Cryogenic sample eject system for electron paramagnetic resonance spectrometers

IF 1.9 3区 化学 Q3 BIOCHEMICAL RESEARCH METHODS Journal of magnetic resonance Pub Date : 2025-01-01 DOI:10.1016/j.jmr.2024.107823
Karl Rieger, Joshua Hoy, Timothy J. Keller, Thorsten Maly
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Abstract

We present a fully automated cryogenic sample insertion and ejection system for use with low-temperature EPR probes. We show how the system can be implemented on a conventional EPR spectrometer and that ejection and insertion is reliably possible at temperatures down to 10 K. Furthermore, we investigate the glass properties of a 0.1 mM sample of TEMPO in d8-glycerol/D2O (25/75, v/v) by measuring the electron phase memory time Tm in addition to determining the effective spin concentration from a PELDOR/DEER background trace. These experiments were done either using the sample eject system or samples that were manually flash frozen. We show that using the ejection system we can consistently obtain a better glass matrix as indicated by the longer Tm times and the lower effective concentrations.

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电子顺磁共振波谱仪低温样品喷射系统。
我们提出了一种全自动低温样品插入和喷射系统,用于低温EPR探针。我们展示了该系统如何在传统的EPR光谱仪上实现,并且在低至10 K的温度下可靠地进行弹射和插入。此外,我们研究了0.1 mM的TEMPO样品在d8-甘油/D2O (25/75, v/v)中的玻璃性质,除了通过PELDOR/DEER背景痕量测定有效自旋浓度外,还通过测量电子相记忆时间Tm。这些实验要么使用样品弹出系统,要么使用手动快速冷冻的样品。我们表明,使用喷射系统,我们可以始终如一地获得更好的玻璃基体,这表明了较长的Tm时间和较低的有效浓度。
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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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