Determination of self-diffusion coefficients in mixtures with benchtop 13C NMR spectroscopy via polarization transfer

IF 1.9 3区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY
Johnnie Phuong, Sarah Mross, Daniel Bellaire, Hans Hasse, Kerstin Münnemann
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Abstract

Nuclear magnetic resonance (NMR) is an established method to determine self-diffusion coefficients in liquids with high precision. The development of benchtop NMR spectrometers makes the method accessible to a wider community. In most cases, 1H NMR spectroscopy is used to determine self-diffusion coefficients due to its high sensitivity. However, especially when using benchtop NMR spectrometers for the investigation of complex mixtures, the signals in 1H NMR spectra can overlap, hindering the precise determination of self-diffusion coefficients. In 13C NMR spectroscopy, the signals of different compounds are generally well resolved. However, the sensitivity of 13C NMR is significantly lower than that of 1H NMR spectroscopy leading to very long measurement times, which makes diffusion coefficient measurements based on 13C NMR practically infeasible with benchtop NMR spectrometers. To circumvent this problem, we have combined two known pulse sequences, one for polarization transfer from 1H to the 13C nuclei (PENDANT) and one for the measurement of diffusion coefficients (PFG). The new method (PENPFG) was used to measure the self-diffusion coefficients of three pure solvents (acetonitrile, ethanol and 1-propanol) as well as in all their binary mixtures and the ternary mixture at various compositions. For comparison, also measurements of the same systems were carried out with a standard PFG-NMR routine on a high-field NMR instrument. The results are in good agreement and show that PENPFG is a useful tool for the measurement of the absolute value of the self-diffusion coefficients in complex liquid mixtures with benchtop NMR spectrometers.

Abstract Image

Abstract Image

偏振转移台式13c核磁共振光谱法测定混合物自扩散系数。
核磁共振(NMR)是一种成熟的高精度测定液体自扩散系数的方法。台式核磁共振光谱仪的发展使该方法可被更广泛的社区使用。在大多数情况下,由于其高灵敏度,采用1h核磁共振谱法来确定自扩散系数。然而,特别是在使用台式核磁共振光谱仪研究复杂混合物时,1 H核磁共振光谱中的信号可能重叠,阻碍了自扩散系数的精确测定。在13c核磁共振光谱中,不同化合物的信号通常被很好地分解。然而,13c核磁共振的灵敏度明显低于1h核磁共振光谱,导致测量时间很长,这使得基于13c核磁共振的扩散系数测量在台式核磁共振光谱仪上实际上是不可实现的。为了解决这个问题,我们结合了两个已知的脉冲序列,一个用于从1h到13c核的极化转移(PENDANT),另一个用于扩散系数的测量(PFG)。采用新方法(PENPFG)测定了三种纯溶剂(乙腈、乙醇和1-丙醇)及其所有二元混合物和不同组成的三元混合物的自扩散系数。为了进行比较,在高场核磁共振仪上使用标准PFG-NMR程序进行了相同系统的测量。结果吻合良好,表明PENPFG是用台式核磁共振光谱仪测量复杂液体混合物中自扩散系数绝对值的有用工具。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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来源期刊
CiteScore
4.70
自引率
10.00%
发文量
99
审稿时长
1 months
期刊介绍: MRC is devoted to the rapid publication of papers which are concerned with the development of magnetic resonance techniques, or in which the application of such techniques plays a pivotal part. Contributions from scientists working in all areas of NMR, ESR and NQR are invited, and papers describing applications in all branches of chemistry, structural biology and materials chemistry are published. The journal is of particular interest not only to scientists working in academic research, but also those working in commercial organisations who need to keep up-to-date with the latest practical applications of magnetic resonance techniques.
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