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核磁共振内标法测定聚酯羟值
http://www.100md.com 《分析化学》 2006年第5期
核磁共振,,核磁共振,聚酯,内标,羟值,摘要,关键词,1引言,2实验部分,3结果与讨论,References
     摘 要

    合成了14种不同组成的聚酯样品以考察聚酯端羟基αH的1H谱谱峰特点。利用聚酯端羟基αH的1H谱谱峰与聚酯其它峰互不干扰的特点,采用优化的1H谱脉冲序列和检测参数,以苯乙烯为内标,建立了一种用核磁共振1H谱检测聚酯端羟基αH在聚酯中的含量,再根据端羟基αH与羟基的比例关系求聚酯羟值的方法。结果显示,其测量的相对偏差小于1% ,测量精密度为±0.2。本方法简单、快速\,准确度高。

     关键词 核磁共振,聚酯,内标,羟值

    Measurement of Hydroxyl Value for Polyester by 1H Nuclear Magnetic ResonanceInternal Standard Method

    Wu Aiqin*, Yu Jing, Zhuang Jian, Ning Qiang

    (Qingdao Dinippon Ink Chemical Fine Chemicals Co.,Ltd. , Qingdao 266101)

    Abstract Fourteen kinds of polyesters were synthesized, which is to study the characteristics of terminal hydroxyl αH of polyester in 1H nuclear magnetic resonance (NMR) spectra. Utilizing the results that the peak of terminal hydroxyl αH of polyester does not interfere by other peaks of polyester, a new simple and sensitive method to determine the hydroxyl value of polyester by 1H NMR was established. In this method, a modified 1H NMR pulse sequence and improved parameters were adopted, and styrene was added as the internal standard. The investigated results show that the relative error of theoretica values and measured valuew in this method is lower than 1% and the precision is ±0.2. This method is characterized not only by simplicity and rapidity but also by high precision. ......

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