Development of a high resolution solid-steate NMR spectrometer and investigation dynamical behavior of organic molecules in the solid state.

开发高分辨率固态核磁共振波谱仪并研究固态有机分子的动力学行为。

基本信息

批准号：
02554016
负责人：
SUGAWARA Tadashi
金额：
$ 12.16万
依托单位：
University of Tokyo
依托单位国家：
日本
项目类别：
Grant-in-Aid for Developmental Scientific Research (B)
财政年份：
1990
资助国家：
日本
起止时间：
1990 至 1992
项目状态：
已结题

项目摘要

The purpose of the project is to produce a new type of a high resolution solid-state NMR spectrometer for investigating dynamical behavior of organic molecules in the solid state.1. The main instrumental problems to be innovated are as follows.(1) Optimize pulse frequencies in order to perform CRAMPS experiments (high resolution solid state ^1HNMR) by introducing a four-phase shifter and other hardwares.(2) Improve a lower limit of variable temperatures for CP/MAS experiments by modifying a cooling system of the probe.(3) Prepare a photo-transmission probe in order to irradiate a sample during CP/MAS measurements.The first problem was successfully solved. High resolution ^1H NMR spectra of maleic acid and citric acid were obtained with a resolution of 0.32 ppm. Technical solutions concerning to the latter two points were proposed, although instrumental modifications could not be achieved due to the financial condition.2. Utilizing the novel spectrometer, CP/MAS measurement were performed on solid samples to elucidate intriguing dynamical behaviors. Typical studies are as follows.(1) Investigate the solid state tautomerization of b-hydroxyenones which exhibit paraelectric and (anti)ferroelectric behaviors(2) Prepare new host molecules such as twin-donors or fused thiophenes and elucidate dynamical behaviors of guest molecules in inclusion complexes.(3) Prepare photolabile diacetylenes carrying a mesogenic group and monitor the photo-induced polymerization by CP/MAS measurements.In summery, novel physical properties and chemical reactions, which are derived from a dynamical behavior of organic molecules in the solid state, have been elucidated by using the newly developed high resolution solid state NMR spectrometer.

该项目的目的是生产一种新型的高分辨率固态NMR光谱仪，以研究固态下有机分子的动态行为1。（1）通过引入四相变速杆和其他硬件来执行抽筋实验（高分辨率固态 ^1HNMR），以执行脉冲实验（高分辨率固态 ^1HRMR）如下。 CP/MAS测量过程中的样本成功解决了第一个问题。高分辨率 ^1H NMR光谱是马来酸和柠檬酸的，分辨率为0.32 ppm。提出了有关后两点的技术解决方案，尽管由于财务状况无法实现工具的修改2。利用新的光谱仪，对固体样品进行了CP/MAS测量，以阐明有趣的动态行为。典型的研究如下。（1）研究表现出降压性和（抗）铁电行为的B-羟基苯乙烯的固态互变异（2）准备新的宿主分子，准备新的宿主分子，例如双胞胎或融合硫代的硫代苯甲酸酯，并阐明了糖尿病中的糖尿病分子的动态，使糖尿病的临床分子均准备好成情异物（3））（3）（3）（3）并通过使用新开发的高分辨率固态NMR光谱仪来阐明，并通过CP/MAS测量来监测通过CP/MAS测量值监测夏季的新型物理特性和化学反应。