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Development of High-Resolution NMR of Quadrupolar Nuclei and Trial Construction of the Spectrometer

四极核高分辨率核磁共振的研制及谱仪的试制

基本信息

批准号：
03504002
负责人：
TERAO Takehiko
金额：
$ 26.56万
依托单位：
KOYOTO UNIVERSITY
依托单位国家：
日本
项目类别：
Grant-in-Aid for Developmental Scientific Research (A)
财政年份：
1991
资助国家：
日本
起止时间：
1991 至 1993
项目状态：
已结题

来源：
https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-03504002/
关键词：
quadrupolar nuclei high-resolution solid-state NMR DAS-NMR 試料高速回転

项目摘要

1. A DAS-NMR-system was developed.2. A computer program for the pulse sequence of DAS-NMR, control of a motor system, and data manipulation, and also a simulation program of one-and two-dimensional spectra were developed to obtain and analyze experimental spectra.3. It was confirmed by carrying out DAS-NMR for ^<23>Na in Rochelle salt that the NMR system normally works. A resolution of 120 Hz was obtained by using proton decoupling.4. A simple and sensitive DAS-NMR method was developed which allows us to observe pure-absorption two-dimensional spectra.5. A new high-resolution NMR spectroscopy of quadrupolar nuclei was proposed which uses ultrasonic sound for dispersing powder in liquid and violently disturbing the particles, It was confirmed from a ^1H NMR study that linewidths become narrower by mixing glass particles.6. A method by which two-dimensional powder spectra for quadrupolar nuclei can be observed between two different spinning orientations was developed, and successfully applied to ^<27>Al of Rochelle salt.7. Details of static and dynamic behaviors of the guest molecules in beta-cyclodextrin/ferrocene and cholic acid/gamma-valerolactone inclusion compounds were studied by measuring temperature dependence of ^<13>C chemical shift powder patterns of the guest molecules using SASS spectroscopy.

1. 研制了das - nmr系统。开发了DAS-NMR脉冲序列、电机系统控制和数据处理的计算机程序，以及一维和二维光谱的仿真程序，以获取和分析实验光谱。通过对Rochelle盐中^<23>Na进行DAS-NMR，证实了核磁共振系统正常工作。采用质子解耦法获得了120 Hz的分辨率。建立了一种简单灵敏的DAS-NMR方法，使我们能够观察到纯吸收的二维光谱。提出了一种新的高分辨率的四极核磁共振波谱方法，该方法利用超声波将粉末分散在液体中，并对颗粒进行剧烈扰动，从^1H核磁共振研究中证实，混合玻璃颗粒会使线宽变窄。提出了一种在两种不同自旋取向间观察四极核二维粉末光谱的方法，并成功地应用于Rochelle盐的^<27>Al。通过SASS光谱测量客体分子^<13>C化学位移粉末模式的温度依赖性，研究了客体分子在β -环糊精/二铁和胆酸/ γ -戊内酯包合物中的静态和动态行为细节。