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Dissolution Dynamic Nuclear Polarization Instrumentation for Real-time Enzymatic Reaction Rate Measurements by NMR

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Room-Temperature Pulsed Dynamic Nuclear Polarization at 7 T.

Alexander A Nevzorov¹, Sergey Milikisiyants¹, Antonin Marek¹

¹Department of Chemistry, North Carolina State University, 2620 Yarbrough Drive, Raleigh, North Carolina 27695-8204, United States.

The Journal of Physical Chemistry Letters

|May 20, 2025

Summary

This summary is machine-generated.

Pulsed dynamic nuclear polarization (DNP) at high magnetic fields (7 T) was achieved using a novel ESR/NMR spectrometer. This technique enhanced natural-abundance 13C NMR signals by up to 800-fold in synthetic diamond.

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Area of Science:

Magnetic Resonance
Spectroscopy
Quantum Information Science

Background:

Pulsed dynamic nuclear polarization (DNP) significantly enhances Nuclear Magnetic Resonance (NMR) signals.
Previous pulsed DNP methods were limited to low magnetic fields.
High magnetic fields (≥7 T) present challenges in generating sufficient microwave (mm-wave) fields (B1e) for pulsed DNP.

Purpose of the Study:

To develop and demonstrate a novel Electron Spin Resonance (ESR)/NMR spectrometer for pulsed DNP at 7 T.
To overcome technical challenges in generating high-amplitude mm-wave B1e fields.
To achieve significant NMR signal enhancement for natural-abundance 13C in synthetic diamond.

Main Methods:

Designed and constructed a first-of-its-kind ESR/NMR spectrometer operating at 7 T.
Employed a pulsed extended interaction klystron and piezo-tunable photonic-band gap resonators (Q ≈ 1500) to generate B1e fields of ~75 MHz.
Utilized phase-sensitive electronic detection for enhanced sensitivity.

Main Results:

Achieved room-temperature Nuclear Overhauser Effect (NOE) dynamic nuclear polarization (DNP) with signal gains up to 800 for a 30 μm synthetic diamond crystal.
Demonstrated simultaneous coherent manipulation of electron and nuclear spins via 13C-detected electron Rabi nutations.
Successfully generated high-amplitude mm-wave B1e fields required for pulsed DNP at 7 T.

Conclusions:

The developed 7 T ESR/NMR spectrometer enables high-performance pulsed DNP.
This advancement significantly enhances NMR sensitivity for challenging samples like natural-abundance 13C.
The system allows for coherent control of coupled electron-nuclear spin systems.