• 제목/요약/키워드: Gas chromatography-electron capture detector

검색결과 65건 처리시간 0.039초

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

  • 김춘성;노재훈;배문주;김치년;임남구;원종욱
    • 한국산업보건학회지
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    • 제7권1호
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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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Gas Chromatography-Electron Capture Detector를 이용한 산분해간장중의 3-Monochloro-1, 2-propanediol 분석법에 관한 연구 (Determination of 3-Monochloro-1, 2-propanediol in Acid Hydrolyzed Soysauce(Ganjang) by Gas-Chromatography with Electron Capture Detector)

  • 최종동;문귀임;오현숙;김동술
    • 한국식품위생안전성학회지
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    • 제16권1호
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    • pp.61-65
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    • 2001
  • Electron capture deteotor가 장착된 gas chromatography를 이용하여 간장에서 3-monochloro-1, 2-propanediol(MCPD)의 효율적인 분석조건을 조사하였다. MCPD를 직접 분석하는 것 보다 MCPD를 phenylboric acid로 유도체화하여 분석하는 경우가 sharp한 peak를 얻을 수 있었으며, 감도도 우수하였다. 유도체화 방법을 실온에서 5분간 vortex혹은 9$0^{\circ}C$에서 20분 반응시켜 분석한 결과, R값이 각각 0.9997과 0.9977로 큰 차이를 보이지는 않았다. MCPD의 추출방법은 Extrelut 3 column을 사용하는 것이 ethyl acetate로 직접 추출하는 것보다 회수율이 월등히 높았으며, MCPD의 농노가 높을수록 회수율이 낮게 나타났다. 하지만 MCPD를 정성적으로 분석하고자 할 경우 ethyl acetate로 직접 추출하는 방법도 유효한 것으로 나타났다. 간장에 MCPD를 spiking 하고 gas chromatography-electron capture detector 및 gas chromatography-mass selective detector로 분석한 결과 sharp한 모양의 peak를 얻을 수 있었으며, mass spectrum으로 MCPD를 확인할 수 있었다.

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

  • 김우성;이봉헌
    • 한국환경과학회지
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    • 제6권4호
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    • pp.385-389
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    • 1997
  • 농약 잔류물을 70% acetone으로 추출한 다음 dichloromethane 층으로 옮겨 추출물을 florisil과 alumina-N으로 충진시켜 column chromatography를 행하였다. 마지막 추출물을 electron-capture detector(GC/ECD)와 nitrogen-phosphorus detector(GC/NPD)를 가진 GC로 분석하였다. 분석 결과 17 가지의 유기염소계 농약과 15 가지의 유기인계 농약의 회수율이 각각 60.8 에서 84.9%와 70.5에서 100.0%의 범위이었으며(phosmet와 azlnphos-methyl은 제외) 본 분석 방법의 최소 검출 준위도 낮았다(0.021-0.058mg/kg).

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폐기물 매립지 토양에서의 PCBs 분석법

  • 이정화;전치완;정영욱
    • 한국지하수토양환경학회:학술대회논문집
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    • 한국지하수토양환경학회 2005년도 총회 및 춘계학술발표회
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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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GC-PDECD를 이용한 공기 중 포름알데하이드의 분석 (Determination of Airborne Formaldehyde Using the Gas Chromatograph-Pulsed Discharge Electron Capture Detector)

  • 김희갑;박미진;김만구
    • Environmental Analysis Health and Toxicology
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    • 제17권2호
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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
    • 한국환경과학회:학술대회논문집
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    • 한국환경과학회 1997년도 가을 학술발표회 프로그램
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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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기체-액체 크로마토그래피에 의한 잔류 유기염소제 농약들의 동시 분석에 관한 연구 (제2보). GLC에 의한 농약의 정량 (Studies on the Simultaneous Analysis of Organochlorine Pesticide Residues by Gas-Liquid Chromatography (II). Determination of Pesticides by GLC)

  • 김택제;박송자;김영상
    • 대한화학회지
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    • 제29권5호
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    • pp.503-509
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    • 1985
  • 농산물에 잔류되어 있는 16종의 유기염소제 농약들을 추출하여 cleanup한 것을 기체 액체 크로마토그래피법으로 분리, 정량하였다. 5% QF-1 정지상의 분리관을 주로 사용하였으며 3% OV-17관과 DC-200/2.5% QF-1 혼합관을 보조적으로 사용하였다. $^{63}Ni$ electron capture detector를 사용하여 각 농약 성분을 검출하였다. 대부분의 농약에 대한 감응곡선은 직선성을 나타냈고 일부는 약간 휘었으나 정량에는 별 지장을 주지 않았다. 16종의 농약을 13종의 농산물에 가하여 분석한 결과 대부분은 85% 이상의 평균회수율을 보였으며 각 5회 분석결과에 대한 상대평균편차는 12.1% 이하로서 AOAC에서 정한 기준을 만족하였다.

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

  • 이재덕;조윤진;이만호;정우원
    • 공업화학
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    • 제9권7호
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    • pp.985-989
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    • 1998
  • 본 연구는 가스크로마토그래피를 이용하여 사과와 고추에 대해 물, 주방용합성세제, 살균소독제 등의 다양한 세척제에 의한 농약의 세척 제거효율을 조사하였다. 농약의 회수율을 높이기 위해 대상 농약별로 상이한 전처리 조건으로 실험하였고 최적의 전처리 조건을 조사하였다. 분리관은 supelco STB-608을 사용했고 검출기로 전자포획검출기(ECD)를 사용했다. 농약제거효율은 알콜소독제>주방용합성세제>물 순서로 높았다.

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

  • 이주상;정수연;오승열;장범수;박상현
    • 방사선산업학회지
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    • 제6권3호
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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.