• Title/Summary/Keyword: GC-determination

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Determination of Arylmethyl Halides by Gas Chromatograph (Gas Chromatograph에 의한 Arylmethy Halides의 정량)

  • Oh, Dos Suk;Choi, Ho Chun
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.4 no.1
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    • pp.25-32
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    • 1994
  • Arylmethyl halides(benzyl chloride, BZYC; benzal chloride, BZYA; benzotrichloride, BZTC) and related compounds(benzyl alcohol, BZYA; benzoyl chloride, BZOC) were determined by GC using capillary column. Detailed results are as follows. 1. Stability In methanol benzotrichloride slowly transferred to benzoyl chloride by hydrolysis(ca. 7.5% for 5 days), but the others were stable. Therefore, benzotrichloride solution should be prepared just before analysis. 2. GC analysis Tenax-GC was used to absorbent and desorption solvents were $CCl_4$ and MeOH. Arylmethyl halides were analyzed within 7.5min without interference with related compounds. The calibration curve(ca. 15-80 ppm in soln), repeatability(n=10) and the desorption efficiency were good. Limit of detection by NIOSH method was about 0.003 ppm for arylmethyl halide, respectively. To analyze arylmethyl halides and related compounds in working places GC using capillary column is anticipated to be used effectively.

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Analysis of Agrochemical Residues in Tobacco Using QuEChERS Method by GC-MS/MS

  • Lee, Jeong-Min;Jang, Gi-Chul;Hwang, Keon-Joong
    • Journal of the Korean Society of Tobacco Science
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    • v.29 no.2
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    • pp.132-139
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    • 2007
  • This study was performed to apply the more rapid and accurate sample preparation, and the high selectivity and sensitivity of the analyte detection by gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). QuEChERS (quick, easy, cheap, effective, rugged and safe) method was validated for 49 agrochemicals in the CORESTA Agrochemical Advisory Committee guide and amenable to GC-MS/MS determination. In QuEChERS method, the effects of sorbents (PSA, $C_{18}$ and GCB) and matrix of the analytes in tobacco types (flue-cured, burley and oriental) were investigated. MS/MS acquisition provided high specificity and selectivity for agrochemicals and low limit of quantification. QuEChERS by using PSA alone and the matrix-matched standards gave good recoveries and RSD values in three types of tobaccos. QuEChERS method was no needed to be complex clean-up procedure and would be used as the fast and easy method for agrochemical residue analysis in tobacco.

Determination of fungicides in wines by solid-phase extraction and gas chromatography with mass selective detection (고체상 추출법과 GC/MS를 이용한 포도주 중의 fungicides 정량)

  • Park, Gyo-Beom;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.16 no.6
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    • pp.438-442
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    • 2003
  • The fungicides, used for grape growth and remained in the wine products from domestic and foreign countries such as vinclozolin, dichlofluanid, penconazole, procymidone were quantitatively analyzed after solid-phase extraction using a GC/MS-SIM method. The results obtained were as follows: for all the samples, the content of procymidone was in the range from 2.2 to $76.1{\mu}g/L$, recoveries 81.3-93.1 %, and standard deviation 1.4-3.4 %.

Building Calibration Curve for Py-GC/MS Analysis of SBR/BR Blend Rubber Compounds

  • Chae, Eunji;Choi, Sung-Seen
    • Elastomers and Composites
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    • v.55 no.4
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    • pp.281-288
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    • 2020
  • A calibration curve is needed to determine the SBR and BR blend ratio of SBR/BR blend rubber compounds using pyrolysis-gas chromatography/mass chromatography (Py-GC/MS) or Py-GC. In general, a calibration curve is obtained using reference SBR/BR vulcanizates with various blend ratios. In this study, the calibration curves were obtained using reference samples made of rubber solutions and were compared to those plotted using the reference SBR/BR vulcanizates. Calibration curves using variations of 1,3-butadiene/styrene, 4-vinylcyclohexene (VCH)/styrene, 2-phenylpropene (PhP)/butadiene, PhP/VCH, 4-phenylcyclohexene (PhCH)/butadiene, and PhCH/VCH ratios with the BR content were examined for the suitability. We found that the calibration curves obtained using the mixed rubber solution references (1,3-butadiene/styrene and PhP/butadiene) could replace those constructed using the reference SBR/BR vulcanizates. The calibration curves of 1,3-butadiene/styrene and PhP/butadiene obtained using the raw references can be used for the determination of the SBR/BR blend ratios by applying some correction factors.

Determination of MTBE, TBA and BTEX in Soil by Headspace Gas Chromatography-Mass Spectrometry

  • Shin, Ho-Sang
    • Bulletin of the Korean Chemical Society
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    • v.33 no.5
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    • pp.1693-1698
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    • 2012
  • A headspace gas chromatographic mass spectrometric (GC-MS) assay method was developed for the simultaneous determination of methyl tertiary butyl ether (MTBE), $tert$-butyl alcohol (TBA) and benzene, toluene, ethyl benzene and xylene (BTEX) in soil contaminated with gasoline. 2 g of soil sample were placed in a 10 mL headspace vial filled with 5 mL of phosphoric acid solution (pH 3) saturated with NaCl, and the solution was spiked with fluorobenzene as an internal standard and sealed with a cap. The vial was heated in a heating block for 40 min at $80^{\circ}C$. The detection limits of the assay were 0.08-0.12 ${\mu}g$/kg for the analytes. For five independent determinations at 10 and 50 ${\mu}g$/kg, the relative standard deviations were less than 10%. The method was used to analyze fifty six soil samples collected from various regions contaminated with gasoline in Korea. The developed method may be valuable for the monitoring of the analytes in soil.

GC/MS-SIM for the Determination of Alkylphenols, Chlorophenols and Bisphenol A in Paper Materials

  • Kim, Hyub
    • Proceedings of the Korea Society of Environmental Toocicology Conference
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    • 2003.05a
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    • pp.145-145
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    • 2003
  • A method for the determination of alkylphenols, chlorophenols and bisphenol A in paper materials using GC/MS-SIM has been developed. Eleven endocrine disrupting chemicals (EDCs) of phenols in paper samples were extracted with acetonitrile. Also, solid-phase extraction (SPE) with XAD-4 and subsequent conversion to isobutoxycarbonyl derivatives or tert.-butyldimethylsilyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The recoveries were 82.4∼108.8 % by area ratio of pheranthrene-d$\sub$10/ vs bisphenol A d$\sub$l6/. (isoBOC derivatization and TBDMS derivatization) The SIM responses were linear with the correlation coefficient varying 0.9717∼0.9995 (isoBOC derivatization), and 0.9842∼0.9980 (TBDMS derivatization). The range of concentrations was respectively, 0.95∼l.44 ng/g in 2,4-dichlorophenol, 1.01∼1.17 ng/g in t-butylphenol, 2.17∼5.84 ng/g in pentachlorophenol, 12.68∼14.88 ng/g in nonylphenol and 30.84∼153.72 ng/g in bisphenol A.

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Part-Per-Trillion level determination of Alkylphenols, Chlorophenols and Bisphenol A using GC/MS-SIM in Tap Water

  • Kim, Hyub
    • Proceedings of the Korea Society of Environmental Toocicology Conference
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    • 2003.10a
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    • pp.149-149
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    • 2003
  • A new technique is proposed for the determination of alkylphenols, chlorophenols and bisphenol A in tap water. The sample preparation consists of a solid phase extraction (SPE) of alkylphenols, chlorophenols and bisphenol A from a water sample with XAD-4 and subsequent conversion to isobutyloxycarbonyl (isoBOC) derivatives or tert.-butyldimethylsilyl (TBDMS) derivatives for sensitive analysis with the GC/MS-SIM mode. The recoveries were 86.6∼105.2 % (isoBOC derivatization) and 97.6∼484.5 % (TBDMS derivatization), respectively. The limit of quantitation of alkylphenols, chlorophenols and bisphenol A for SIM were 0.001∼0.050 $\mu\textrm{g}$/l (isoBOC derivatization) and 0.003∼0.050 $\mu\textrm{g}$/l (TBDMS derivatization). The SIM responses were linear with the correlation coefficient varying 0.9755∼0.9981 (isoBOC derivatization), and 0.9908∼0.9996 (TBDMS derivatization). The derivative methods and their application to tap water samples will be disscussed.

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Simultaneous Determination of 285 Chemicals in Water at ppt Levels by GC-Ion Trap Mass Spectrometry

  • Kadokami, Kiwao;Sato, Kenji;Koga, Minoru;Shinohara, Ryota
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.771-778
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    • 1995
  • The authors have developed an analytical method for determining trace amounts of 285 kinds of chemicals in natural waters by GC-ion trap MS. The results of overall recovery tests at $0.1{\mu}g/l$ showed that the mean recovery was 92.1% and the mean relative standard deviation was 10.8%. The mean of the method detection limits was $0.036{\mu}g/l$. From the results of analysis of real samples, it was confirmed that this method is useful to elucidate the concentration levels and the fate of chemicals in the aquatic environment.

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Sorbent Thermal Desorption/Gas Chromatography/Mass Selective Detection Method for Determination of Gaseous Polycyclic Aromatic Hydrocarbons in Indoor Air

  • Dai, Shugui;Zhang, Lin;Zhu, Tan
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.753-758
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    • 1995
  • Thermal desorption/gas chromatography/mass selective detection method using Tenax cartridges for the determination of gaseous polycyclic aromatic hydrocarbons(PAH) is described. Glass fiber filter can collect only PAH in particulate. Gaseous PAH may penetrate the filter. Glass cartridge packed Tenax-GC was uses fur adsorption of gaseous PAH. The air of inhalation zone was collected fur 2-10 hours. Cartridges were thermally desorbed in the reverse direction to sample flow. The desorption conditions were as follows; desorption temperature; $300^{\circ}C$; desorption time; 20min; column head pressure; 30psi; inlet split vent; closed during desorption.

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Determination of Icing Inhibitors (Ethylene Glycol Monomethyl Ether and Diethylene Glycol Monomethyl Ether) in Ground Water by Gas Chromatography-Mass Spectrometry

  • Shin, Ho-Sang;Jung, Dong-Gyun
    • Bulletin of the Korean Chemical Society
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    • v.25 no.6
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    • pp.806-808
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    • 2004
  • A gas chromatography/mass spectrometric assay method has been developed for the simultaneous determination of icing inhibitors, ethylene glycol monomethyl ether and diethylene glycol monomethyl ether in ground water contaminated with JP-8. Ethylene glycol monobutyl ether and ethylene glycol monoethyl ether were used as the internal standard and surrogate, respectively. 100 mL of ground water was extracted twice with 20 mL of methylene chloride. The extract was concentrated to dryness, dissolved with 100 ${\mu}$L of methanol and analyzed by GC-MS (SIM). The use of an Innowax column gave the peaks good chromatographic properties, and the extraction of these compounds from samples gave recoveries of about 50% with small variations. The method detection limits of the target compounds were in a range of 0.5-0.8 ng/mL in ground water.