利用体积排阻快速原位表征整体固定相的孔结构

Rapid Determination the Pore Structure of Monolithic Stationary Phases by Size-Exclusion Chromatography

利用体积排阻色谱原理,在自制的径向色谱柱上,测定了具有窄分子量分布且已知平均分子量418～190000的聚苯乙烯标准品的保留数据,这些数据可用于计算柱子的外部(55.1%)、内部(4.9%)和总孔隙率以及整体材料孔尺寸分布的信息。此种技术用于整体填料孔结构的表征,具有无破坏性、原位、快速的特点。整体固定相的外部和总孔隙率高于颗粒填充柱,表明整体柱的高通透性;流速与压力关系的分析,证明了整体固定相在高流速下具有低背压的特征。

Retention data of polystyrene samples of narrow molecular size distribution and known average molecular mass from 418 to 190 000 were measured on radial flow monolithic column by size-exclusion chromatography (SEC). These data were used to determine the external (55.1%), internal (4.9%), and total porosities of the column. These data provided also information on the pore-size distribution of the adsorbent medium. The SEC applied in the determination of the pore structure possesses the characteristics of speediness, easiness, in-situ and nondestructive. The external and the total porosities of the column are much higher than those of conventional packed columns. The results illustrate the high penetrability and low pressure drop even in the case of high mobile phase flow velocities.