分析测试学报
分析測試學報
분석측시학보
JOURNAL OF INSTRUMENTAL ANALYSIS
2009年
12期
1373-1377
,共5页
半制备柱%柱效%稀匀浆法
半製備柱%柱效%稀勻漿法
반제비주%주효%희균장법
semi-preparative column%column efficiency%homogenate slurry method
对稀匀浆法填充半制备柱(Ф10 mm×100 mm)的过程进行研究,并用正交法对柱填充条件进行了优化,考察了压力、匀浆液组成、匀浆液体积对半制备柱填充效果的影响.由柱效和分离度定义式中的参数入手,讨论填充条件对柱性能的影响.通过计算总孔隙率ε_t、内部孔隙率ε_p、外部孔隙率ε_e、Van-Deemter曲线、吸附等温线等参数,发现填充压力对填充密度的作用最大,是最重要的影响因素;匀浆配比和匀浆体积共同影响其填充的均匀性.在压力11 MPa,流速275 mL/min,120 mL纯乙醇为匀浆液的条件下得到了最好的填充效果.
對稀勻漿法填充半製備柱(Ф10 mm×100 mm)的過程進行研究,併用正交法對柱填充條件進行瞭優化,攷察瞭壓力、勻漿液組成、勻漿液體積對半製備柱填充效果的影響.由柱效和分離度定義式中的參數入手,討論填充條件對柱性能的影響.通過計算總孔隙率ε_t、內部孔隙率ε_p、外部孔隙率ε_e、Van-Deemter麯線、吸附等溫線等參數,髮現填充壓力對填充密度的作用最大,是最重要的影響因素;勻漿配比和勻漿體積共同影響其填充的均勻性.在壓力11 MPa,流速275 mL/min,120 mL純乙醇為勻漿液的條件下得到瞭最好的填充效果.
대희균장법전충반제비주(Ф10 mm×100 mm)적과정진행연구,병용정교법대주전충조건진행료우화,고찰료압력、균장액조성、균장액체적대반제비주전충효과적영향.유주효화분리도정의식중적삼수입수,토론전충조건대주성능적영향.통과계산총공극솔ε_t、내부공극솔ε_p、외부공극솔ε_e、Van-Deemter곡선、흡부등온선등삼수,발현전충압력대전충밀도적작용최대,시최중요적영향인소;균장배비화균장체적공동영향기전충적균균성.재압력11 MPa,류속275 mL/min,120 mL순을순위균장액적조건하득도료최호적전충효과.
The semi-preparative columns(Ф10 mm×100 mm) were packed by homogenate slurry method.The packing conditions,such as pressure,packing solvent and homogenate volume were optimized by the orthogonal experiment.The influence of the packing conditions was discussed from the parameters of the column efficiency and the resolutions defining equation.The total porosity(ε_t),internal porosity(ε_p),external porosity(ε_e),Van-Deemter plot,adsorption isotherm were calculated.The result shows that pressure is the most important affecting factor for the density,and packing solvent and homogenate volume affect the homogeneity of the column.The best column in this experiment was obtained with 120 mL of ethanol as packing solvent under using pressure of 11 MPa and flow rate of 275 mL/min.