Rossini, A.J., et al., One hundred fold overall sensitivity enhancements for Silicon-29 NMR spectroscopy of surfaces by dynamic nuclear polarization with CPMG acquisition. Chemical Science, 2012. 3(1): p. 108-115.
Dynamic nuclear polarization (DNP) 29Si solid-state NMR spectra of a hybrid mesoporous silica material impregnated with aqueous biradical solutions have been acquired with cross-polarization (CP) and cross-polarization Carr-Purcell Meiboom-Gill (CP/CPMG) pulse sequences. The integrated intensities (II) and signal to noise ratios (S/N) of the 29Si solid-state NMR spectra are monitored in order to measure the DNP enhancement factors (?Si CP) as well as the overall sensitivity enhancement ([capital Sigma]Si CP) available from the combination of DNP and CPMG acquisition. Here, , where [small theta]Si is a factor which quantifies reduction of the NMR signal by paramagnetic effects (quenching) and [small kappa] is the square root of the ratio of nuclear longitudinal relaxation times of the dry material and material impregnated with radical solution. It is found that [capital Sigma]Si CP is always substantially lower than the measured value of ?Si CP due to paramagnetic effects which reduce the II of the 29Si CP solid-state NMR spectra at high biradical concentrations. In this system, it is observed that the sample preparation which provides optimal DNP signal enhancement does not provide optimal overall signal enhancement. Notably, optimal signal enhancements are obtained for CPMG acquisition of the 29Si solid-state NMR spectra when lower radical concentrations are employed due to slower transverse relaxation rates. To the best of our knowledge this is the first study which seeks to quantify the overall sensitivity enhancements available from DNP solid-state NMR experiments.
Analysis of sensitivity enhancement by dynamic nuclear polarization in solid-state NMR: a case study of functionalized mesoporous materials
From The DNP-NMR Blog:
Analysis of sensitivity enhancement by dynamic nuclear polarization in solid-state NMR: a case study of functionalized mesoporous materials
Kobayashi, T., et al., Analysis of sensitivity enhancement by dynamic nuclear polarization in solid-state NMR: a case study of functionalized mesoporous materials. Phys Chem Chem Phys, 2013. 15(15): p. 5553-62.
http://www.ncbi.nlm.nih.gov/pubmed/23459985
nmrlearner
News from NMR blogs
0
04-17-2013 08:15 PM
Analysis of sensitivity enhancement by dynamic nuclear polarization in solid-state NMR: a case study of functionalized mesoporous materials
From the The DNP-NMR Blog:
Analysis of sensitivity enhancement by dynamic nuclear polarization in solid-state NMR: a case study of functionalized mesoporous materials
Kobayashi, T., et al., Analysis of sensitivity enhancement by dynamic nuclear polarization in solid-state NMR: a case study of functionalized mesoporous materials. Phys Chem Chem Phys, 2013. 15(15): p. 5553-62.
http://www.ncbi.nlm.nih.gov/pubmed/23459985
nmrlearner
News from NMR blogs
0
04-15-2013 08:52 AM
Dynamic Nuclear Polarization Enhanced Natural Abundance 17O Spectroscopy
From the The DNP-NMR Blog:
Dynamic Nuclear Polarization Enhanced Natural Abundance 17O Spectroscopy
Blanc, F., et al., Dynamic Nuclear Polarization Enhanced Natural Abundance 17O Spectroscopy. J. Am. Chem. Soc., 2013. 135(8): p. 2975-2978.
http://dx.doi.org/10.1021/ja4004377
nmrlearner
News from NMR blogs
0
04-15-2013 08:52 AM
Dynamic nuclear polarization-enhanced 13C NMR spectroscopy of static biological solids
Dynamic nuclear polarization-enhanced 13C NMR spectroscopy of static biological solids
Available online 27 February 2013
Publication year: 2013
Source:Journal of Magnetic Resonance</br>
</br>
We explore the possibility of using dynamic nuclear polarization (DNP) to enhance signals in structural studies of biological solids by solid state NMR without sample spinning. Specifically, we use 2D 13C-13C exchange spectroscopy to probe the peptide backbone torsion angles (?,?) in a series of selectively 13C-labeled 40-residue ?-amyloid (A ?1-40) samples, in both fibrillar and...
nmrlearner
Journal club
0
02-28-2013 07:57 PM
Enhanced Solid-State NMR Correlation Spectroscopy of Quadrupolar Nuclei Using Dynamic Nuclear Polarization
Enhanced Solid-State NMR Correlation Spectroscopy of Quadrupolar Nuclei Using Dynamic Nuclear Polarization
Daniel Lee, Hiroki Takahashi, Aany S. L. Thankamony, Jean-Philippe Dacquin, Michel Bardet, Olivier Lafon and Gae?l De Pae?pe
http://pubs.acs.org/appl/literatum/publisher/achs/journals/content/jacsat/0/jacsat.ahead-of-print/ja307755t/aop/images/medium/ja-2012-07755t_0004.gif
Journal of the American Chemical Society
DOI: 10.1021/ja307755t
http://feeds.feedburner.com/~ff/acs/jacsat?d=yIl2AUoC8zA
http://feeds.feedburner.com/~r/acs/jacsat/~4/NcXbDBD9aBc
nmrlearner
Journal club
0
11-03-2012 03:56 PM
Fast Characterization of Functionalized Silica Materials by Silicon-29 Surface-Enhanced NMR Spectroscopy Using Dynamic Nuclear Polarization
Fast Characterization of Functionalized Silica Materials by Silicon-29 Surface-Enhanced NMR Spectroscopy Using Dynamic Nuclear Polarization
Moreno Lelli, David Gajan, Anne Lesage, Marc A. Caporini, Veronika Vitzthum, Pascal Mie?ville, Florent He?roguel, Fernando Rasco?n, Arthur Roussey, Chloe? Thieuleux, Malika Boualleg, Laurent Veyre, Geoffrey Bodenhausen, Christophe Cope?ret and Lyndon Emsley
http://pubs.acs.org/appl/literatum/publisher/achs/journals/content/jacsat/0/jacsat.ahead-of-print/ja110791d/aop/images/medium/ja-2010-10791d_0005.gif
Journal of the American Chemical Society...
nmrlearner
Journal club
0
02-01-2011 06:33 AM
Surface Enhanced NMR Spectroscopy by Dynamic Nuclear Polarization
Surface Enhanced NMR Spectroscopy by Dynamic Nuclear Polarization
Anne Lesage, Moreno Lelli, David Gajan, Marc A. Caporini, Veronika Vitzthum, Pascal Mie?ville, Johan Alauzun, Arthur Roussey, Chloe? Thieuleux, Ahmad Medhi, Geoffrey Bodenhausen, Christophe Cope?ret and Lyndon Emsley
http://pubs.acs.org/appl/literatum/publisher/achs/journals/content/jacsat/0/jacsat.ahead-of-print/ja104771z/aop/images/medium/ja-2010-04771z_0004.gif
Journal of the American Chemical Society
DOI: 10.1021/ja104771z
http://feeds.feedburner.com/~ff/acs/jacsat?d=yIl2AUoC8zA...
nmrlearner
Journal club
0
09-11-2010 01:25 AM
Dynamic nuclear polarization-enhanced solid-state NMR spectroscopy of GNNQQNY nanocry
Dynamic nuclear polarization-enhanced solid-state NMR spectroscopy of GNNQQNY nanocrystals and amyloid fibrils.
http://www.ncbi.nlm.nih.gov/corehtml/query/egifs/http:--www.rsc.org-images-entities-char_z_RSClogo.gif Related Articles Dynamic nuclear polarization-enhanced solid-state NMR spectroscopy of GNNQQNY nanocrystals and amyloid fibrils.
Phys Chem Chem Phys. 2010 Jun 14;12(22):5911-9
Authors: Debelouchina GT, Bayro MJ, van der Wel PC, Caporini MA, Barnes AB, Rosay M, Maas WE, Griffin RG
Dynamic nuclear polarization (DNP) utilizes the...