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通过核磁共振进行的磁化率测量:1. 四甲基硅烷的温度依赖性。

Magnetic susceptibility measurement by NMR: 1. The temperature dependence of TMS.

作者信息

Hoffman Roy E

机构信息

Institute of Chemistry, The Hebrew University of Jerusalem, Edmond Y. Safra Campus, Jersualem 9190401, Israel.

出版信息

J Magn Reson. 2020 Mar;312:106689. doi: 10.1016/j.jmr.2020.106689. Epub 2020 Jan 29.

Abstract

Usually a dedicated susceptometer is needed to measure diamagnetism accurately. An NMR spectrometer is more readily available in most chemistry departments but till now has been inaccurate for measuring diamagnetism. An improved NMR method is introduced to measure the magnetic susceptibility, or diamagnetism with similar absolute accuracy as other methods. This is achieved by accurate modelling of the NMR sample shape and response profile of the probe. The new method is validated by comparing the measured diamagnetism of water against the literature standard to within 0.05%. As a first example of its application, the diamagnetism of CDCl was measured over a range of temperatures and used to reanalyze earlier measurements of the variation of the chemical shift of tetramethylsilane in CDCl against He gas. This improved on the accuracy and reliability of the result and will allow, for the first time, accurate studies of the absolute effect of temperature on chemical shift.

摘要

通常需要一台专用的磁化率测量仪来精确测量抗磁性。在大多数化学系,核磁共振光谱仪更容易获得,但到目前为止,它在测量抗磁性方面并不准确。本文介绍了一种改进的核磁共振方法来测量磁化率,即抗磁性,其绝对精度与其他方法相似。这是通过对核磁共振样品形状和探头响应曲线进行精确建模来实现的。通过将测量的水的抗磁性与文献标准进行比较,验证了新方法的准确性在0.05%以内。作为其应用的第一个例子,在一系列温度范围内测量了CDCl的抗磁性,并用于重新分析之前关于CDCl中四甲基硅烷相对于氦气的化学位移变化的测量结果。这提高了结果的准确性和可靠性,并将首次允许对温度对化学位移的绝对影响进行精确研究。

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