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Development of Novel Inorganic Material for Chromatographic Column Without Particle Packing

Research Project

Project/Area Number 07555480
Research Category

Grant-in-Aid for Scientific Research (A)

Allocation TypeSingle-year Grants
Section試験
Research Field Inorganic materials/Physical properties
Research InstitutionKYOTO UNIVERSITY

Principal Investigator

SOGA Naohiro  Kyoto University, Graduate School of Engineering, Professor, 工学研究科, 教授 (80026179)

Co-Investigator(Kenkyū-buntansha) TANAKA Nobuo  Kyoto Insitute of Technology, Department of Polymer Science and Engineering Prof, 繊維学部, 教授 (60127165)
NAKANISHI Kazuki  Kyoto University, Graduate School of Engineering, Associate Professor, 工学研究科, 助教授 (00188989)
Project Period (FY) 1995 – 1996
Project Status Completed (Fiscal Year 1996)
Budget Amount *help
¥4,500,000 (Direct Cost: ¥4,500,000)
Fiscal Year 1996: ¥4,500,000 (Direct Cost: ¥4,500,000)
KeywordsSilica Gel / Sol-Gel Method / Pore Structure / Liquid Chromatography / Columns / Theoretical Plate Height
Research Abstract

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.

Report

(3 results)
  • 1996 Annual Research Report   Final Research Report Summary
  • 1995 Annual Research Report
  • Research Products

    (10 results)

All Other

All Publications (10 results)

  • [Publications] Nobuo Tanaka: "Polymer-supported pseudo-stationary phase for electrokinetic chromatography." Journal of Chromatography A. 716. 57-67 (1995)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1996 Final Research Report Summary
  • [Publications] Kazuki Nakanishi: "Phase separation in Silica Sol-Gel System Containing Poly (Ethyleneoxide) II, Effects of Molecular Weight and Temperature" Bulletin of the Chemical Society of Japan. 70(印刷中). (1997)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1996 Final Research Report Summary
  • [Publications] Kazuki Nakanishi: "Double Pore Silica Gel Monolith Applied to Liquid Chromatography" Journal of Sol-Gel Science and Technology. 8(印刷中). (1997)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1996 Final Research Report Summary
  • [Publications] N.Tanaka et al.: "Polymer-supported pseudo-stationary phase for electrokinetic chromatography" Journal of Chromatography A. 716. 57-67 (1995)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1996 Final Research Report Summary
  • [Publications] 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)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1996 Final Research Report Summary
  • [Publications] K.Nakanishi et al.: "Double pore silica gel monolith applied to liquid chromatography" Journal of Sol-Gel Science and Technology. 8(in press). (1997)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1996 Final Research Report Summary
  • [Publications] Hiroshi Minakuchi: "Octadecylsilyated Porous Silica Rods as Separation Media for Reversed-Phase Liquid Chromatography" Analytical Chemistry. 68(19). 3498-3501 (1996)

    • Related Report
      1996 Annual Research Report
  • [Publications] Hiroshi Minakuchi: "Effect of skeleton size on the performance of octadecylsilylated continuous porous silica columns in reversedphase liquid chromatogrophy" Jouinal of Chromatography A. (印刷中). (1997)

    • Related Report
      1996 Annual Research Report
  • [Publications] Kazuki Nakanishi: "Double Pore Silica Gel Morilith Applied to Liquid Chromatogeaphy" Jounal of Sol-Gel Science and Technology. 8(印刷中). (1997)

    • Related Report
      1996 Annual Research Report
  • [Publications] Kazuki Nakanishi: "Double Pore Silica Gel Monolith Applied to Liquid Chromotography" Journal of Sol-Gel Science & Technology. (印刷中).

    • Related Report
      1995 Annual Research Report

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Published: 1996-04-01   Modified: 2016-04-21  

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