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Frequency-Swept Integrated and Stretched Solid Effect Dynamic Nuclear Polarization

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Specialty Chemistry
Date 2018 May 15
PMID 29756781
Citations 12
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Abstract

We investigate a new time domain approach to dynamic nuclear polarization (DNP), the frequency-swept integrated solid effect (FS-ISE), utilizing a high power, broadband 94 GHz (3.35 T) pulse EPR spectrometer. The bandwidth of the spectrometer enabled measurement of the DNP Zeeman frequency/field profile that revealed two dominant polarization mechanisms, the expected ISE, and a recently observed mechanism, the stretched solid effect (SE). At 94 GHz, despite the limitations in the microwave chirp pulse length (10 μs) and the repetition rate (2 kHz), we obtained signal enhancements up to ∼70 for the SE and ∼50 for the ISE. The results successfully demonstrate the viability of the FS-ISE and SE DNP at a frequency 10 times higher than previous studies. Our results also suggest that these approaches are candidates for implementation at higher magnetic fields.

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References
1.
Spindler P, Schops P, Kallies W, Glaser S, Prisner T . Perspectives of shaped pulses for EPR spectroscopy. J Magn Reson. 2017; 280:30-45. DOI: 10.1016/j.jmr.2017.02.023. View

2.
Hunter R, Cruickshank P, Bolton D, Riedi P, Smith G . High power pulsed dynamic nuclear polarisation at 94 GHz. Phys Chem Chem Phys. 2010; 12(22):5752-6. DOI: 10.1039/c002251a. View

3.
Smith A, Corzilius B, Bryant J, DeRocher R, Woskov P, Temkin R . A 140 GHz pulsed EPR/212 MHz NMR spectrometer for DNP studies. J Magn Reson. 2012; 223:170-9. PMC: 3459153. DOI: 10.1016/j.jmr.2012.07.008. View

4.
Corzilius B, Smith A, Griffin R . Solid effect in magic angle spinning dynamic nuclear polarization. J Chem Phys. 2012; 137(5):054201. PMC: 3422330. DOI: 10.1063/1.4738761. View

5.
Lange S, Franks W, Rajagopalan N, Doring K, Geiger M, Linden A . Structural analysis of a signal peptide inside the ribosome tunnel by DNP MAS NMR. Sci Adv. 2016; 2(8):e1600379. PMC: 4991931. DOI: 10.1126/sciadv.1600379. View