scholarly journals Dynamic nuclear polarization of quadrupolar nuclei using cross polarization from protons: surface-enhanced aluminium-27 NMR

2012 ◽  
Vol 48 (14) ◽  
pp. 1988 ◽  
Author(s):  
Veronika Vitzthum ◽  
Pascal Miéville ◽  
Diego Carnevale ◽  
Marc A. Caporini ◽  
David Gajan ◽  
...  
2015 ◽  
Vol 137 (43) ◽  
pp. 13964-13971 ◽  
Author(s):  
Laura Piveteau ◽  
Ta-Chung Ong ◽  
Aaron J. Rossini ◽  
Lyndon Emsley ◽  
Christophe Copéret ◽  
...  

2012 ◽  
Vol 4 (1) ◽  
pp. 111-114 ◽  
Author(s):  
Aurélien Bornet ◽  
Roberto Melzi ◽  
Angel J. Perez Linde ◽  
Patrick Hautle ◽  
Ben van den Brandt ◽  
...  

2018 ◽  
Vol 30 (4) ◽  
pp. 1344-1352 ◽  
Author(s):  
Sung Min Kim ◽  
Wei-Chih Liao ◽  
Agnieszka M. Kierzkowska ◽  
Tigran Margossian ◽  
Davood Hosseini ◽  
...  

The Analyst ◽  
2015 ◽  
Vol 140 (17) ◽  
pp. 5860-5863 ◽  
Author(s):  
Jean-Nicolas Dumez ◽  
Jonas Milani ◽  
Basile Vuichoud ◽  
Aurélien Bornet ◽  
Julie Lalande-Martin ◽  
...  

Natural abundance 13C 1D and 2D NMR spectra of biological extracts are recorded in a single scan for samples hyperpolarised by dissolution dynamic nuclear polarization combined with cross polarization.


2012 ◽  
Vol 134 (45) ◽  
pp. 18491-18494 ◽  
Author(s):  
Daniel Lee ◽  
Hiroki Takahashi ◽  
Aany S. L. Thankamony ◽  
Jean-Philippe Dacquin ◽  
Michel Bardet ◽  
...  

2021 ◽  
Author(s):  
Yunhua Chen ◽  
Rick Dorn ◽  
Michael Hanrahan ◽  
Lin Wei ◽  
Rafael Blome-Fernandez ◽  
...  

<p>Dynamic nuclear polarization (DNP) solid-state NMR (SSNMR) spectroscopy was used to obtain detailed surface structures of zinc blende CdSe nanocrystals (NCs) with plate or spheroidal morphologies and which are capped by carboxylic acid ligands. 1D <sup>113</sup>Cd and <sup>77</sup>Se cross-polarization magic angle spinning (CPMAS) NMR spectra revealed distinct signals from Cd and Se atoms on the surface of the NCs, and those residing in bulk-like environments below the surface. <sup>113</sup>Cd cross-polarization magic-angle-turning (CP-MAT) experiments identified CdSe<sub>3</sub>O, CdSe<sub>2</sub>O<sub>2</sub>, and CdSeO<sub>3</sub> Cd coordination environments on the surface of the NCs, where the oxygen atoms are presumably from coordinated carboxylate ligands. The sensitivity gain from DNP enabled natural isotopic abundance 2D homonuclear <sup>113</sup>Cd-<sup>113</sup>Cd and <sup>77</sup>Se-<sup>77</sup>Se and heteronuclear <sup>113</sup>Cd-<sup>77</sup>Se scalar correlation solid-state NMR experiments that reveal the connectivity of the Cd and Se atoms. Importantly, <sup>77</sup>Se{<sup>113</sup>Cd} scalar heteronuclear multiple quantum coherence (<i>J</i>-HMQC) experiments were used to selectively measure one-bond <sup>77</sup>Se-<sup>113</sup>Cd scalar coupling constants (<sup>1</sup><i>J</i>(<sup>77</sup>Se, <sup>113</sup>Cd)). With knowledge of <sup>1</sup><i>J</i>(<sup>77</sup>Se, <sup>113</sup>Cd), heteronuclear <sup>77</sup>Se{<sup>113</sup>Cd} spin echo (<i>J</i>-resolved) NMR experiments were then used to determine the number of Cd atoms bonded to Se atoms and vice versa. The <i>J</i>-resolved experiments directly confirmed that major Cd and Se surface species have CdSe<sub>2</sub>O<sub>2</sub> and SeCd<sub>4</sub> stoichiometries, respectively. Considering the crystal structure of zinc blende CdSe, and the similarity of the solid-state NMR data for the platelets and spheroids, we conclude that the surface of the spheroidal CdSe NCs is primarily composed of {100} facets. The methods outlined here will generally be applicable to obtain detailed surface structures of various main group semiconductors.</p>


2021 ◽  
Author(s):  
Stuart J. Elliott ◽  
Olivier Cala ◽  
Quentin Chappuis ◽  
Samuel Cousin ◽  
Morgan Ceillier ◽  
...  

<p>Dissolution-dynamic nuclear polarization can be boosted by employing multiplecontact cross-polarization techniques to transfer polarization from 1H to 13C spins. The method is efficient and significantly reduces polarization build-up times, however, it involves high-power radiofrequency pulses in a superfluid helium environment which limit its implementation and applicability and prevent a significant scaling-up of the sample size.</p> <p>We propose to overcome this limitation by a stepwise transfer of polarization using a lowenergy and low-peak power radiofrequency pulse sequence where the 1H®13C polarization transfer is mediated by a dipolar spin order reservoir. An experimental demonstration is presented for [1-13C]sodium acetate. A solid-state 13C polarization of ~43.5% was achieved using this method with a build-up time constant of ~5.1 minutes, leading to a ~28.5% 13C polarization in the liquidstate after sample dissolution. The low-power multiple-step polarization transfer efficiency with respect to the most advanced and highest-power multiple-contact cross-polarization approach was found to be ~0.69.</p>


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