Spherical silica nanoparticles of various particle sizes ( approximately 10 to 100 nm), produced by a modified Stoeber method employing amino acids as catalysts, are investigated using Dynamic Nuclear Polarization (DNP) enhanced Nuclear Magnetic Resonance (NMR) spectroscopy. This study includes ultra-sensitive detection of surface-bound amino acids and their supramolecular organization in trace amounts, exploiting the increase in NMR sensitivity of up to three orders of magnitude via DNP. Moreover, the nature of the silicon nuclei on the surface and the bulk silicon nuclei in the core (sub-surface) is characterized at atomic resolution. Thereby, we obtain unique insights into the surface chemistry of these nanoparticles, which might result in improving their rational design as required for promising applications, e.g. as catalysts or imaging contrast agents. The non-covalent binding of amino acids to surfaces was determined which shows that the amino acids not just function as catalysts but become incorporated into the nanoparticles during the formation process. As a result only three distinct Q-types of silica signals were observed from surface and core regions. We observed dramatic changes of DNP enhancements as a function of particle size, and very small particles (which suit in vivo applications better) were hyperpolarized with the best efficiency. Nearly one order of magnitude larger DNP enhancement was observed for nanoparticles with 13 nm size compared to particles with 100 nm size. We determined an approximate DNP penetration-depth ( approximately 4.2 or approximately 5.7 nm) for the polarization transfer from electrons to the nuclei of the spherical nanoparticles. Faster DNP polarization buildup was observed for larger nanoparticles. Efficient hyperpolarization of such nanoparticles, as achieved in this work, can be utilized in applications such as magnetic resonance imaging (MRI).
First tests of a 527 GHz gyrotron for dynamic nuclear polarization
From The DNP-NMR Blog:
First tests of a 527 GHz gyrotron for dynamic nuclear polarization
Felch, K., et al. First tests of a 527 GHz gyrotron for dynamic nuclear polarization. in Vacuum Electronics Conference (IVEC), 2013 IEEE 14th International. 2013.
http://dx.doi.org/10.1109/IVEC.2013.6571048
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09-02-2013 10:45 PM
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
Dynamic Nuclear Polarization of Sedimented Solutes
From the The DNP-NMR Blog:
Dynamic Nuclear Polarization of Sedimented Solutes
Ravera, E., et al., Dynamic Nuclear Polarization of Sedimented Solutes. J. Am. Chem. Soc., 2013. 135(5): p. 1641-1644.
http://dx.doi.org/10.1021/ja312553b
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04-15-2013 08:52 AM
Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25K
Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25K
January 2013
Publication year: 2013
Source:Journal of Magnetic Resonance, Volume 226</br>
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We describe an apparatus for solid state nuclear magnetic resonance (NMR) with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS) at 20–25K and 9.4Tesla. The MAS NMR probe uses helium to cool the sample space and nitrogen gas for MAS drive and bearings, as described earlier , but also includes a corrugated waveguide for transmission of microwaves from...
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12-15-2012 09:51 AM
Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25 K
Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25 K
Available online 20 November 2012
Publication year: 2012
Source:Journal of Magnetic Resonance</br>
</br>
We describe an apparatus for solid state nuclear magnetic resonance (NMR) with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS) at 20-25 K and 9.4 Tesla. The MAS NMR probe uses helium to cool the sample space and nitrogen gas for MAS drive and bearings, as described earlier (Thurber et al., J. Magn. Reson. 2008) , but also includes a...
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12-01-2012 06:10 PM
Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25 K
Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25 K
Publication year: 2012
Source:Journal of Magnetic Resonance</br>
Kent R. Thurber, Alexey Potapov, Wai-Ming Yau, Robert Tycko</br>
We describe an apparatus for solid state nuclear magnetic resonance (NMR) with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS) at 20-25 K and 9.4 Tesla. The MAS NMR probe uses helium to cool the sample space and nitrogen gas for MAS drive and bearings, as described earlier (Thurber et al., J. Magn. Reson. 2008) ,...