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Design of a measuring system of minute differential pressure by capillary and application to analysis of chemical state of polymeric materials

毛细管微差压测量系统设计及其在高分子材料化学状态分析中的应用

基本信息

批准号：
06650933
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：
1994
资助国家：
日本
起止时间：
1994 至 1995
项目状态：
已结题

项目摘要

The measuring system designed consisted of two capillaries of the same size (0.5 mm i.d. and 40 cm in length) ; one for the mobile phase and the other for both the mobile phase and the sample solution. Two differential pressure transducers were installed at the both ends of capillaries. Amplifier for the difference of the output of two transducer was prepared. Mobile phase was flowed with a pump and the amount of the sample solutions injected was 3 ml. Several polystiren solutions of different molecular weight and different concentrations were prepared and diffrential pressure was measured. From the plot of differential pressure and sample concentration, intrinsic viscosities of the polystirene samples were calculated. From the measurement of the differential pressure of polystirene samples of narrow molecular weight distributions, Mark-Houwink-Sakurada parameters were measured. Molecular weights of polystirene samples were calculated using these parameters and intrisic viscosities and the results were in good aggreament to the vendor values. Similary the parameters of polyvinyl chloride were measured. Sample concentrations of polyvinyl chloride had to be 1/10 to the usual ones and the viscosity measurement of such dilute solutions was possible only this system. Comparison of the performance of the system with an Ubelohde glass capillary viscometer showed that this system was superior to the latter viscometer on the points of analysis time, sample volume, and precision. This measuring system was connected to the SEC system and molecular weight averages of polystirenes were measured. The measurement was capable after minor modification in the system and the results were in good agreement with the usual relative method. The system investigated here can be used as the molecular sensitive detector for SEC.

所设计的测量系统由两个相同尺寸（0.5mm i. d.）的毛细管组成。和40 cm长）;一个用于移动的相，另一个用于移动的相和样品溶液。在毛细管的两端安装了两个差压传感器。研制了双传感器输出差放大器。用泵使移动的相流动，样品溶液的注入量为3 ml。制备了几种不同分子量、不同浓度的聚苯乙烯溶液，测定了其压差。从差压和样品浓度的曲线图，计算聚苯乙烯样品的特性粘度。通过测量窄分子量分布的聚苯乙烯样品的压差，测量了Mark-Houwink-Sakurada参数。使用这些参数和特性粘度计算了聚苯乙烯样品的分子量，结果与供应商的值吻合良好。并对聚氯乙烯的相关参数进行了测定。聚氯乙烯的样品浓度必须是通常浓度的1/10，只有该系统才能测量这种稀溶液的粘度。与Ubelohde玻璃毛细管粘度计的性能比较表明，该系统在分析时间、样品体积和精密度方面上级后者。将该测量系统与SEC系统连接，并测量聚苯乙烯的分子量平均值。对该系统进行了微小的改进后，可用于测定，其结果与常用的相关方法一致。该体系可作为SEC的分子灵敏检测器。