• Title/Summary/Keyword: capillary column

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Analysis of Volatile Organic Compounds in Water by Modified Injection Mode for Purge & Trap-GC/MS Method (Purge & Trap-GC/MS 분석법의 주입방식 개선에 의한 물 중의 휘발성 유기물 분석)

  • Jeon, Chi Wan;Lee, Sang Hak;Eum, Chul Hun
    • Journal of the Korean Chemical Society
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    • v.39 no.8
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    • pp.635-642
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    • 1995
  • Improved sample introduction system has been investigated for the determination of volatile organic compounds in water using a purge & trap preconcentration apparatus and a capillary gas chromatography/mass spectrometry. The present limitations associated with the moisture control module and cryorefocusing system suggested by EPA were discussed. To solve the problems such as improper separation of peaks due to the adsorption of water and contamination of purge & trap system, a more efficient connection system between the purge & trap apparatus and the gas chromatograph was introduced and the optimum operational conditions were suggested. A carbopack B/carboxen 1000 and 1001 trap was used for the purge & trap procedure and a custom made crosslinked dimethyldiphenylpolysiloxane capillary column was used for the separation of compounds. Accuracy and precision of the method suggested in this report were examined and the method detection limit of each compound was proposed for the simultaneous determination of 54 volatile organic compounds in water.

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On-Channel Micro-Solid Phase Extraction Bed Based on 1-Dodecanethiol Self-Assembly on Gold-Deposited Colloidal Silica Packing on a Capillary Electrochromatographic Microchip

  • Park, Jongman;Kim, Shinseon
    • Bulletin of the Korean Chemical Society
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    • v.35 no.1
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    • pp.45-50
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    • 2014
  • A fully packed capillary electrochromatographic (CEC) microchip with an on-column micro-solid phase extraction (SPE) bed for the preconcentration and separation of organic analytes was prepared. A linear microchannel with monodisperse colloidal silica packing was formed on a cyclic olefinic copolymer microchip with two reservoirs on both ends. Silver-cemented silica packing frit structure was formed at the entrance of the microchannel by electroless plating treatment as a base layer. A gold coating was formed on it by reducing $Au^{3+}$ to gold with hydroxylamine. Finally micro-SPE bed was formed by self-assembly adsorption of 1-dodecanethiol on it. Micro-SPE beds were about 100-150 ${\mu}m$ long. Approximately $10^3$ fold sensitivity enhancements for Sulforhodamine B, and Fluorescein in nM concentration levels were possible with 80 s preconcentration. Basic extraction characteristics were studied.

Comparison of Enantioselective CEC Separation of OT-MIP Capillary Columns with Templates of Various Camphor Derivatives Made by the Pre-established General Preparation Protocol

  • Zaidi, Shabi Abbas;Lee, Seung-Mi;Lee, Ju-Young;Cheong, Won-Jo
    • Bulletin of the Korean Chemical Society
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    • v.31 no.10
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    • pp.2934-2938
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    • 2010
  • Some open tubular (OT) molecule imprinted polymer (MIP) silica capillary columns with templates of camphor derivatives such as 10-camphorsulfonic acid (10-CSA), 10-camphorsulfonamide (10-CS) and camphor-p-tosyl hydrazone (CTH) have been successfully prepared by the prior generalized preparation protocol. The three MIP thin layers of different templates showed quite different morphologies. The chiral selectivity of each MIP column for the template enantiomers was optimized by changing eluent composition and pH. The optimization conditions were found to be different for the three MIPs. This work suggests prospective successful extension of the generalized preparation protocol for OT-MIP silica capillary columns toward templates of a variety of chemical groups.

Analysis of Inorganic Acids by Capillary Zone Electrophoresis (Capillary Zone Electrophoresis를 이용한 음이온 동시분석에 관한 연구)

  • Park, Sung-Woo;Jin, Kwang-Ho;You, Jae-Hoon;Kim, Dong-Hwan;Seo, Baeseuk;Kim, Young-Sang
    • Analytical Science and Technology
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    • v.11 no.3
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    • pp.213-221
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    • 1998
  • The determination of inorganic anions by capillary zone electrophoresis is reported. A ten component synthetic mixture of anions of bromide, chloride, fluoride, nitrite, nitrate, sulfite, sulfate, perchlorate, chlorate and chlorite was separated by the capillary column and detected by indirect UV method. The running buffer contained 5 mM ammonium dichromate, 10 mM ammonium acetate, 20 mM diethylenetriamine, 10% methanol solution at pH 9.3. A potential of 15 kV at the cathode (reversed polarity) was utilized for the separation of inorganic anions. A complete separation of anions was achieved in less then 10 min and the applicabilities of the method for the analysis of real samples was demonstrated. We compare the concentration of anions in toluene inhaled humen's urine and in postmortem bloods obtained by capillary zone electrophoresis and ion chromatograph.

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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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Identification of Lignan Compounds in Fruits of Schisandra chinensis BAILLON by Gas Chromatography/Mass Spectrometry (GC/MS에 의한 오미자 Lignan성분의 동정)

  • Sohn, Hyun-Joo;Bock, Jin-Young
    • Applied Biological Chemistry
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    • v.32 no.4
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    • pp.344-349
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    • 1989
  • Eleven lignan compounds in fruits of Schisandra chinensis BAILLON were identified by gas chromatography/mass spectrometry(GC/MS). The GC/MS conditions were as followed: the GC column used was SPB-1 fused silica capillary $(0.25mm\;id{\times}30m,Supelco)$ and the column oven temperature was programmed from $200^{\circ}C$ to $300^{\circ}C$ at the rate of $4^{\circ}C$ per minute; the MS ionization voltage was 70eV (EI mode). The compounds identified were gomisin J $(M^+;\;388)$, deoxyschizandrin$(M^+;\;416)$, gomisin N $(M^+;\;400)$, schizandrin$(M^+;\;432)$, wuweizisu C $(M^+;\;384)$, gomisin A $(M^+;\;416)$, angeloylgomisin H $(M^+;\;500)$, tigloylgomisin H $(M^+;\;500)$, angeloylgomisin Q $(M^+;\;530)$, gomisin B $(M^+;\;514)$ and benzoylgomisin H $(M^+;\;522)$, peaks of which were separated well on the GC chromatogram.

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Gas-chromatographic determination of methylthiohydantoin amino acid as N(O)-butyldimethylsilyl derivatives in amino acid sequencing with methylisothiocyanate (Methylisothiocyanate를 이용한 아미노산 배열결정시 N(O)-butyldimethylsilyl 유도체로서의 methylthiohydantoin 아미노산의 기체 크로마토그래피에 의한 분석)

  • Woo, Kang-Lyung
    • Applied Biological Chemistry
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    • v.35 no.2
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    • pp.132-138
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    • 1992
  • For effective determination of methylthiohydantoin amino acids(MTHs) by gas liquid chromatography in the protein sequencing, derivatization with N-methyl-N-(tert.-butyl-dimethylsilyl)trifluoroacetamide(MTBSTFA), a new silylating reagents, was attempted instead of trimethylsilyl(TMSi) derivatives by N,O-bis(trimethylsilyl)trifluoroacetamide(BSTFA) used up to the present and N(O)-butyldimethylsilyl MTHs derivatized by MTBSTFA were analysed on HP-1 capillary column. Twenty one protein amino acids except cystine were indentified. Especially arginine that did not detected with TMSi derivative on packed column until now was resolved by derivatization with MTBSTFA. N(O)-butyldimethylsilyl MTHs showed multiple peaks by MTBSTFA were proline, isoleucine, glycine and tyrosine and hydroxyproline especially showed several extraneous peaks more than two. Calibration curves of N(O)-butyldimethysilyl MTHs of amino acids in the range of $2.5\;nmol{\sim}7.5\;nmole$ showed good linearity. however, those of lysine, histidine and arginine showed linearity in the range of $5.0\;nmole{\sim}15.0\;nmole$. Correlation coefficients and regression coefficients of all calibration curves were highly significant(p<0.001).

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Capillary Size-exclusion Chromatography as a Gel-free Strategy in Plasma Proteomics

  • Cho, Man-Ho;Wishnok, John S.;Tannenbaum, Steven R.
    • Molecular & Cellular Toxicology
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    • v.1 no.2
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    • pp.87-91
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    • 2005
  • Although 2D-PAGE has been widely used as the primary method for protein separation, difficulties in displaying proteins with an extreme values of isoelectric paint (pI), molecular size and hydrophobicity limit the technique. In addition, time consuming steps involving protein transfer and extraction from the gel-pieces can result in sample loss. Here, we describe a novel protein separation technique with capillary size-exclusion chromatography (CSEC) for rapid protein identification from human plasma. The method includes protein fractionation along with molecular size followed by in-solution tryptic digestion and peptide analysis through reversed phase liquid chromatography (RPLC) coupled to nanoflow electrospray-tandem mass spectrometry (ESI-MS/MS). Tryptic peptides are applied an a $100\;{\mu}m\;i.d.{\times}10mm$ length pre-column and then separated on a $75\;{\mu}m{\times}200mm$ analytical column at -100 nL/min flaw rate. Proteins were identified over the wide ranges of pI (3.7-12.3) when this technique was applied to the analysis of $1-2\;{\mu}L$ of human plasma. This gel-free system provides fast fractionation and may be considered a complementary technique to SDS-PAGE in proteomics.

Measurement and Analysis of Diffusivity for SBS/cyclic Solvent Systems Using CCIGC Technique (CCIGC 기법을 사용한 SBS/cyclic solvent 시스템에서의 확산계수 측정 및 해석)

  • Kim, Jiui;Hong, Seong Uk
    • Applied Chemistry for Engineering
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    • v.25 no.2
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    • pp.147-151
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    • 2014
  • In many polymer processing operations, the diffusion of small molecules in polymeric materials plays an important role. The fundamental physical property required to design and optimize processing operations is the mutual diffusion coefficient. To investigate the transport properties of polymer/solvent systems at infinite dilution, capillary column inverse gas chromatography (CCIGC) is often employed. In this study, diffusion and partition coefficients of cyclic solvents in styrene/butadiene/styrene (SBS) block copolymer were measured over a wide temperature range using the CCIGC technique.

The Stimultaneous Determination of Phenolic Compounds by GC and GC/MS

  • Kim, Jong-Bae;Park, Jyung-Rewng
    • Preventive Nutrition and Food Science
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    • v.3 no.2
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    • pp.111-118
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    • 1998
  • To develop a simple, rapid and simultaneous analytical method of phenolic compounds using gas chromatography (GC) and gas chromatography/mass spectrophometer (GC/Ms), this experiment was carried out to search the retention times of capillary columns and the characteristics of fragment ions in electron impact mass spectra. Most of trimethylsilyl derivatives and underivatized phenolic compounds were separated very well on three kinds of capillary columns(HP-1), Ultra-2 and HP-35). Quantitiative determination of phenolic compounds was achieved by internal standards (p-hydroxybenzoic acid iopropyl ester, p-hydroxybenzoic acid ethyl ester). Calibration plts were linear in the investigated range, and the limits of detection were about 5 ng at split mode method. When analyzed by three columns, theseparation times were fairly constant on two nonpolar columns, but a few compounds showed slightly different separation order by the itnermediate polar HP-35 column. The important characteristic patterns of TMS derivatives of phenolic compounds on the EI/MS spectrra appeared at the base peak of [M-15]+ ion and presented at high abundance in most TMS derivatives of phenoloc compounds. [M]+, [M-CH3-COO]+, [M-Si(CH3)4]+ and [M-Si(CH3)4 -CH3]+ also observed in mass spectra of these compounds . Although several compounds have the same retention times on GC column, it might be possible to identify these compounds by the different patternsof mass frgement ions. The TMS derivatives, thus , provide additional information for identification of phenolic compounds in biological systems.

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