A high-volume resonator for L-band DNP-NMR

IF 2 3区 化学 Q3 BIOCHEMICAL RESEARCH METHODS
Adam R. Altenhof , Qing Yang , Michal Kern , Shaun G. Newman , Jens Anders , Michael W. Malone
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Abstract

DNP-NMR and EPR experiments that operate at or greater than L-band (i.e., ν0(e) = 1–2 GHz) are typically limited to maximum sample volumes of several hundred µL. These experiments rely on well-known resonator designs for DNP/EPR irradiation such as the loop-gap resonator and Alderman-Grant coil, where their maximum volumes limit further application to imaging experiments and high-throughput screening beyond L-band. Herein, we demonstrate a birdcage (BC) resonator design that can accommodate several mL of sample while operating around 1.5 GHz. The sample volume is maximized by using two identical BC resonators in a stacked configuration. Simulations are used to optimize the BC design and the performance is validated experimentally with liquid-state Overhauser-DNP-NMR experiments. This BC design exploits just the parasitic capacitance of conductive rings and features no fixed tuning capacitors. An enhancement of −77 is achieved on a 10 mM 4-Amino-TEMPO in H2O sample for a 5 mL sample volume. The associated sample heating is minimal due to the low-E-fields generated and the large sample mass with +3.4 K when driving 100 W for several seconds.

Abstract Image

用于 L 波段 DNP-NMR 的大容量谐振器。
在 L 波段或更高波段(即 ν0(e-) = 1-2 GHz)运行的 DNP-NMR 和 EPR 实验通常仅限于几百微升的最大样品量。这些实验依赖于众所周知的 DNP/EPR 辐照谐振器设计,如环隙谐振器和奥尔德曼-格兰特线圈,它们的最大体积限制了成像实验和 L 波段以上高通量筛选的进一步应用。在这里,我们展示了一种鸟笼(BC)谐振器设计,它可以容纳几毫升样品,同时工作频率在 1.5 GHz 左右。通过在堆叠配置中使用两个相同的 BC 谐振器,最大限度地增加了样品体积。模拟用于优化 BC 设计,液态 Overhauser-DNP-NMR 实验验证了其性能。这种 BC 设计只利用了导电环的寄生电容,没有固定的调谐电容。在 5 mL 样品体积下,在 10 mM 4-Amino-TEMPO in H2O 样品上实现了 -77 的增强。由于产生的电场较低,且样品质量较大,在 100 W 的功率下持续数秒后,样品的加热温度为 +3.4 K,因此相关的样品加热温度极低。
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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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