| Co-Investigator(Kenkyū-buntansha) |
MINAKUCHI Hiroyoshi MRC Corporation, Research Division, Research Leader, 研究部, リーダー(研究職)
NAKANISHI Kazuki Kyoto Univ., Graduate School of Eng., Assoc. Prof., 大学院・工学研究科, 助教授 (00188989)
HOSOYA Ken Kyoto Inst. Tech., Faculty of Textile Sci., Assoc. Prof., 繊維学部, 助教授 (00209248)
IKEGAMI Tohru Kyoto Inst. Tech., Faculty of Textile Sci., Instructor, 繊維学部, 助手 (20301252)
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| Research Abstract |
The development of porous monolithic silica columns in capillary for micro-HPLC was studied to achieve higher performance than columns packed with particles. Following experiments were carried out.
(1) Preparation of a monolithic silica column in a capillary from alkoxysilanes.
(2) Preparation of monolithic silica columns in capillaries of various sizes, 25-250 μm.
(3) Study on the effect of domain size (through-pore size + silica skeleton size) and the ratio between through-pore size and skeleton size on the performance.
(4) Preparation of ultrahigh efficiency monolithic silica columns.
(5) Preparation of monolithic silica columns showing high efficiency in a short time.
(6) Study on the factors determining band-broadening in a monolithic silica column.
(7) Evaluation of monolithic silica columns in micro-HPLC and CEC.
(8) Application of monolithic silica columns for the separation of various types of compounds including bases, dissociable compounds, and hydrocarbons.
Following results were ob
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tained.
(1) It is possible to prepare network-type monolithic silica attached to the tube wall of fused silica capillary having 50-250 μm diameter.
(2) Decrease in domain size showed similar effects as the decrease in particle size in a particle-packed column, causeing higher column pressure drop and higher column efficiency.
(3) A monolithic silica capillary column of 100 μm, 250 cm gave 200, 000 - 300, 000 theoretical plates with to = 1000 s.
(4) A monolithic silica capillary column with through-pores = 1.5 μm and skeleton size 0.8 μm gave 10.000 theoretical plates with to = 15 S.
(5) The band-broadening in a monolithic silica column is dominated by A-term, or the contrubution of slow mass transfer in mobile phase, especially when the monolith possesses large through-pore size. Monoliths having small domain size showed the major contibution of stationary phase mass transfer.
(6) Hybrid-type monolithic silica columns showed high performance for the separation of various types of compounds including bases, b-blockers, steroids, ketones, phthalates, aicohols, and hydrocarbon of various structures.
Monolithic silica columns in 200 μm capillary can show performance 2 - 3 times higher than particle-packed columns under common conditions and are relatively easy to use. They can be applied for the separatin of a wide range of compounds. Thus they are close to practical use. (1) Preparation of larger-sized capillary, (2) various surface monofication by on-column reactions(3) optimization of domain structures, and (4) theoretical and experimental study on band-broadening in monolithic silica columns will be practical and basic subjects to study in this area. Other study will include the preparation of monolithic silica in a chip channels and multidimensional chromatography in a microscale HPLC. Less
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