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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：
SOGA Naohiro
金额：
$ 2.88万
依托单位：
KYOTO UNIVERSITY
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：
https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-07555480/
关键词：
Silica Gel Sol-Gel Method Pore Structure Liquid Chromatography Columns Theoretical Plate Height

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。