• Title/Summary/Keyword: Gas chromatography-electron capture detector

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The study on the analysis of α-naphthylamine in urine (요중 알파나프틸아민 분석에 관한 연구)

  • kim, Choon Sung;Roh, Jae Hoon;Bae, Mun Joo;Kim, Chi Nyon;Lim, Nam Gu;Won, Jong Uk
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.7 no.1
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    • pp.49-59
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    • 1997
  • This study was performed to analyze the purity of technical grade ${\alpha}$-naphthylamine, to establish optimal analytical condition of ${\alpha}$-naphthylamine in urine and to determine the urine sample of workers exposed to ${\alpha}$-naphthylamine. The purity of technical grade ${\alpha}$-naphthylamine were $96.5{\pm}2.38%$, $94.1{\pm}0.97%$, $97.0{\pm}0.02%$ by gas chromatography-mass selective detector. To analyze ${\alpha}$-naphthylamine in urine, high performance liquid chromatography-electrochemical detector and gas chromatography-electron capture detector operating conditions have been optimized by preliminary expriment. In high performance liquid chromatography-electrochemical detector, the mobile phase was consisted of acetonitrile(35%) and water(65%), and the flow rate was maintained at 1.0ml per minute. Optimal detective condition was 9.0V(10nA/V) of electrochemical detector. The recovery of sep-pak treatment method was highly estimated as pretreatment of ${\alpha}$-naphthylamine in urine. The free amine was isolated by gas chromatography-electron capture detector after basic hydrosis, sep-pak treatment, toluene elution and HFBA(heptafluoro-butyric anhydride) derivatization of urine. The recovery of ${\alpha}$-naphthylamine in urine was $98.73{\pm}3.29%$ by gas chromatography-electron capture detector. The sensitivity was more higher than that of high performance liquid chromatography-electrochemical detector. Urinary ${\alpha}$-naphthylamine was detected in only one worker among nine workers. The level of ${\alpha}$-naphthylamine in urine was 6.42 ng/ml.

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Determination of 3-Monochloro-1, 2-propanediol in Acid Hydrolyzed Soysauce(Ganjang) by Gas-Chromatography with Electron Capture Detector (Gas Chromatography-Electron Capture Detector를 이용한 산분해간장중의 3-Monochloro-1, 2-propanediol 분석법에 관한 연구)

  • 최종동;문귀임;오현숙;김동술
    • Journal of Food Hygiene and Safety
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    • v.16 no.1
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    • pp.61-65
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    • 2001
  • To investigate the optimum condition of 3-monochloro-1, 2-propanediol(MCPD) analysis, gas chromatography with electron capture detector was used. Determination of MCPD derivatized with phenylboric acid was more effective than that of underivatized MCPD. In derivatization of MCPD with phenyl boric acid, there were no significantly different between boiling for 2min at 9$0^{\circ}C$ and vortexing for 5min at room temperature. Extrelut column was suitable for extraction of MCPD diluted in 20% NaCl solution and recovery rates were higher than direct extraction of MCPD with ethyl acetate. But, the method of direct extraction of MCPD with ethyl acetate was useful for rapid ants qualitative analysis. The sample extracted in soysauce(ganjang) was derivatized with phenylboric acid and analyzed by gas chromatography-mass selective detector. That was confirmed as MCPD-phenylboronate.

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Multi-Pesticide Residue Method for Organopesticide Analysis (유기농약 분석을 위한 Multi-Pesticide Residue Method)

  • 김우성;이봉헌
    • Journal of Environmental Science International
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    • v.6 no.4
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    • pp.385-389
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    • 1997
  • Pesticide residues were extracted with 70% acetone and transferred to dichloromethane. Extracts were applied to open-column chromatography with florisil and alumina-N. The final extract was analyzed by gas chromatography with electron-capture detector(GC /ECD) and nitrogen-phosphorus detector(GC/NPD). Recoveries of the 17 organochlorine pegticides were ranged from 60.8 to 84.9% and those of 15 organophosphate pesticides, from 70.5% to 100.0%(except phosmet and azlnphos-methyls. The minimum detectable levels of this analytical method were low(0.021-0.058mg/kg).

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폐기물 매립지 토양에서의 PCBs 분석법

  • Lee Jeong-Hwa;Jeon Chi-Wan;Jeong Yeong-Uk
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2005.04a
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    • pp.199-201
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    • 2005
  • This paper describes a simple procedure for the quantitative analysis of 7 PCBs (polychlorinated biphenyls) in soils on the waste reclaimed land, The procedure involved sample clean up using silicagel column, acetonitrile partition and sulfuric acid procedures. The instrumental technique is applied GC/PDD(gas chromatography/pulsed discharge detector) and GC/ECD(gas chromatography/electron capture detector). Concentration of $sub-{\mu}g/g$ level was attainable with 20g soils on the waste reclaimed land.

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Determination of Airborne Formaldehyde Using the Gas Chromatograph-Pulsed Discharge Electron Capture Detector (GC-PDECD를 이용한 공기 중 포름알데하이드의 분석)

  • 김희갑;박미진;김만구
    • Environmental Analysis Health and Toxicology
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    • v.17 no.2
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    • pp.117-123
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    • 2002
  • A gas chromatographic method for the determination of airborne formaldehyde was established. In order to be highly detectable with the electron capture detector, formaldehyde was derivatized to its pentafluorobenzyl oxime form by reacting with O- (2,3,4,5,6- pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA) at pH of 4.6 and temperature of 50$^{\circ}C$ for 1 hour. Air samples were collected into a Tedlar$\^$(R)/ bag followed by transferring into water contained in two impingers in series. Collection efficiency in the front trap was higher than 90%. Measurement of selected indoor and outdoor air samples showed higher formaldehyde concentrations in indoor air environments and the importance of ventilation for reducing indoor pollution.

Multi-Pesticide Residue Method for Analysis of Organochlorine and Organophosphorus Pesticide

  • Bonghun Lee;Woo
    • Proceedings of the Korean Environmental Sciences Society Conference
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    • 1997.10a
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    • pp.37-39
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    • 1997
  • Pesticide residues were extracted with 70% acetone and transferred to dichloromethane. Extracts were applied to open-column chromatography with florisil and alumina-N, The final extract was analyzed by gas chromatography with electron-capture detector(GC/ECD) and nitrogen-phosphorus detector(GC/NPD). Recoveries of the 17 organochlorine pesticides were ranged from 60.8 to 84.9% and those of 15 organophosphorus pesticides, from 70.5 to 100.0%(except phosmet and azinphos-methyl). The minimum detectable levels of this analytical method were low (0.021-0.058 mg/kg).

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Studies on the Simultaneous Analysis of Organochlorine Pesticide Residues by Gas-Liquid Chromatography (II). Determination of Pesticides by GLC (기체-액체 크로마토그래피에 의한 잔류 유기염소제 농약들의 동시 분석에 관한 연구 (제2보). GLC에 의한 농약의 정량)

  • Taek-Jae Kim;Song-Ja Park;Young-Sang Kim
    • Journal of the Korean Chemical Society
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    • v.29 no.5
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    • pp.503-509
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    • 1985
  • Sixteen organochlorine pesticides extracted out from the crops and cleaned by solvent-solvent partitioning and Florisil column chromatography were determined by gas-liquid chromatography. The majority of the pesticides were well separated by being eluted through 5% QF-1 column and some of them through 3% OV-17 column and 2.596 DC-200/2.5% QF-1 column, and the eluted pesticides were detected by $^{63}Ni$ electron capture detector. The linear calibration curves were obtained for the most of pesticides while some curves were slightly deviated from the linearity. In the determination of 16 pesticides added to thirteen kinds of crops, the recoveries were showed over 85% for the most cases and the relative standard deviations of 5 analyses were less than 12.1%. The results were within the criteria of the AOAC method.

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Analysis of Removal Efficiency of Pesticide Residue on Dishwashing Detergent and Alcoholic Disinfectant by Gas Chromatography (가스 크로마토그래피에 의한 주방용 합성세제와 알콜소독제의 잔류농약 제거효과 분석)

  • Lee, Jae-Duk;Cho, Yun-Jin;Lee, Man-Ho;Jeung, Woo-Won
    • Applied Chemistry for Engineering
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    • v.9 no.7
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    • pp.985-989
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    • 1998
  • In this study, removal efficiencies of pesticides on apples and peppers with water, dishwashing detergent, and alcoholic disinfectant were investigated by Gas Chromatography. Different conditions of pretreatment for increase of pesticide recovery were investigated for optimum condition. In our experiment, the supelco-STB-608 column and electron capture detector(ECD) were used to analyze pesticides residue. Removal efficiency of pesticide was in the order of alcoholic disinfectant>dishwashing detergent>water.

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Study on Decomposition of Several Pesticides by Gamma-Irradiation (감마선 조사에 의한 농약 성분의 분해 연구)

  • Lee, Joo-Sang;Jung, Su-Yeon;Oh, Seung-Yeol;Jang, Beom-Su;Park, Sang Hyun
    • Journal of Radiation Industry
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    • v.6 no.3
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    • pp.205-209
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    • 2012
  • The decomposition of 50 pesticides present in an aqueous solution using ${\gamma}-irradiation$ from a $^{60}Co$ gamma-ray source was investigated using laboratory-scale experiment. The rates of decomposition were determined using a gas chromatography-electron capture detector (GC-ECD), high-performance liquid chromatography-photo diode array detector (HPLC-PDA), and HPLC-fluorescence detector (FLD). When the initial concentration of pesticides was 10 ppm, and the radiation dose was 2, 5, 10, 20, and 30 kGy, respectively, 14 pesticide samples showed high removal rates (>50%) at absorbed doses of more than 10 kGy. With the exception of procymidone, they were all completely removed at a 30 kGy irradiation dose. These results provide fundamental data on the reactivity between gamma-irradiation and pesticides in an aqueous solution. Further, an evaluation of the toxicity of radiolytic intermediate products is required.