scholarly journals J-driven Dynamic Nuclear Polarization for sensitizing high field solution state NMR

2022 ◽  
Author(s):  
Maria Grazia Concilio ◽  
Ilya Kuprov ◽  
Lucio Frydman
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Solid State ◽  
Magnetic Resonance ◽  
Dynamic Nuclear Polarization ◽  
Liquid State ◽  
High Field ◽  
Nuclear Polarization ◽  
Solution State ◽  
Field Solution ◽  
Nmr Sensitivity

Dynamic nuclear polarization (DNP) is widely used to enhance solid state nuclear magnetic resonance (NMR) sensitivity. Its efficiency as a generic signal-enhancing approach for liquid state NMR, however, decays rapidly...

Large volume liquid state scalar Overhauser dynamic nuclear polarization at high magnetic field

2019 ◽  
Vol 21 (38) ◽  
pp. 21200-21204 ◽  
Author(s):  
Thierry Dubroca ◽  
Sungsool Wi ◽  
Johan van Tol ◽  
Lucio Frydman ◽  
Stephen Hill
Keyword(s):  
Magnetic Field ◽  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Magnetic Fields ◽  
High Magnetic Field ◽  
Dynamic Nuclear Polarization ◽  
Large Volume ◽  
Liquid State ◽  
Nuclear Polarization ◽  
High Magnetic Fields

Dynamic Nuclear Polarization (DNP) can increase the sensitivity of Nuclear Magnetic Resonance (NMR), but it is challenging in the liquid state at high magnetic fields.

scholarly journals Solid-State <sup>1</sup>H Spin Polarimetry by <sup>13</sup>CH<sub>3</sub> Nuclear Magnetic Resonance

2021 ◽  
Author(s):  
Stuart J. Elliott ◽  
Quentin Stern ◽  
Sami Jannin
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Solid State ◽  
Magnetic Resonance ◽  
Microwave Irradiation ◽  
Dynamic Nuclear Polarization ◽  
Thermal Equilibrium ◽  
Sodium Acetate ◽  
Nuclear Polarization ◽  
Nuclear Magnetic ◽  
Dissolution Dynamic Nuclear Polarization

Abstract. Dissolution-dynamic nuclear polarization is emerging as a promising means to prepare proton polarizations approaching unity. At present, 1H polarization quantification remains fastidious due to the requirement of measuring thermal equilibrium signals. Lineshape polarimetry of solid-state nuclear magnetic resonance spectra is used to determine a number of useful properties regarding the spin system under investigation. In the case of highly polarized nuclear spins, such as those prepared under the conditions of dissolution-dynamic nuclear polarization experiments, the absolute polarization of a particular isotopic species within the sample can be directly inferred from the characteristics of the corresponding resonance lineshape. In situations where direct measurements of polarization are complicated by deleterious phenomena, indirect estimates of polarization using coupled heteronuclear spins prove informative. We present a simple analysis of the 13C spectral lineshape asymmetry of [2-13C]sodium acetate based on relative peak intensities, which can be used to indirectly evaluate the proton polarization of the methyl group moiety, and very likely the entire sample in the case of rapid and homogeneous 1H-1H spin diffusion. 1H polarizations greater than ~10–25 % (depending on the sign of the microwave irradiation) were found to be linearly proportional to the 13C peak asymmetry, which responds differently to positive or negative microwave irradiation. These results suggest that, as a dopant, [2-13C]sodium acetate could be used to indirectly gauge 1H polarizations in standard sample formulations, which is potentially advantageous for: samples polarized in commercial dissolution-dynamic nuclear polarization devices that lack 1H radiofrequency hardware, measurements which are deleteriously influenced by radiation damping or complicated by the presence of large background signals, and situations where the acquisition of a thermal equilibrium spectrum is not feasible.

scholarly journals Solid-state <sup>1</sup>H spin polarimetry by <sup>13</sup>CH<sub>3</sub> nuclear magnetic resonance

2021 ◽  
Vol 2 (2) ◽  
pp. 643-652
Author(s):  
Stuart J. Elliott ◽  
Quentin Stern ◽  
Sami Jannin
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Solid State ◽  
Magnetic Resonance ◽  
Dynamic Nuclear Polarization ◽  
Line Shape ◽  
Thermal Equilibrium ◽  
Sodium Acetate ◽  
Nuclear Polarization ◽  
Centre Of Gravity ◽  
Dissolution Dynamic Nuclear Polarization

Abstract. Dissolution dynamic nuclear polarization is used to prepare nuclear spin polarizations approaching unity. At present, 1H polarization quantification in the solid state remains fastidious due to the requirement of measuring thermal equilibrium signals. Line shape polarimetry of solid-state nuclear magnetic resonance spectra is used to determine several useful properties regarding the spin system under investigation. In the case of highly polarized nuclear spins, such as those prepared under the conditions of dissolution dynamic nuclear polarization experiments, the absolute polarization of a particular isotopic species within the sample may be directly inferred from the characteristics of the corresponding resonance line shape. In situations where direct measurements of polarization are complicated by deleterious phenomena, indirect estimates of polarization using coupled heteronuclear spins prove informative. We present a simple analysis of the 13C spectral line shape of [2-13C]sodium acetate based on the normalized deviation of the centre of gravity of the 13C peaks, which can be used to indirectly evaluate the proton polarization of the methyl group moiety and very likely the entire sample in the case of rapid and homogeneous 1H–1H spin diffusion. For the case of positive microwave irradiation, 1H polarization was found to increase with an increasing normalized centre of gravity deviation. These results suggest that, as a dopant, [2-13C]sodium acetate could be used to indirectly gauge 1H polarizations in standard sample formulations, which is potentially advantageous for (i) samples polarized in commercial dissolution dynamic nuclear polarization devices that lack 1H radiofrequency hardware, (ii) measurements that are deleteriously influenced by radiation damping or complicated by the presence of large background signals and (iii) situations where the acquisition of a thermal equilibrium spectrum is not feasible.

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