• Title/Summary/Keyword: Capillary Gas Chromatography

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A Study on the Separation and Determination of Organochlorine Pesticides by Capillary Column Gas-liquid Chromatography (모세관 컬럼 기체크로마토그래피에 의한 유기염소제 농약의 분리 정량에 관한 연구)

  • Taek-Jae Kim;Yun-Woo Eo;Young-Sang Kim
    • Journal of the Korean Chemical Society
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    • v.31 no.5
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    • pp.425-433
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    • 1987
  • The separation of 19 organochlorine pesticides was studied by capillary column gas chromatography. The applicability of this method to the fresh rice was investigated. Comparison of the resolution of pesticides by OV-17 and SE-30 capillary columns revealed that OV-17 column (25m ${\times}$ 0.20mm, 0.27${\mu}$m thickness) showed better resolution. The relative standard deviations (RSD) for their retention times and peak areas obtained by splitless injection mode were within 0.16% and 8.2%, respectively. The recoveries of pesticides spiked in fresh rice were mostly over 85% and their RSDS did not exceed 11.4%.

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Analysis and Quantitation of Di- and Trisaccharides in Native-bee Honeys Using Capillary Gas Chromatography (Capillary GC를 이용한 토종꿀중의 Disaccharides 와 Trisaccharides의 분석)

  • Kim, Eun-Seon;Rhee, Chong-Ouk
    • Korean Journal of Food Science and Technology
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    • v.27 no.4
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    • pp.605-611
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    • 1995
  • Carbohydrase enzymes in honey catalyze transglucosylation reactions which result in the formation of structurally similar oligosaccharides. These oligosaccharides make up a small portion of the total carbohydrates in honey. These minor oligosaccharides in native-bee honeys were identified and quantitated employing trimethylsilylation by capillary Gas Chromatography. The minor oligosaccharides found in honey were eight disaccharides and five trisaccharides. The main oligosaccharide components of honey were erlose, maltose, turanose and sucrose.

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Chiral Separation of $\beta$-Blockers after Derivatization with (-)-$\alpa$- Methoxy-$\alpa$-(trifuoromethyl)phenylacetyl Chloride by Gas Chromatography

  • Kim, Kyeong-Ho;Lee, Joo-Hyun;Ko, Mi-Young;Hong, Seon-Pyo;Youm, Jeong-Rok
    • Archives of Pharmacal Research
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    • v.24 no.5
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    • pp.402-406
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    • 2001
  • Gas chromatographic method was investigated for the chiral separation of several $\beta$-blockeros(atenolol, betaxolol, bisoprolol, metoprolol and pindolol) using (-)-$\alpa$-methoxy-$\alpa$-(trifluoromethyl)phenylacetyl chloride as a chiral derivatizing agent for amino group. Prior to N-acylation, hydroxyl group was converted into O-silyl ethers by react with N-methyl-H-(taimethylsilyl)trifluoroacetamide. The reaction was selective and rapid and the diasteromeric derivatives were well separated by capillary gas chromatography. (R)-isomers were eluted faster than (S)-isomers when (-)-$\alpa$-methoxy-$\alpa$-(trifluoromethyl)phenylacetyl chloride was used as the chiral derivatizing agent. But in the opposite sequence when (+)-$\alpa$-methoxy-$\alpa$-(trifluoromethyl)phenylacetyl chloride was used. No racemization was found during the reaction.

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Dual Capillary Column System for the Qualitative Gas Chromatography: 2. Comparison between Splitless and On-Column Injection Modes

  • Kim, Kyoung-Rae;Kim, Jung-Han;Park, Hyoung-Kook;Oh, Chang-Hwan
    • Bulletin of the Korean Chemical Society
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    • v.14 no.2
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    • pp.250-255
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    • 1993
  • A dual capillary column system is described for the simultaneous analysis of a given sample and measurement of retention index (RI) and area ratio (AR) values of each peak on two capillary columns of different polarity, DB-5 & DB-1701 from a single injection. Both capillary columns were connected to either a splitless injector or an on-column injector via a deactivated fused-silica capillary tubing of 1 m length and a 'Y' splitter. Both injection modes allowed to measure RI and AR values with high reproducibility (<0.01% RSD) and high accuracy (<10% RE), respectively with the exception that the trace and high boiling solutes required the on-column mode for the accurate quantification and AR comparison. When the dual capillary column system in on-column injection mode was applied to the blind samples containing organic acids, each acid was positively indentified by the combined computer RI library search-AR comparison.

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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Simultaneous Analysis of Stimulants and Narcotic Analgesics by Capillary Column Gas Chromatography with Nitrogen Phosphorus Detector (Capillary Column Gas Chromatography/Nitrogen Phosphorus Detector를 이용한 흥분제 및 마약성 진통제의 동시분석에 관한 연구)

  • Lho, Dong-Seok;Shin, Ho-Sang;Kang, Bo-Kyung;Paek, Heang-Kee;Kim, Seung-Ki;Lee, Jeong-Ae;Kim, Young-Lim;Park, Jong-Sei
    • Journal of the Korean Chemical Society
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    • v.35 no.6
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    • pp.659-666
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    • 1991
  • A systematic analysis of 18 stimulants and narcotic analgesics containing nitrogen atom (s) in human urine by gas chromatography with nitrogen phosphorus detector (GC-NPD), is described. The urinary extract with diethyl ether at pH 8.5 showed good recoveries of the drugs and less interference peaks on GC chromatogram. Retention data were standardized by the calculation of relative retention times using diphenylamine as the internal standard. The relative standard deviations of retention times were less than 0.1% for the within-run analyses. The response factor (RRF) of a drug relative to the internal standard was calculated. RRF decreased with increasing number of nitrogen atoms. This technique can be adapted to various analytical toxicology problems.

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Dual Capillary Column System for the Qualitative Gas Chromatography: 1. Comparison Between Split and Splitless Injection Modes

  • Kim, Kyoung-Rae;Kim, Jung-Han;Park, Hyoung-Kook;Oh, Chang-Hwan
    • Bulletin of the Korean Chemical Society
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    • v.12 no.1
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    • pp.87-92
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    • 1991
  • A dual capillary column system is described for the simultaneous measurement of retention index (RI) and area ratio (AR) values of each peak on two capillary columns of different polarity, DB-5 & DB-1701. Both capillary columns were connected to a common splitless injector via a deactivated fused-silica capillary tubing of 1 m length and a 'Y' splitter, the dead volume effect of which was found to be negligible. RI and AR were measured with high reproducibility(${\leq}$0.05% RSD) and with high accuracy (<10% RE), respectively. When applied to the test samples of the organic acid mixture, each acid was positively identified by the combined computer RI library search-AR comparison.

Simultaneous Determination of (-)-Menthone and (-)-Menthol in Menthae Herba by Gas Chromatography and Principal Component Analysis

  • Kim, Jung-Hoon;Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Natural Product Sciences
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    • v.16 no.3
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    • pp.180-184
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    • 2010
  • The simple and accurate method was established for the simultaneous determination of (-)-menthone and (-)-menthol in Menthae herba obtained from Korea and China. A quantitative analysis was performed with a gas chromatography-flame ionization detector and reference compounds were separated on a capillary HP-Innowax column (30 m $\times$ 0.23 mm, 0.50 ${\mu}m$, Agilent, MA, USA). The correlation coefficients of the compounds showed good linearity ($r^2$ > 0.9997) over the linear range. The precision, repeatability and stability showed less than 1.7% of relative standard deviation (RSD) values for two compounds. Recovery rates were within the range of 95.72 - 103.76%. The method was applied successfully to analyze 15 samples of Menthae herba and achieved sufficient and specific separation of reference compounds. The principal component analysis (PCA) exhibited the classification of 15 samples according to their locations of origin.

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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