Development of Novel Inorganic Material for Chromatographic Column Without Particle Packing
无颗粒填料色谱柱新型无机材料的研制
基本信息
- 批准号:07555480
- 负责人:
- 金额:$ 2.88万
- 依托单位:
- 依托单位国家:日本
- 项目类别:Grant-in-Aid for Scientific Research (A)
- 财政年份:1995
- 资助国家:日本
- 起止时间:1995 至 1996
- 项目状态:已结题
- 来源:
- 关键词:
项目摘要
Tetramethoxysilane was hydrolyzed in thepresence of polyethylene oxide having an average molecular weight of 10000 using acetic acid as a catalyst, which gave a wet silica gel with inetrconnected macropores about 2mum wide. The gel was subsequently immersed in aqueous solutions of ammonia with varied concentration for varied periods, then dried by evaporating the solvent, and finally heat-treated at 600゚C for 2 hours. The resultant gel retained narrowly distributed mesopores with their median size distributing from 5 to 20nm. The rod-shaped gel thus obtained was clad with a thermoshrinking resin on its side wall, suface-modified by a flow reaction with silane coupling agents, equipped with connecting devices for an ordinary HPLC apparatus, then the separation performance was investigated.A mixture of alkylbenzenes was analyzed using the rod-shaped column with the average macropore diameter of 1.6mum and mesopore diameter of 11nm. The pressure drop for the rod-shaped colummn at the same sample flow rate was less than half that of conventional particle-packed columns. Furthermore, the height equivalent to theoretical plate (HETP) remained almost unchanged for the rod-shaped column between 1mm/s and 5mm/s of linear flow rate, whereas that of conventional particle packed columns increased almost linearly with the flow rate. As a result, the HETP of the rod-shaped column became five times smaller than that of conventional ones. Simmilar difference in the pressure drop and the flowrate dependence of HETP was obsereved also in the case of separation of insulin. These results indicate that the rod-shaped column gives almost an order better separation performance than conventional ones. The superiority of the rod column in the high speed separation was experimentally confirmed to be due to the existence of thin silica skeleton associated with high fraction of macropores.
在平均分子量为10000的聚氧乙烯存在下,以乙酸为催化剂水解四甲基氧基硅烷,得到宽约2mum的大孔互联的湿硅胶。凝胶在不同浓度的氨水溶液中浸泡不同时间,然后蒸发溶剂干燥,最后在600℃下加热2小时。所得凝胶保留狭窄分布的中孔,中位尺寸分布在5 ~ 20nm之间。制备的棒状凝胶侧壁包覆热缩树脂,用硅烷偶联剂流动反应对其进行表面改性,在普通高效液相色谱仪上安装连接装置,考察其分离性能。采用大孔平均为1.6 nm,中孔平均为11nm的棒状色谱柱对烷基苯混合物进行分析。在相同的样品流速下,杆状柱的压降小于传统颗粒填充柱的一半。在线性流速为1mm/s ~ 5mm/s范围内,杆状柱的等效理论板高度(HETP)基本保持不变,而常规颗粒填充柱的等效理论板高度几乎随流速线性增加。结果,杆状柱的HETP比传统柱的HETP小5倍。在分离胰岛素的情况下,HETP的压降和流量依赖性也有类似的差异。结果表明,杆状柱的分离性能比传统柱的分离性能好近一个数量级。实验证实了棒柱在高速分离中的优势是由于存在薄硅骨架和高比例的大孔。
项目成果
期刊论文数量(10)
专著数量(0)
科研奖励数量(0)
会议论文数量(0)
专利数量(0)
Hiroshi Minakuchi: "Octadecylsilyated Porous Silica Rods as Separation Media for Reversed-Phase Liquid Chromatography" Analytical Chemistry. 68(19). 3498-3501 (1996)
Hiroshi Minakuchi:“十八烷基硅化多孔二氧化硅棒作为反相液相色谱的分离介质”分析化学。
- DOI:
- 发表时间:
- 期刊:
- 影响因子:0
- 作者:
- 通讯作者:
K.Nakanishi et al.: "Phase separation in silica sol-gel system containing poly (ethylene oxide) II.Effects of molecular weight and temperature" Bulletin of the Chemical Society of Japan. 70(in press). (1997)
K.Nakanishi 等人:“含有聚环氧乙烷的二氧化硅溶胶-凝胶体系中的相分离 II.分子量和温度的影响”日本化学会通报。
- DOI:
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- 影响因子:0
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Nobuo Tanaka: "Polymer-supported pseudo-stationary phase for electrokinetic chromatography." Journal of Chromatography A. 716. 57-67 (1995)
Nobuo Tanaka:“用于动电色谱的聚合物支持的伪固定相。”
- DOI:
- 发表时间:
- 期刊:
- 影响因子:0
- 作者:
- 通讯作者:
Kazuki Nakanishi: "Double Pore Silica Gel Monolith Applied to Liquid Chromotography" Journal of Sol-Gel Science & Technology. (印刷中).
Kazuki Nakanishi:“双孔硅胶整体应用于液相色谱”《溶胶-凝胶科学与技术》杂志(正在出版)。
- DOI:
- 发表时间:
- 期刊:
- 影响因子:0
- 作者:
- 通讯作者:
K.Nakanishi et al.: "Double pore silica gel monolith applied to liquid chromatography" Journal of Sol-Gel Science and Technology. 8(in press). (1997)
K.Nakanishi 等人:“双孔硅胶整体应用于液相色谱”《溶胶-凝胶科学与技术杂志》。
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- 影响因子:0
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SOGA Naohiro其他文献
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{{ truncateString('SOGA Naohiro', 18)}}的其他基金
Non-Brittle Behavior of Inorganic Glasses
无机玻璃的非脆性行为
- 批准号:
09450244 - 财政年份:1997
- 资助金额:
$ 2.88万 - 项目类别:
Grant-in-Aid for Scientific Research (B)
Preparation and Characterization of Transparent Magnetic Oxide Meterials
透明磁性氧化物材料的制备及表征
- 批准号:
06453122 - 财政年份:1994
- 资助金额:
$ 2.88万 - 项目类别:
Grant-in-Aid for Scientific Research (B)
Development of bio-science materials by designing porous structure and surface property of oxide gels.
通过设计氧化物凝胶的多孔结构和表面性质来开发生物科学材料。
- 批准号:
05555170 - 财政年份:1993
- 资助金额:
$ 2.88万 - 项目类别:
Grant-in-Aid for Developmental Scientific Research (B)
Desighn and Development of Infrared-to-Visible Upconversion Rare Earth Laser
红外-可见光上转换稀土激光器的设计与研制
- 批准号:
04453069 - 财政年份:1992
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$ 2.88万 - 项目类别:
Grant-in-Aid for General Scientific Research (B)
Development of materials with ordered structure through phase separation of inorganic-organic mixed sol-gel system
通过无机-有机混合溶胶-凝胶体系的相分离开发有序结构材料
- 批准号:
02555161 - 财政年份:1990
- 资助金额:
$ 2.88万 - 项目类别:
Grant-in-Aid for Developmental Scientific Research (B)
Studies on Middle Range Structure of Amorphous Inorganic Materials and its Controlling
非晶无机材料中程结构及其控制研究
- 批准号:
63430014 - 财政年份:1988
- 资助金额:
$ 2.88万 - 项目类别:
Grant-in-Aid for General Scientific Research (A)
Study on Strength and Fatigue of Ceramic Materials
陶瓷材料强度与疲劳研究
- 批准号:
58430014 - 财政年份:1983
- 资助金额:
$ 2.88万 - 项目类别:
Grant-in-Aid for General Scientific Research (A)
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