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High-Temperature and High-Pressure In situ Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy

High-Temperature and High-Pressure In situ Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy

Published on: October 9, 2020

High-field pulsed EPR spectroscopy under magic angle spinning.

Orit Nir-Arad¹, Alexander B Fialkov¹, David H Shlomi¹

¹School of Chemistry, Tel-Aviv University, 6997801 Tel-Aviv, Israel.

Science Advances

|August 30, 2024

Summary

This study presents the first pulsed electron paramagnetic resonance (EPR) experiments using magic angle spinning (MAS) at high magnetic fields. These advancements enable new investigations into electron spin dynamics crucial for dynamic nuclear polarization (DNP) mechanisms.

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Area of Science:

Physics
Chemistry
Spectroscopy

Background:

Electron paramagnetic resonance (EPR) is typically performed at low magnetic fields.
Magic angle spinning (MAS) and high magnetic fields enhance sensitivity and resolution in Nuclear Magnetic Resonance (NMR) and Dynamic Nuclear Polarization (DNP).
Investigating DNP mechanisms requires understanding electron spin dynamics under DNP-relevant conditions, which has been experimentally limited.

Purpose of the Study:

To perform the first pulsed EPR experiments under magic angle spinning (MAS) at high magnetic fields.
To overcome instrumental challenges that have historically prevented MAS-EPR at high fields.
To provide experimental data on electron spin dynamics under conditions relevant to DNP.

Main Methods:

Development and implementation of a dedicated, homebuilt MAS-EPR probehead.
Conducting pulsed EPR experiments under MAS at a high magnetic field (7 tesla).
Recording and analyzing pulsed MAS-EPR spectra of P1 center diamond defects.
Utilizing time-domain simulations to interpret spectral changes.

Main Results:

Demonstration of successful pulsed EPR experiments under MAS at high magnetic field.
Observation of unique effects of MAS on EPR line shape, intensity, and signal dephasing.
P1 center diamond defect spectra recorded at 7 tesla revealed MAS-induced spectral alterations.
Time-domain simulations accurately reproduced observed line shape changes and intensity trends.

Conclusions:

Pulsed MAS-EPR at high magnetic fields is now feasible, overcoming significant instrumental hurdles.
MAS significantly influences EPR spectral characteristics, including line shape, intensity, and dephasing.
This technique provides crucial experimental insights into electron spin dynamics relevant for DNP mechanism studies.