Suppr超能文献

动态核极化是否增强了固态核磁共振?

Is solid-state NMR enhanced by dynamic nuclear polarization?

作者信息

Lee Daniel, Hediger Sabine, De Paëpe Gaël

机构信息

Univ. Grenoble Alpes, INAC, SCIB, F-38000 Grenoble, France; CEA, INAC, SCIB, F-38000 Grenoble, France.

Univ. Grenoble Alpes, INAC, SCIB, F-38000 Grenoble, France; CEA, INAC, SCIB, F-38000 Grenoble, France; CNRS, SCIB, F-38000 Grenoble, France.

出版信息

Solid State Nucl Magn Reson. 2015 Apr-May;66-67:6-20. doi: 10.1016/j.ssnmr.2015.01.003. Epub 2015 Feb 7.

Abstract

The recent trend of high-field (5-20 T), low-temperature (100 K) ssNMR combined with dynamic nuclear polarization (DNP) under magic angle spinning (MAS) conditions is analyzed. A brief overview of the current theory of hyperpolarization for so-called MAS-DNP experiments is given, along with various reasons why the DNP-enhancement, the ratio of the NMR signal intensities obtained in the presence and absence of microwave irradiation suitable for hyperpolarization, should not be used alone to gauge the value of performing MAS-DNP experiments relative to conventional ssNMR. This is demonstrated through a dissection of the current conditions required for MAS-DNP with particular attention to resulting absolute sensitivities and spectral resolution. Consequently, sample preparation methods specifically avoiding the surplus of glass-forming solvents so as to improve the absolute sensitivity and resolution are discussed, as are samples that are intrinsically pertinent for MAS-DNP studies (high surface area, amorphous, and porous). Owing to their pertinence, examples of recent applications on these types of samples where chemically-relevant information has been obtained that would have been impossible without the sensitivity increases bestowed by MAS-DNP are also detailed. Additionally, a promising further implementation for MAS-DNP is exampled, whereby the sensitivity improvements shown for (correlation) spectroscopy of nuclei at low natural isotopic abundance, facilitate internuclear distance measurements, especially for long distances (absence of dipolar truncation). Finally, we give some speculative perspectives for MAS-DNP.

摘要

分析了近期在魔角旋转(MAS)条件下,高场(约5 - 20 T)、低温(约100 K)的固态核磁共振(ssNMR)与动态核极化(DNP)相结合的趋势。简要概述了所谓MAS - DNP实验的超极化当前理论,以及为何DNP增强(即在存在和不存在适用于超极化的微波辐射情况下获得的NMR信号强度之比)不应单独用于衡量相对于传统ssNMR进行MAS - DNP实验的价值的各种原因。通过剖析MAS - DNP所需的当前条件,特别关注由此产生的绝对灵敏度和光谱分辨率来证明这一点。因此,讨论了专门避免过量玻璃形成溶剂以提高绝对灵敏度和分辨率的样品制备方法,以及对MAS - DNP研究本质相关的样品(高表面积、无定形和多孔)。由于它们的相关性,还详细介绍了近期在这些类型样品上的应用实例,在这些实例中获得了化学相关信息,而如果没有MAS - DNP赋予的灵敏度提高,这些信息是不可能获得的。此外,举例说明了MAS - DNP的一种有前景的进一步实施方案,即对于低天然同位素丰度的核的(相关)光谱显示出的灵敏度提高,有助于核间距离测量,特别是对于长距离(不存在偶极截断)。最后,我们给出了一些关于MAS - DNP的推测性观点。

文献AI研究员

20分钟写一篇综述,助力文献阅读效率提升50倍。

立即体验

用中文搜PubMed

大模型驱动的PubMed中文搜索引擎

马上搜索

文档翻译

学术文献翻译模型,支持多种主流文档格式。

立即体验