Park Sin Young, Cheong Won Jo
Department of Chemistry, Inha University, Namku, Incheon, South Korea.
J Sep Sci. 2015 Sep;38(17):2938-44. doi: 10.1002/jssc.201500465. Epub 2015 Jul 14.
This study introduces a preparation method for polymer-encased monolith frits with improved durability for liquid chromatography columns. The inner surface of the polyether ether ketone tubing is pretreated with sulfuric acid in the presence of catalysts (vanadium oxide and sodium sulfate). The tubing was rinsed with water and acetone, flushed with nitrogen, and treated with glycidyl methacrylate. After washing, the monolith reaction mixture composed of lauryl methacrylate, ethylene glycol dimethacrylate, initiator, and porogenic solvent was filled in the tubing and subjected to in situ polymerization. The tubing was cut into thin slices and used as frits for microcolumns. To check their durability, the frit slices were placed in a vial and a heavy impact was applied on the vial by a vortex mixer for various periods. The frits made in the presence of catalysts were found to be more durable than those made without catalysts. Furthermore, when the monolith-incorporated tubing was used as a chromatography column, the column prepared in the presence of catalysts resulted in a better separation efficiency. The separation performance of the columns installed with the polyether ether ketone encased monolith frits was comparable to that of the columns installed with the commercial stainless-steel screen frits.
本研究介绍了一种用于液相色谱柱的具有更高耐久性的聚合物包裹整体式筛板的制备方法。聚醚醚酮管的内表面在催化剂（氧化钒和硫酸钠）存在的情况下用硫酸进行预处理。该管先后用水和丙酮冲洗，用氮气吹扫，并用甲基丙烯酸缩水甘油酯处理。洗涤后，将由甲基丙烯酸月桂酯、乙二醇二甲基丙烯酸酯、引发剂和成孔溶剂组成的整体反应混合物填充到管中并进行原位聚合。将该管切成薄片用作微柱的筛板。为了检查它们的耐久性，将筛板薄片放入小瓶中，用涡旋混合器对小瓶施加不同时间段的强烈冲击。发现有催化剂存在下制备的筛板比无催化剂时制备的筛板更耐用。此外，当将包含整体的管用作色谱柱时，在催化剂存在下制备的柱具有更好的分离效率。安装有聚醚醚酮包裹整体式筛板的柱的分离性能与安装有商用不锈钢筛网筛板的柱相当。
