Spectroscopy</br>
C. Griesinger, M. Bennati, H.M. Vieth, C. Luchinat, G. Parigi, P. Höfer, F. Engelke, S.J. Glaser, V. Denysenkov, T.F. Prisner</br>
Graphical Abstract
http://ars.sciencedirect.com/content/image/1-s2.0-S0079656511000689-fx1.jpg Graphical abstract Highlights
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03-09-2012 09:16 AM
Dynamic Nuclear Polarization at High Magnetic Fields in Liquids
Dynamic Nuclear Polarization at High Magnetic Fields in Liquids
Publication year: 2011
Source: Progress in Nuclear Magnetic Resonance Spectroscopy, Available online 4 November 2011</br>
C.*Griesinger, M.*Bennati, H.M.*Vieth, C.*Luchinat, G.*Parigi, ...</br>
Highlights
? High field Dynamic Nuclear Polarization spectrometers for liquid samples have been constructed, working at 7, 9.2 and 14 T, respectively. ? The field dependence of the Overhauser DNP efficiency has been measured experimentally for the first time up to a field of 9.2 T and compared with experimental results from...