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首页> 外文期刊>Applied Magnetic Resonance >Complexes Based on Calix[4]arene Sulfonic Acid with Acetic Acid and Its Derivatives: NMR Analysis
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Complexes Based on Calix[4]arene Sulfonic Acid with Acetic Acid and Its Derivatives: NMR Analysis

机译：基于CALIX [4]芳烃磺酸的复合物及其衍生物：NMR分析

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Calix[4]arene sulfonic acid complexes with acetic acid CH3COOH and its derivatives CCl3COOH, CF3COOH were studied by nuclear magnetic resonance (NMR). The formation of guest-host type complexes was shown by magic angle spinning (MAS) NMR and high-resolution NMR techniques. Increase in calixarene molecule conformational flexibility with moisture content rising was observed by C-13 MAS NMR. Consequently, CCl3COOH, CF3COOH molecules vacate calixarene cavity at relative humidity RH 33%. While the complex with CH3COOH remains stable up to RH=64%. The self-diffusion processes were investigated by H-1 pulsed field gradient technique. Spin-echo attenuation curves show non-exponential shape indicating the occurrence of several phases with a different translational mobility. The existence CCl3COOH, CF3COOH acid molecules inside the calixarene cavity leads to average self-diffusion coefficient Dsaver reduction compared with pure calix[4]arene sulfonic acid. The values of Dsaver for the CH3COOH complex are close to average self-diffusion coefficient of calix[4]arene sulfonic acid. From Dsaver proton conductivities sigma(calc) on the basis of the Nernst-Einstein equation were calculated. Calculated sigma(calc) and experimental sigma(exp) conductivities are agreed well in the RH range from 33% to 75%. At low water content (RH=10%) sigma(exp) isabout one order of magnitude less compare with sigma(calc) in calixarene and its complexes with CH3COOH and CCl3COOH. It may be explained by low conductivity boundary formation at these conditions between grains in process of target sample preparation for conductivity measurement.
机译：Calix [4]通过核磁共振（NMR）研究了乙酸CH3COOH及其衍生物CCL3COOH的芳烃磺酸配合物，CCL3COOH，CF 3核酸。通过魔法角度旋转（MAS）NMR和高分辨率NMR技术表示旨在级宾馆类型复合物的形成。 C-13 Mas NMR观察到钙喹分子的增加与水分含量上升的柔韧性。因此，CCl3COOH，CF3COOH分子在相对湿度RH和GT的相对湿度RH＆GT; 33％的钙葡萄腔。虽然与CH3COOH的复合物保持稳定至rH = 64％。通过H-1脉冲场梯度技术研究了自扩散过程。旋转回波衰减曲线显示非指数形状，表示具有不同平移移动性的几个阶段的发生。钙含有腔内的CCL3COOH，CCL3COOH，CF3COOH酸分子导致平均自扩散系数DSAVER与纯胶砜[4]芳烃磺酸相比。 CH 3 COOH复合物的DSAVER的值接近胶胶中的平均自扩散系数[4]芳烃磺酸。从Dsaver质子电导率计算，基于NERNST-EINSTEIN方程的SIGMA（CAP）计算。计算的Sigma（Calc）和实验性Sigma（EXP）导体在RH范围内均匀约为33％至75％。在低含水量（RH = 10％）SIGMA（EXP）中，依数级别比钙喹（CCl3COOH和CCL3COOH）的锡酮（Calc）与Sigma（Calc）进行比较。可以通过低导电性边界形成在谷物之间的这些条件下进行导电性测量的靶样样品制剂的方法。

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