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  • 學位論文

SBA-15中孔徑分子篩於高效能液相層析靜相之應用

Application of SBA-15 mesoporous molecular sieves on HPLC stationary phase

指導教授 : 鄭吉豐
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摘要


摘要 本論文旨在研究,如何同時控制中孔徑分子篩SBA-15的顆粒大小及孔徑大小,並將中孔徑分子篩的表面修飾後作為靜相填充材料,探討其於HPLC分離多苯環混合物上的應用。 在同時控制SBA-15的顆粒大小及孔徑大小方面,首先簡單的利用改變其反應溫度,來控制其顆粒大小,平均粒徑在1.0?8.5μm之間;而改變其後處理溫度,來控制其孔徑大小,孔徑在5?9nm之間;由於後處理溫度並不會影響其顆粒大小,因此可同時控制其反應溫度及後處理溫度來合成出範圍內顆粒大小及孔徑大小之中孔徑分子篩SBA-15,使其應用更加廣泛。 另外將合成出不同顆粒大小及孔徑大小之中孔徑分子篩,經修飾後填充至管柱中,可應用於HPLC方面。經修飾後的中孔徑分子篩皆可分離多苯環混合物,更進一步探討顆粒大小及孔徑大小對層析的影響,發現當靜相顆粒較小時,會促使分析物進入孔洞中作分離,而有較佳的分離效果;與商業用的填充材料作比較,得知因自製的填充材料具規則性孔洞及孔徑大小分佈範圍小,而有較好的分離效果。也將不同碳鏈長的修飾劑修飾於其表面上,發現修飾劑的碳鏈長度對分離效果的影響相當大,且與動相的極性也有所關連,而較長碳鏈者有較好的分離效果,其較佳到較差的排序是C18?C8> Cph> C3,當靜相的碳鏈較長時,因其表面的極性較小,須調整動相極性成較為非極性,即可得較佳之分析圖譜。

關鍵字

中孔徑分子篩

並列摘要


Abstract The particle size and pore size of mesoporous silica SBA-15 can be controlled by reaction temperature and thermal treatment temperature. The current study shows that SBA-15 with different particle size is prepared at different reaction temperatures of the initial gel mixture. All products have well defined hexagonal structure at these reaction temperatures. The reasonable formation model of particle size control is proposed. Furthermore, when increasing the thermal treatment temperature the pore size of SBA-15 increases from 5.17 to 9.37 nm without affecting original particle size SBA-15. A novel method for controlling both particle size and pore size of SBA-15 in a pot is developed successfully. SBA-15 mesoporous silicas with controlled pore size and particle size are successfully functionalzed by using octadecyltrichlorosilane(C18). Separations of PAHs molecules using functionalized mesoporous SBA-15 silica with different particle size and pore size are systematically studied for the first time. Porous stationary phase with larger pore size favors separation of larger analyte then that of smaller pore size. Effective separation of PAHs molecules can be obtained when pore size of nanoporous stationary phase must be larger 3 times than molecular size of analyte. The mesoporous SBA-15 silicas are functionalized effectively using alkylsilanes of different carbon length. Separations of PAHs using mobile phases with different polarity and flow rates are carried out on these porous materials.

並列關鍵字

mesoporous

參考文獻


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