下行式匀浆法填充细内径毛细管液相色谱柱  

Preparation of small-diameter capillary liquid chromatography columns using downward packing method

作　　者：石蒙 时佳荣 常洋洋 张强[2] 刘猛 SHI Meng;SHI Jiarong;CHANG Yangyang;ZHANG Qiang;LIU Meng(School of Environmental Science and Technology,Key Laboratory of Industrial Ecology and Environmental Engineering(Ministry of Education),Dalian University of Technology,Dalian,116024,China;School of Bioengineering,Dalian University of Technology,Dalian,116024,China)

机构地区：[1]大连理工大学环境学院,工业生态与环境工程教育部重点实验室,大连116024 [2]大连理工大学生物工程学院,大连116024

出　　处：《环境化学》2023年第8期2651-2658,共8页Environmental Chemistry

基　　金：国家自然科学基金(21922601,21777013)资助.

摘　　要：本文采用下行式匀浆法填充内径为25-250μm,有效长度为100 mm和150 mm的毛细管液相色谱柱,填料为3μm C18修饰的多孔硅球.经实验条件优化,匀浆溶剂是体积比为9:1丙酮/甲醇,匀浆浓度的变化范围为5-30 mg·mL^(−1).在此条件下,色谱柱的柱效随柱内径减小而提高.通过比较Van Deemter方程中A、B和C项系数与毛细管内径之间的关系发现,随着柱内径减小,A项的系数呈线性减小的趋势,B和C项的系数与内径无明显关系.在最佳流速下,内径为25μm毛细管柱的折合塔板高度低至2.25,接近理论塔板高度.We developed a downward packing method for preparing the efficient capillary column with inner diameters(i.d.)from 25-250µm in the effective length of 100-150 mm.The columns were packed by 3μm of C18 modified silica particles with 5-30 mg·mL^(−1) slurries in acetone/methanol(9:1,V/V).In this condition,the column efficiency was increased as the diameter of the column decreased.By comparing the coefficients of A,B and C term in the Van Deemter equation with the inner diameters of the capillary columns,we found the coefficient of A term decreased linearly with decreasing the i.d.of the column.However,there is no linear relationship between the coefficients of the B and C terms with the i.d.of the column.At the optimum reduced velocity,the hmin(the minimum plate height)of the 25μm i.d.column was as low as 2.25,which is very close to the theoretical plate(HETP).

关 键 词：下行法 毛细管柱 柱效 VAN Deemter 方程 

分 类 号：O652.63[理学—分析化学]