An NMR thermometer for cryogenic magic-angle spinning NMR: The spin-lattice relaxation of 127I in cesium iodide

2011 ◽  
Vol 212 (2) ◽  
pp. 460-463 ◽  
Author(s):  
Riddhiman Sarkar ◽  
Maria Concistrè ◽  
Ole G. Johannessen ◽  
Peter Beckett ◽  
Mark Denning ◽  
...  
Author(s):  
ASIF EQUBAL ◽  
Kan Tagami ◽  
Songi Han

In this paper, we report on an entirely novel way of improving the MAS-DNP efficiency by shaped μw pulse train irradiation for fast and broad-banded (FAB) saturation of the electron spin resonance. FAB-DNP achieved with Arbitrary Wave Generated shaped μw pulse trains facilitates effective and selective saturation of a defined fraction of the total electron spins, and provides superior control over the DNP efficiency under MAS. Experimental and quantum-mechanics based numerically simulated results together demonstrate that FAB-DNP significantly outperforms CW-DNP when the EPR-line of PAs is broadened by conformational distribution and exchange coupling. We demonstrate that the maximum benefit of FAB DNP is achieved when the electron spin-lattice relaxation is fast relative to the MAS frequency, i.e. at higher temperatures and/or when employing metals as PAs. Calculations predict that under short T<sub>1e </sub>conditions AWG-DNP can achieve as much as ~4-fold greater enhancement compared to CW-DNP.


Molecules ◽  
2020 ◽  
Vol 25 (8) ◽  
pp. 1812
Author(s):  
Ae Ran Lim

The thermal, physical, and molecular dynamics of layered hybrid type (C2H5NH3)2MCl4 (M = 59Co, 63Cu, 65Zn, and 113Cd) crystals were investigated by thermogravimetric analysis (TGA) and magic angle spinning nuclear magnetic resonance (MAS NMR) spectroscopy. The temperatures of the onset of partial thermal decomposition were found to depend on the identity of M. In addition, the Bloembergen–Purcell–Pound curves for the 1H spin-lattice relaxation time T1ρ in the rotating frames of CH3CH2 and NH3, and for the 13C T1ρ of CH3 and CH2 were shown to exhibit minima as a function of the inverse temperature. These results confirmed the rotational motion of 1H and 13C in the C2H5NH3 cation. Finally, the T1ρ values and activation energies Ea obtained from the 1H measurements for the H‒Cl···M (M = Zn and Cd) bond in the absence of paramagnetic ions were larger than those obtained for the H‒Cl···M (M = Co and Cu) bond in the presence of paramagnetic ions. Moreover, the Ea value for 13C, which is distant from the M ions, was found to decrease upon increasing the mass of the M ion, unlike in the case of the Ea values for 1H.


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