• Title/Summary/Keyword: supercritical fluid chromatography

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Development of New Separation Technique, Modifier Composition Programming in Supercritical Fluid Chromatography (초임계 유체 크로마토그래피에서 새로운 분리방식인 변형제 조성 프로그래밍법 개발)

  • Kim, Hohyun;Pyo, Dongjin
    • Analytical Science and Technology
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    • v.10 no.5
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    • pp.350-356
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    • 1997
  • Supercritical Fluid Chromatography(SFC) has been developed as an analytical technique for the compounds that is difficult to analyze by conventional chromatography. Since supercritical fluid $CO_2$ is difficult to elute solutes with high polarity, modified supercritical $CO_2$, was used as a mobile phase. In conventional method, silica column which is saturated with modifier was used. However, with this method, we can not control the quantity of modifier. In this paper, we developed a new method which can control quantity of modifier mixed in supercritical fluid $CO_2$. The quantity of $H_2O$ mixed was measured with amperometric microsensor which was made by perflurosulfonate ionomer(PFSI) film. we have also obtained a good supercritical fluid chromatogram of PAH mixture by use of a modifier composition programming method.

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Development of New Analytical Method of Vitamins Using Supercritical Fluid (초임계 유체를 이용한 비타민류의 새로운 분석법 개발)

  • Pyo, Dongjin;Park, Dongjin;Kim, Hohyun;Lee, Hakju;Lee, Taejoon
    • Analytical Science and Technology
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    • v.10 no.2
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    • pp.131-138
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    • 1997
  • Supercritical Fluid Chromatography(SFC) has become a technique for solving problems that are difficult to be monitored by other chromatographic methods. However, the most widely used fluid, is no more polar than hexane. Polar samples which are difficult to be analyzed with pure supercritical $CO_2$ because of their high polarity can be separated by adding polar modifiers to supercritical $CO_2$. In this paper, a new method for monitoring the mobile phase composition in modified supercritical fluid chromatography was developed. The amount of water dissolved in supercritical $CO_2$ was measured by amperometric microsensor which is made of thin film of perfluorosulfonate ionomer(PFSI). The amount of water dissolved in supercritical $CO_2$ stayed constant for a much longer time than with a saturator column. With this new mixing device, we could get good resolutions for vitamins which are difficult to separate with pure $CO_2$.

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Addition and Measurement of Modifier(Water) in Carbon Dioxide Mobile Phase for Supercritical Fluid Chromatography (초임계 유체 크로마토그래피에서 이동상에 Modifier를 첨가시키는 새로운 방법과 첨가된 Modifier(H2O) 양의 측정방법)

  • Ju Doweon;Pyo Dongjin
    • Journal of the Korean Chemical Society
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    • v.37 no.6
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    • pp.604-611
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    • 1993
  • Supercritical Fluid Chromatography(SFC) has become a technique for solving problems that are difficult by other chromatographic methods. However, the most widely used fluid, is no more polar than hexane. Polar samples which are difficult to be analyzed with pure supercritical C$O_2$ because of their high polarity can be separated by adding polar modifiers to supercritical C$O_2$. In this paper, a new method for monitering the mobile phase composition in modified supercritical fluid chromatography was developed. The amount of water dissolved in supercritical C$O_2$ was measured by amperometric microsensor which is made of thin film of perfluorosulfonate ionomer (PFSI). The amount of water dissolved in supercritical C$O_2$ stayed constant for a much longer time than with a saturator column. With this new mixing device, we could do good separations for insecticides and fungicides which are difficult to separate with pure C$O_2$.

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Supercritical Fluid Extraction of Physiologically Active materials from Agaricus blazei Fruiting Bodies (Agaricus blazei 자실체로부터 초임계 유체를 이용한 생리활성물질 추출공정)

  • 최정우
    • KSBB Journal
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    • v.15 no.4
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    • pp.408-410
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    • 2000
  • The supercritical fluid extraction(SFE) technique was applied for the isolation and purification of nonpolar physiologically acitve mateials from Agaricus blazei fruiting bodies. the qualitative analysis of extract was accomplished by gas chromatography-mass spectrometer(GC-MS) and extract was determined as linoleic acid(cis-9 cis-12-octadecadienoic acid) In order to obtain the optimum operating conditions of supercritical fluid extraction process the various temperatures and pressures were applied for process operation. From the comparison of exraction efficiencies $50^{\circ}C and 200 kg_f/cm^2$ were determined as optimum conditions.

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Temperature-controlled Restrictor for UV Detection in Capillary Supercritical Fluid Chromatography

  • Pyo, Dong-Jin
    • Bulletin of the Korean Chemical Society
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    • v.27 no.9
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    • pp.1429-1432
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    • 2006
  • Polyaromatic hydrocarbons were separated by a capillary supercritical fluid chromatographic (SFC) column and detected by a UV detector at the wavelength of 280 $\mu$m. The temperature-controlled restrictor was designed for UV detection. The temperature-controlled restrictor is a 20 cm length of deactivated fused silica of 7 mm i.d. which is held right after UV detector of the capillary SFC. The temperature of the restrictor will control the flow rate of the supercritical carbon dioxide mobile phase through the capillary column in SFC. Thus as the pressure in the column is increased from 1500 psi to 4000 psi during a pressure program, the temperature of 7 $\mu$m fused-silica tube can be varied from 100 to 350 ${^{\circ}C}$ to maintain a constant flow rate.

New Device for Addition of Modifier to Supercritical Fluid Carbon Dioxide Mobile Phase

  • 표동진;김호현
    • Bulletin of the Korean Chemical Society
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    • v.18 no.6
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    • pp.584-588
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    • 1997
  • A new device to accurately deliver small amount of modifier into supercritical carbon dioxide fluid is described. Carbon dioxide, the most widely used mobile phase in supercritical fluid chromatography, is a relatively non-polar fluid, and hence the addition of small amount of polar modifiers could be necessary to migrate polar solutes. In this work, supercritical CO₂and modifier are delivered from the pump to a 100 μL mixing chamber in which a small magnetic bar is rotating. After passing through the mixing chamber, supercritical CO₂is changed to a new mobile phase with different polarity. The amount of modifier added into supercritical CO₂is measured by an amperometric microsensor, which is prepared from a thin film of perfluorosulfonate ionomer.

New Analytical Method Using Polar Modifiers in Supercritical Fluid Chromatography and Its Application to the Separation of Fatty Alcohol Ethers

  • 표동진;이규선;이학주;김호현;Milton L. Lee
    • Bulletin of the Korean Chemical Society
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    • v.17 no.6
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    • pp.496-498
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    • 1996
  • Fatty alcohol ethers, nonionic surfactants which are used as general purpose emulsifiers were separated by use of water-modified carbon dioxide mobile phase in capillary supercritical fluid chromatography. Much greater peak intensities and improved separation were observed in the chromatogram with on-line modified mobile phase than with pure CO2. A simple method for the preparation of on-line modified mobile phase is also introduced.

Chiral Separation of Ibuprofen by Supercritical Fluid Chromatography (초임계유체 크로마토그래피를 이용한 Ibuprofen의 키랄분리)

  • 한순구;노경호
    • KSBB Journal
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    • v.19 no.4
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    • pp.263-268
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    • 2004
  • The separation method using chiral stationary phase in preparation of chiral compound was wildly used, but in this work, supercritical fluid chromatography was suggested in the stability to resolve the chiral mixtures. To determine the optimum operating condition of the racemic ibuprofen, the retention factor and resolution with change in pressures, temperatures and the contents of IPA % (vol.) in CO$_2$ were investigated. The retention factor was decreased with increase in pressure and decrease in temperature. The factor was also influenced by the content of IPA in mobile phase, while the resolution was worse with a increase in IPA %. From the experimental results, the desirable separation condition was 130 bar, 311.15 K and 4% IPA in CO$_2$. Compared to the asymmetric peak shape by liquid chromatography, that of supercritical fluid chromatography was symmetric which was a favorable condition for preparative separation.