ANALYSIS OF MIXTURES BASED ON MOLECULAR-SIZE AND HYDROPHOBICITY BY MEANS OF DIFFUSION-ORDERED 2D NMR

ANALYSIS OF MIXTURES BASED ON MOLECULAR-SIZE AND HYDROPHOBICITY BY MEANS OF DIFFUSION-ORDERED 2D NMR
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DOI:
10.1021/ac00074a006
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发表时间:
1994-01-15
影响因子:
7.4
通讯作者:
JOHNSON, CS
JOHNSON, CS
中科院分区:
化学1区
文献类型:
--
作者:
MORRIS, KF;STILBS, P;JOHNSON, CS

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扩散有序二维核磁共振波谱 (DOSY) 已应用于水性混合物的分析。脉冲场梯度核磁共振 (PFG-NMR) 实验采用特殊措施进行,以尽量减少脉冲感应涡流的影响,并在数据采集期间进行样品旋转。 FT PFG-NMR 数据集使用数据反演程序 SPLMOD 进行处理,以根据通常与分子大小相关的扩散系数解析和识别溶质。然后构建等值线图,其中传统的一维核磁共振谱在一维中显示,而扩散谱在另一维中显示。除非两种组分具有基本相同的扩散系数,否则可以获得分子种类的完全分辨率。添加浓度高于其临界胶束浓度的表面活性剂可以根据溶质在形成的胶束中的溶解程度进行解析。 DOSY 被证明是研究平衡的有力工具,涉及比以前认为可以通过传统 PFG-NMR 方法实现的更为复杂的系统中的结合、吸收和分配。
Diffusion-ordered 2D NMR spectroscopy (DOSY) has been applied to the analysis of aqueous mixtures. Pulsed field gradient NMR (PFG-NMR) experiments were performed with special provisions for minimizing the effects of pulse-induced eddy currents and with sample spinning during the data acquisition period. The FT PFG-NMR data sets were processed with the data inversion program SPLMOD to resolve and identify the solutes on the basis of diffusion coefficients that normally are related to molecular size. Contour plots were then constructed in which conventional 1D NMR spectra were displayed in one dimension and diffusion spectra in the other. Complete resolution of molecular species was obtained except when two components had essentially identical diffusion coefficients. The addition of surfactants at concentrations above their critical micelle concentrations permitted solutes to be resolved on the basis of their degree of solubilization in the micelles formed. DOSY is shown to be a powerful tool for the study of equilibria involving binding, absorption, and partitioning in more complex systems than previously considered accessible by conventional PFG-NMR methods.