以钛酸四异丙酯为钛源,聚氧化乙烯(PEO)为结构改良剂,采用无需模板的溶胶-凝胶技术制得了具有高比表面积、大孔-介孔双连接结构的钛胶整体柱.研究了PEO、冰乙酸、水以及凝胶化时间对钛胶整体柱形貌和比表面积的影响.采用扫描电子显微镜(SEM)和比表面分析仪对所合成的钛胶整体柱进行了表征.结果表明,经过350℃煅烧后得到钛胶整体柱:孔骨架尺寸为1μm、较窄的孔径分布(平均孔径为10.5 nm)、BET比表面积101.3m2/g、Langmuir比表面积143.3 m2/g、孔体积0.21 mL/g,并将其成功应用于HPLC对羧酸类化合物的分析.
参考文献
| [1] | Klodzinska E;Moravcova D;Jandera P;Buszewski B .Monolithic continuous beds as a new generation of stationary phase for chromatographic and electro-driven separations[J].Journal of chromatography, A: Including electrophoresis and other separation methods,2006(1):51-59. |
| [2] | Konishi, J;Fujita, K;Nakanishi, K;Hirao, K;Morisato, K;Miyazaki, S;Ohira, M .Sol-gel synthesis of macro-mesoporous titania monoliths and their applications to chromatographic separation media for organophosphate compounds[J].Journal of chromatography, A: Including electrophoresis and other separation methods,2009(44):7375-7383. |
| [3] | Nawrocki J;Dunlap C;McCormick A et al.Part Ⅰ.Chromatography using ultra-stable metal oxide-based stationary phases for HPLC[J].Journal of Chromatography A,2004,1028(01):1. |
| [4] | Berthod A .Silica:Backbone material of liquid chromatographic column packings[J].Journal of Chromatography A,1991,549:1. |
| [5] | Nawrocki J .THE SILANOL GROUP AND ITS ROLE IN LIQUID CHROMATOGRAPHY [Review][J].Journal of chromatography, A: Including electrophoresis and other separation methods,1997(1/2):29-71. |
| [6] | Kirkland J J;Glajch J L;Farlee R D .Synthesis and characterization of highly stable bonded phases for high-performance liquid chromatography column packings[J].Analytical Chemistry,1989,61(01):2. |
| [7] | Rappsilber J;Mann M;Ishihama Y .Protocol for micro-purification,enrichment,pre-fractionation and storage of peptides for proteomics using stage tips[J].Nat Protocols,2007,2(08):1896. |
| [8] | Martijn W. H. Pinkse;Pauliina M. Uitto;Martijn J. Hilhorst;Bert Ooms;Albert J. R. Heck .Selective Isolation at the Femtomole Level of Phosphopeptides from Proteolytic Digests Using 2D-NanoLC-ESI-MS/MS and Titanium Oxide Precolumns[J].Analytical chemistry,2004(14):3935-3943. |
| [9] | Backlund S;Smatt JH;Rosenholm JB;Linden M .Template-free sol-gel synthesis of hierarchically macro- and mesoporous monolithic TiO2[J].Journal of Dispersion Science and Technology,2007(1):115-119. |
| [10] | Wei, J.;Jiang, Z.-T.;Li, R.;Tan, J. .Use of the Synthesized Titania Monolith to Determine Benzoic Acid and Vanillin in Foodstuffs by HPLC[J].Analytical Letters,2012(9/12):1724-1735. |
| [11] | Wei, J.;Jiang, Z.-T.;Li, R.;Tan, J. .Preparation of titania monolith column and application in determination of benzoic acid by HILIC[J].Chromatographia,2012(11/12):563-569. |
| [12] | 黄剑峰.溶胶-凝胶原理与技术[M].北京:化学工业出版社,2005:54. |
| [13] | Konishi J;Fujita K;Nakanishi K;Hirao K .Monolithic TiO2 with controlled multiscale porosity via a template-free sol-gel process accompanied by phase separation[J].Chemistry of Materials: A Publication of the American Chemistry Society,2006(25):6069-6074. |
| [14] | Junko Konishi;Koji Fujita;Kazuki Nakanishi;Kazuyuki Hirao .Phase-Separation-Induced Titania Monoliths with Well-Defined Macropores and Mesostructured Framework from Colloid-Derived Sol-Gel Systems[J].Chemistry of Materials: A Publication of the American Chemistry Society,2006(4):864-866. |
| [15] | Brunauer S;Deming L S;Deming W E et al.On a theory of the van der Waals adsorption of gases[J].Journal of the American Chemical Society,1940,62(07):1723. |
上一张
下一张
上一张
下一张
计量
- 下载量()
- 访问量()
文章评分
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%