• Title/Summary/Keyword: Chromatographic factors

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A NUMERICAL STUDY ON THE FLOW CHARACTERISTICS OF GAS CHROMATOGRAPHIC COLUMN (가스 크로마토그래픽 컬럼의 유동특성에 대한 수치적 연구)

  • Kim T.-A.;Kim Youn J.
    • 한국전산유체공학회:학술대회논문집
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    • 2005.10a
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    • pp.21-26
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    • 2005
  • Gas Chromatography (GC) is a wisely technique used for the separation and analysis of liquid and gas sample. Separation of the sample vapors is achieved via their differential migration through a capillary column with an insert carrier gas. The identity and quantity of each vapor in the mixer can be determined from its retention time in the column and a particular property of the gas, such as thermal conductivity, which can be related to the concentration of sample vapor in the carrier gas. Therefore, the flow characteristics in the spiral gas chromatographic column are numerically investigated in this study. Especially, different pressure drop between the front and the rear of GC column with various flow rates is estimated the governing equations are derived from making using of three-dimensional Naver-Stokes equation with incompressible and laminar model due to the nature of low Reynolds number flow. Using a commercial code, FLUENT, the pressure and flow fields in GC column are calculated with various flow rates. The characteristics of thermal cycling which is one of the most important factors affecting the column efficiency and analysis time is also estimated. Furthermore, numerical analyses are also carried out by using commercial code, ANSYS, with various values of power, which is applied to the heating element located at lower GC column.

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Separation of Positional Isomers in a Calix[4]arene-methylsiloxane Polymer as Stationary Phase in Capillary GC

  • Seo, Jeong Gi;Kim, In Hwan;Jang, Seung Hyeon;Kim, Byeong Ok;Ryu, Jae Uk;Park, Jeong Hak
    • Bulletin of the Korean Chemical Society
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    • v.22 no.4
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    • pp.409-412
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    • 2001
  • Poly(p-tert-butyltrimethoxymonopropyloxycalix[4]arene-methylsiloxane) (TBCX-MS) has been prepared and used as a stationary phase in isothermal capillary gas chromatographic separation of some positional isomers. Retention factors (k) and separatio n factors $(\alpha)$ for the isomers were measured and compared with those on poly(p-tert-butyl-dimethoxydipropyloxycalix[4]arene-tetramethyldisiloxane) (TBCX-TMDS), poly(dimethoxydipropyloxycalix[4]arenetetramethyl-disiloxane) (CX-TMDS). Most of the isomers investigated are well resolved on TBCX-MS. Retention of all the compounds decreases on the three phases in the order, TBCX-TMDS ${\geq}$ TBCX-MS > CX-TMDS. Similar retention values on TBCX-TMDS and TBCX-MS seem to indicate that retention property of the two phases is not significantly affected by the spatial position of the calixarene moiety.

Resolution of β-Amino Acids on a Chiral Stationary Phase Based on (+)-(18-Crown-6)-2,3,11,12-tetracarboxilic Acid without Extra Free Aminopropyl Groups on Silica Surface

  • Hyun, Myung- Ho;Choi, Hee-Jung;Kang, Bu-Sung;Tan, Guang-Hui;Cho, Yoon-Jae
    • Bulletin of the Korean Chemical Society
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    • v.27 no.11
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    • pp.1775-1779
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    • 2006
  • A liquid chromatographic chiral stationary phase (CSP) based on (+)-(18-crown-6)-2,3,11,12-tetracarboxilic acid without extra free aminopropyl groups on silica surface has been demonstrated to be quite effective for the resolution of various $\beta$-amino acids. The retention factors ($k_1$) for the resolution of $\beta$-amino acids on the CSP were quite large and the large retention factors might be quite attractive along with the reasonable separation factors ($\alpha$) for preparative scale enantioselective chromatography. The large retention factors on the CSP were found to be reduced effectively by adding ammonium ion to mobile phase without sacrificing the chiral recognition efficiency of the CSP. Consequently, the CSP is also quite applicable for use in analytical enantioselective chromatography.

Comparative Enantiomer Separation on Chiral Stationary Phases Derived from Chiral Crown Ether by HPLC (고성능 액체 크로마토그래피에서 키랄 크라운 에테르로부터 유도된 키랄 고정상을 이용한 광학분리의 비교)

  • Huang, Hu;Jeon, So-Hee;Kim, Ji-Yeon;Lee, Won-Jae
    • KSBB Journal
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    • v.27 no.4
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    • pp.232-236
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    • 2012
  • Comparative liquid chromatographic enantiomer separation of ${\alpha}$-amino acids, their esters and primary amino compounds was performed using two chiral stationary phases (CSPs) prepared by covalently bonding (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid (18-C-6-TA) of the same chiral selector. In general, the separation factors and resolution factors for these analytes on CSP 1 were greater than on CSP 2, while these capacity factors on CSP 2 were quite greater than on CSP 1. Except for leucine methyl ester and phenylalanine methyl ester, the elution orders of all analytes including ${\alpha}$-amino ${\alpha}$-alkyl acids and phenylglycine alkyl esters on CSP 1 are identical to those on CSP 2. This study showed that different connecting structures for these two CSPs might influence their ability to resolve the analytes depending on their structures related to the chiral recognition mechanism.

Factors Affecting HETP in Preparative Liquid Chromatography (제조용 액체 크로마토그래피에서 HETP에 영향을 미치는 인자)

  • Choi, Du Chan;Choi, Dai-Ki;Row, Kyung Ho
    • Applied Chemistry for Engineering
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    • v.7 no.5
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    • pp.985-991
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    • 1996
  • In chromatographic separation, HETP(height equivalent to a theoretical plate) is a useful quanititive parameter and it is wildely designated as column efficiency. The effects of operating conditions (sample concentration, injection volume, flow rate and mobile phase composition) on HETP were investigated in perparative liquid chromatography (PLC). Water and organic modifier of methanol were used as mobile phase. The sample of thymidine was injected into preparative C18 columns. The system was run by a isocratic mode in 1.5~5.5ml/min. The larger amounts of sample and higher flow rates of mobile phase increased HETP, which means that column efficiencies were worse. As the weight of sample injected into a chromatographic system could be prepared with different concentrations and injection volumes, for the same amount of sample, HETP was approximately increased two times with the ten-fold injection volume. HETP was mainly affected by the resistance of stationary and mobile phase mass transfer in the intraparticle section of packings at higher velocities.

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Effect of Functional Monomer on Retention Factor of Chiral Racemate (기능성 단량체가 키랄 물질의 체류인자에 미치는 영향)

  • Jin, Yin-Zhe;Row, Kyung-Ho
    • KSBB Journal
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    • v.20 no.4
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    • pp.260-265
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    • 2005
  • In this work, molecular imprinted polymers (MIPs) using the template of the N-CBZ (carbobenzyloxy)-L-phenylalanine, MAA and 4-VPY as a monomer, EGDMA as a crosslinker and AIBN as an initiator were considered. The prepared polymer particles $(Ca.\;25-35\;{\mu}m)$ were packed into a chromatographic column $(3.9\;\times\;150\;mm)$. The chromatographic characteristics of the retention on the MIP were experimented with acetonitrile as a mobile phase at the flow rate of mobile phase, 0.5 ml/min. The retention factors and resolutions of chiral racemate of the N-CBZ-D, L-phenylalanine were measured. The results showed that the retention factor and resolution by the two co-monomer imprinting polymer were higher than the single monomer imprinting polymers, which indicated an increase in the affinity of the MIP with the sample as a result of the cooperation effect of the binding sites.

The Effect of Mobile Phase and Dissolving Solvent on the Enantiomer Separation Using a Covalently Immobilized Chiral Column Derived from Polysaccharide Derivative (다당유도체로 공유결합된 카이랄 칼럼에서 이동상과 분석물질의 용매가 거울상 이성질체의 광학분할에 미치는 영향)

  • Huang, Hu;Lee, Beom-Gyu;Baek, Chae-Sun;Lee, Won-Jae
    • Journal of the Korean Chemical Society
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    • v.53 no.2
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    • pp.137-143
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    • 2009
  • Liquid chromatographic enantiomer separation of N-tert-butoxycarbonyl (BOC) $\alpha$-amino acids and their ethyl esters was performed on covalently immobilized chiral column (Chiralpak IC) derived from polysaccharide derivative. The solvent versatility of the covalently immobilized Chiralpak IC in enantiomer separation of N-BOC $\alpha$-amino acid ethyl ester derivatives was shown and the chromatographic parameters of their enantioselectivities and resolution factors were greatly influenced by the nature of the mobile phase. Also the effect on the dissolving solvent for these analytes on the enantiomer separation using the same mobile phase and the examples of preparative enantiomer separation on analytical column were shown.

Separation of Amino Acid Enantiomers by Gas Chromatography I With Optically Active N-Benzoyl-L-Valine Derivative as Stationary Phase (가스크로마토그라피에 의한 아미노산 광학이성체의 분리 I 광학활성 N-Benzoyl-L-Valine 유도체의 고정상으로의 응용)

  • 박만기;류재하;강종성
    • YAKHAK HOEJI
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    • v.29 no.6
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    • pp.375-379
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    • 1985
  • The gas chromatographic behavior of optically active N-(N-benzoyl-L-valyl)-anilide used as stationary phase is described. N-(N-benzoyl-L-valyl)-anilide has been synthesized with good yield under mild condition via Schotten-Bauman process and coated on the Chromosorb W AW (80-100mesh) for the purpose of enantiomer separation. The behavior of this compound as optically active stationary phase for the separation of the enantiomers of N-TFA-D, L-amino acid isopropyl esters has been examined with respect to the correlation between the separation factors and column temperatures. All amino acid enantiomers examined were eluted within one hour and the elution pattern showed retention times increasing in the order of alanine, valine, leucine, threonine, proline and methionine.

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Determination of Fluorescent Whitening Agents in Paper Materials by Ion-Pair Reversed-Phase High-Performance Liquid Chromatography

  • Kim, Jeong Soo;Kim, Do Hwan;Kim, Keon
    • Bulletin of the Korean Chemical Society
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    • v.33 no.12
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    • pp.3971-3976
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    • 2012
  • A simple method was developed for the analysis of seven stilbene-type fluorescent whitening agents (FWAs) in paper materials by ion-pair reversed-phase high-performance liquid chromatography with fluorescence detection. These stilbene-type FWAs included two disulfonate, two tetrasulfonate, and three hexasulfonate compounds. After optimization of chromatographic conditions, the FWAs were satisfactorily separated using a reversed-phase column (RP-18) with the following isocratic mobile phase: methanol-water (60:40) containing 17.5 mM TBABr and 10 mM citrate buffer (pH = 7.0). The calibration plot was linear in the range from 5 to 500 ng/mL for two disulfo-FWAs and from 1 to 500 ng/mL for the other five FWAs. Precision levels of the calibration curve as indicated by RSD of response factors were 1.2 and 8.1%. Limits of quantitation (LOQ) ranged from 1.2 to 11 ng/mL.

Separation of Amino Acid Enantiomers by Gas Chromatography II (가스크로마토그라피에 의한 아미노산 광학이성체의 분리 II)

  • 박만기;강종성;유재하;박정일;전동원
    • YAKHAK HOEJI
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    • v.30 no.1
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    • pp.47-50
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    • 1986
  • The enantiomers of five amino acids (alanine, valine, threonine, leucine and phenylalanine) could be separated by gas chromatography with optically active (S)-5-isopropyll-$N^3$-phenyl-2-thiohydantoinic stationary phase, which prepared from L-valine and phenylisothiocyanate. Gas chromatographic separations on methylesterificated and N-trifluoroacetylated amino acids have been conducted in isothermal at several column temperatures (180~190, 200, $210^{\circ}C$). The separation factors were 1.29 (alanine, $190^{\circ}C$), 1.35 (valine, $190^{\circ}C$), 1.33 (threonine, $190^{\circ}C$), 1.17 (leucine, $190^{\circ}C$) and 1.05 (phenylalanine, $190^{\circ}C$) and D-isomers eluted prior to L-isomers in every instance. The result of this experiment shows that this stationary phase can be used for the separation of the other amino acids enantiomers.

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