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辛基型毛细管液相色谱整体柱的制备、表征及评价 被引量:4

Preparation Characterization and Evaluation of Octyl-type MonolithicColumn for Capillary Liquid Chromatography
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摘要 本研究采用以甲基丙烯酸辛酯为单体,乙二醇二甲基丙烯酸酯为交联剂,偶氮二异丁腈为引发剂,正丙醇、1, 4丁二醇和水三元混合物为共溶剂,制备了内径为0. 53mm的毛细管整体柱材料。详细考察了单体/交联剂比例、单体混合物与致孔剂之间的比例,对所制得材料的通透性、孔径分布、粒度大小等性能的影响;应用包括扫描电镜和压汞法对其进行表征;在毛细管液相色谱(c HPLC)操作模式进行了初步色谱评价,结果表明:所制得的整体柱具有优良的通透性能,可在高达100μL/min的流速下进行快速分离,同时在离子对模式下对3种金属离子进行了分离,取得了较理想的效果。 A series of monolithic capillary columns (0. 53 mm i. d.) were prepared for capillary high performance liquid chromatography (c-HPLC) by in-situ copolymerization of octyl methacrylate and ethylenedimethacrylate ( EDMA) in the presence of a porogen solvent containing 1-propanol, 1,4-butanol and water. The influences of the contents of the porogen solvent and EDMA in the polymerization mixture on the morphology, porosity and globule size were investigated. The morphology and pore size distribution of monolithic capillary columns were characterized by scanning electorn microscopy and mercury intrusion porosimetry, respectively. Chromatographic evaluations of the columns were performed under c-HPLC model. The results show that good permeability can be obtained under optimal experimental conditions, which result in a flow rate upto 100 μ L/min for fast separation. Three metal ions were also separated under ion-pair model on the new monolithic capillary column and the results were acceptable.
出处 《分析化学》 SCIE EI CAS CSCD 北大核心 2005年第4期467-470,共4页 Chinese Journal of Analytical Chemistry
基金 国家自然科学基金面上项目 (No. 20175019 ) 高等学校博士学科点专项科研基金 (No. 20040384002 ) 厦门市科技创新基金(No. 3502Z20031058) 中国博士后科学基金 (No. 2003034438) 厦门大学预研基金 (No. 2003sdyy08)资助
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