The CW-EPR Capabilities of a Dual DNP/EPR Spectrometer Operating at 14 and 7 T

IF 2 3区 化学 Q3 BIOCHEMICAL RESEARCH METHODS Journal of magnetic resonance Pub Date : 2024-02-10 DOI:10.1016/j.jmr.2024.107635
Orit Nir-Arad, David H. Shlomi, Amit Israelstam, Tomer Amit, Nurit Manukovsky, Alexander B. Fialkov, Ilia Kaminker
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Abstract

High-field electron paramagnetic resonance (EPR) measurements are indispensable for a better understanding of dynamic nuclear polarization (DNP), which relies on polarization transfer between electron and nuclear spins. DNP experiments are typically performed at high > 7 T magnetic fields and low ≤ 100 K temperatures, while EPR instrumentation capable of EPR measurements under these conditions is scarce. In this paper, we describe the CW EPR capabilities of a dual DNP/EPR spectrometer that is designed to carry out EPR experiments under “DNP conditions” at 14 and 7 T. In the first part, we present the design of this instrument, highlighting the choices made to allow for both DNP and EPR operations. The spectrometer uses a sweepable cryogen-free magnet with NMR-grade homogeneity, a closed-cycle cooling system, a quasi-optical induction mode bridge, and a superheterodyne receiver system. The probe design is optimized for low heat load and fast sample exchange under cryogenic conditions. The spectrometer can operate in frequency and field sweep modes, including wide field sweeps using the main coil of the magnet. In the second part, we present EPR spectra acquired over a wide range of samples and operating conditions, illustrating the CW EPR capabilities of the instrument.

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在 14 和 7 T 下运行的双 DNP/EPR 光谱仪的 CW-EPR 功能
高场电子顺磁共振(EPR)测量对于更好地理解动态核极化(DNP)是不可或缺的,动态核极化依赖于电子和核自旋之间的极化转移。DNP 实验通常在高 > 7 T 的磁场和低≤ 100 K 的温度下进行,而能够在这些条件下进行 EPR 测量的 EPR 仪器却很少。在本文中,我们介绍了一台双 DNP/EPR 光谱仪的 CW EPR 功能,该仪器设计用于在 14 和 7 T 的 "DNP 条件 "下进行 EPR 实验。该光谱仪使用了具有核磁共振级均匀性的可扫描无低温磁铁、封闭循环冷却系统、准光感应模式桥和超外差接收器系统。探头设计经过优化,可在低温条件下实现低热负荷和快速样品交换。光谱仪可在频率和磁场扫描模式下运行,包括使用磁体的主线圈进行宽磁场扫描。在第二部分中,我们展示了在各种样品和操作条件下获得的 EPR 光谱,说明了该仪器的 CW EPR 功能。
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来源期刊
CiteScore
3.80
自引率
13.60%
发文量
150
审稿时长
69 days
期刊介绍: The Journal of Magnetic Resonance presents original technical and scientific papers in all aspects of magnetic resonance, including nuclear magnetic resonance spectroscopy (NMR) of solids and liquids, electron spin/paramagnetic resonance (EPR), in vivo magnetic resonance imaging (MRI) and spectroscopy (MRS), nuclear quadrupole resonance (NQR) and magnetic resonance phenomena at nearly zero fields or in combination with optics. The Journal''s main aims include deepening the physical principles underlying all these spectroscopies, publishing significant theoretical and experimental results leading to spectral and spatial progress in these areas, and opening new MR-based applications in chemistry, biology and medicine. The Journal also seeks descriptions of novel apparatuses, new experimental protocols, and new procedures of data analysis and interpretation - including computational and quantum-mechanical methods - capable of advancing MR spectroscopy and imaging.
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