We present and discuss a sensitive spectroscopic means of detecting and quantifying network defects within a series of polysiloxane elastomers through a novel application of ¹⁹F solution state nuclear magnetic resonance (NMR). Polysiloxanes are the most utilized non-carbon polymeric material today. Their final network structure is complex, hierarchical, and often ill-defined due to modification. Characterization of these materials with respect to starting and age-dependent network structure is obfuscated by the intractable nature of polysiloxane network elastomers. We report a synthetic strategy for selectively tagging chain-end silanols with an organofluorine compound, which may then be conveniently and quantitatively measured as a function of structure and environment by means of ¹⁹F NMR. This study represents a new and sensitive means of directly quantifying aspects of network architecture in polysiloxane materials and has the potential to be a powerful new tool for the spectroscopic assessment of structural dynamic response in polysiloxane networks.

中文翻译：

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用于硅胶网络中纳米结构缺陷的检测和定量的NMR方法

我们提出并讨论了通过¹⁹ F溶液态核磁共振（NMR）的新颖应用来检测和量化一系列聚硅氧烷弹性体中网络缺陷的灵敏光谱方法。聚硅氧烷是当今使用最多的非碳聚合物材料。它们的最终网络结构是复杂的，分层的，并且由于修改而常常是不确定的。聚硅氧烷网络弹性体的难处理特性使这些材料相对于起始和与年龄有关的网络结构的表征变得模糊。我们报告了一种使用有机氟化合物选择性标记链端硅烷醇的合成策略，然后可以方便地和定量地根据结构和环境对化合物进行测量，方法是通过¹⁹1 H NMR。这项研究代表了一种直接量化聚硅氧烷材料中网络体系结构方面的新颖而灵敏的手段，并且有可能成为光谱分析聚硅氧烷网络中结构动力响应的有力新工具。