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作 者:马继平[1] 陈令新[1] 朱道乾[1] 关亚风[1]
机构地区:[1]中国科学院大连化学物理研究所
出 处:《色谱》2003年第4期430-433,共4页Chinese Journal of Chromatography
基 金:国家自然科学基金资助项目(20075030).
摘 要:制备液相色谱柱柱头筛板的选择直接影响到样品在柱头的分配情况及色谱柱柱效的高低。利用柱后可见 紫外检测,比较了采用多孔聚四氟乙烯材料和多孔烧结不锈钢材料作为台锥形制备液相色谱柱柱头筛板材料时的柱效;用柱上可视化方法研究了柱头筛板的直径对流型的影响。结果表明,多孔聚四氟乙烯的变形使得采用该材料做柱间筛板的色谱柱柱效比使用多孔不锈钢筛板的色谱柱柱效低约40%;样品流经直径小于柱入口内径的筛板导致样品在柱头分配不均,而流经直径与柱入口内径相同的筛板时因受到的阻力相同,可以实现柱塞状进样。还观察到不同直径的筛板导致不同的流型。使用直径与色谱柱入口内径相同的筛板可以提高柱效约20%。The inlet frit of preparative liquid chromatographic column influences the distr ibution of samples on the column header, the flow profile of sample band and col umn efficiency. By Vis-UV detector, column efficiencies of conically shaped preparative chromatographic columns with porous polytetrafluor oethylene (PTFE) frit and porous stainless steel frit were compared. The effect of the inside diameter of the frit on the column header on flow profile was stud ied by on-column visualization method. The results showed that the resulting co lumn efficiencies with the PTFE frit were lower than that of the porous stainl ess steel fri t by 40% because of the distortion of the porous PTFE frit. The distr ibution of sample on the column header was not uniform when the sample flowed th ro ugh a frit that had a smaller diameter than the column inlet inner diameter (ID) . However, the resistance force on the frit was uniform when the sample flowed t hrough a frit that had the same diameter as the column inlet ID, so the f low profile at initial moment was plug-like at the exit of the frits. Differen t flow profiles were produced by using different ID of frits. About 20% higher column efficiency could be obtained by using the same frit ID as that of the col umn inlet.
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