Diethanolamine/DMSO-d₆ as a viscous binary solvent is first reported for the individualization of low-polarity mixture components by multidimensional heteronuclear ViscY NMR experiments under spin diffusion conditions. Solvent viscosity induces the slowing down of molecular tumbling, hence promoting magnetization transfer by dipolar longitudinal cross-relaxation. As a result, all ¹H nuclei resonances within the same molecule may correlate in a 2D nuclear Overhauser effect spectroscopy (NOESY) spectrum, giving access to mixture analysis. We offer a new way to analyze mixtures by considering 3D heteronuclear heteronuclear single-quantum coherence–NOESY (HSQC-NOESY) experiments under viscous conditions. We state the individualization of four low-polarity chemical compounds dissolved in the diethanolamine/DMSO-d₆ solvent blend using homonuclear selective 1D, 2D ¹H–¹H NOESY experiments and heteronuclear 1D, 2D ¹H–¹⁹F heteronuclear Overhauser effect spectroscopy, 2D ¹H–¹⁹F, ¹H–³¹P HSQC-NOESY, and 3D ¹H–¹⁹F–¹H, ¹H–³¹P–¹H HSQC-NOESY experiments by taking profit from spin diffusion.

中文翻译：

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使用二乙醇胺作为粘性溶剂进行多维异核 ViscY NMR 实验的混合物分析

首次报道了二乙醇胺/DMSO- d ₆作为粘性二元溶剂，通过自旋扩散条件下的多维异核ViscY NMR 实验对低极性混合物组分进行个体化。溶剂粘度导致分子翻滚减慢，因此通过偶极纵向交叉弛豫促进磁化转移。结果，所有¹同一分子内的 H 核共振可能与二维核 Overhauser 效应光谱 (NOESY) 光谱相关，从而可以进行混合物分析。我们通过考虑粘性条件下的 3D 异核异核单量子相干-NOESY (HSQC-NOESY) 实验，提供了一种分析混合物的新方法。我们使用同核选择性 1D、2D ¹ H– ¹ H NOESY 实验和异核 1D、2D ¹ H– ¹⁹ F 异核 Overhauser 效应光谱来说明溶解在二乙醇胺/DMSO- d ₆溶剂混合物中的四种低极性化合物的个体化， 2D ¹ H– ¹⁹ F, ¹ H– ³¹P HSQC-NOESY 和 3D ¹ H– ¹⁹ F– ¹ H、¹ H– ³¹ P– ¹ H HSQC-NOESY 实验通过从自旋扩散中获利。