毛细管干凝胶整体色谱柱的制备及其应用-分析化学专业毕业论文.docxVIP

燥过程中不会发生柱床断裂和塌陷，此特点明显优于以烷氧基硅烷 燥过程中不会发生柱床断裂和塌陷，此特点明显优于以烷氧基硅烷 为前驱体制备无机整体柱的方法。比较了不同模数硅酸钾对整体柱柱 床结构的影响，采用扫描电镜(SEM)和氮吸附法对整体柱结构进行 了表征，并考察了整体柱柱压与流速的关系。对整体柱进行十八烷基 修饰后，测定了反相整体柱(C18整体柱)对葸的柱效，通过考察甲 苯在该柱上的突破曲线，获得了其对甲苯的柱容量。结果表明该整体 柱柱床刚性好，在高温、高柱压、高流速条件下能保持其物理结构的 稳定性，对葸的柱效达到41400塔板数／米，对甲苯的柱容量为6．1xlO。2 岭o 3、采用制备的C18硅胶整体柱作为固相微萃取柱对水质中苯类 及氯苯类化合物进行萃取富集，然后将其解吸后利用气相色谱进行检 测分析，证实了该整体柱的实用性。 4、将C18硅胶整体柱与商品化的固相微萃取柱进行萃取富集比 较，结合气相色谱分析，考察了萃取温度、萃取时间、离子强度以及 存放时间对萃取效率的影响，提示该柱可进一步扩展到挥发性水质污 染物分析的采样及长时间储存。 关键词：硅胶整体柱；C。8键合；表征；固相微萃取；气相色谱 II AbstractIt Abstract It is difficult to realize high effective and rapid separation by using the chromatographic columns packing traditional porous microspheres． By reducing the size of porous microspheres materials，chromatographic columns can obtain higher efficiency in a short period of time． Nevertheless，the chromatographic column filled with the smaller particles can result in the increase of back pressure inevitably,which Can cause the design and manufacture of chromatographic apparatus more difficult．Since 1 990s，the monolithic column technology has been developed to overcome the problem of high-pressure caused by the usage of smaller particles．Monolithic column is a continuous bed stationary phase prepared by in。situ polymerization of organic or inorganic polymer, which has the advantages of simple preparation procedure，high ratio of through pore，low backpressure，high specific surface and sharp separation．Due to the excellent properties，such as high mechanical strength，low column back pressure and good column stability,monolithic column prepared by silica material has been applied in high throughput analysis and high effective separation and it plays more important role in separation and analysis． There are two ways of preparation of monolithic silica column．One is that employing sol-gel technology to prepare it using alkoxy silane as the precursor．Another is that preparing monolithic silica column via in—suit polymerization using potassium silicate and f