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Development of analytical system of composition- and molecular weight-distributions for organic functional materials

有机功能材料组成和分子量分布分析系统的开发

基本信息

批准号：
03650604
负责人：
MORI Sadao
金额：
$ 1.28万
依托单位：
Mie University
依托单位国家：
日本
项目类别：
Grant-in-Aid for General Scientific Research (C)
财政年份：
1991
资助国家：
日本
起止时间：
1991 至 1992
项目状态：
已结题

项目摘要

The purpose of this research project has been the development of the analytical system to measure both the composition- and molecular weight distributions independently each other and successively. Temperature descending adsorption chromatography (TDAC) was designed and preheater tubing and a by-pass column were connected in a column-oven of the TDAC system. The performance of the system was estimated with styrene-methyl methacrylate copolymers. The mobile phase was a mixture of 1,2-dichlo-roethane and ethanol and a silica gel column was connected in the column-oven as the stationary phase. Column temperature at the begining was 60 ﾟC and a sample solution was injected into the system. The column temperature was decreased from 60 ﾟC to room temperature every 5 ﾟC and the fraction at each column temperature was monitored with UV detectors. Two UV detectors at 260 nm and 233 nm were used to monitor the effluent from the column: the wavelength at 260 nm was used to measure the composition and that at 233 nm the content of the copolymers. The results showed that the copolymers were separated according to their composition. Next step was to connect the size exclusion chromatography (SEC) system to the TDAC system. The effluent from the TDAC column at each column temperature was then introduced to the SEC system directly and molecular weight and molecular weight distribution of the copolymers were thus determined. With this TDAC-SEC system, both distributions, composition and molecular weight, could be measured directly without any fractionation technique.

该研究项目的目的是开发分析系统，以相互独立地连续测量组成和分子量分布。设计了降温吸附色谱（TDAC）系统，并在TDAC系统的柱温箱中连接预热管和旁通柱。用苯乙烯-甲基丙烯酸甲酯共聚物评价了该体系的性能。移动的相为1，2-三氯乙烷和乙醇的混合物，硅胶柱连接在柱温箱中作为固定相。开始时柱温为60 ℃，并将样品溶液注入系统中。柱温每隔5 ℃从60 ℃降至室温，并用UV检测器监测各柱温下的馏分。使用260 nm和233 nm处的两个UV检测器来监测来自柱的流出物：260 nm处的波长用于测量共聚物的组成，233 nm处的波长用于测量共聚物的含量。结果表明，共聚物按其组成分离。下一步是将尺寸排阻色谱（SEC）系统连接至TDAC系统。然后将在每个柱温下来自TDAC柱的流出物直接引入SEC系统，从而测定共聚物的分子量和分子量分布。利用该TDAC-SEC系统，可以直接测量分布、组成和分子量，而无需任何分级技术。