• 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.

• 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.

• 한국정밀공학회지
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• 제25권4호
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• pp.53-60
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• 2008

Electron detectors used in scanning electron microscope accept electrons emitted from the specimen and convert them to an electrical signal that, after amplification, is used to modulate the gray-level intensities on a cathode ray tube, producing an image of the specimen. Electron detector is one of the key components dominating the performance of scanning electron microscope so that the development of electron detectors having high performance is indispensable to acquire high quality images using scanning electron microscope. In this paper, we designed and manufactured an electron detector and conducted a couple of image capture experiments using it. In particular, scintillator which generates light photons when it is struck by high-energy electrons was manufactured and experimental studies on the optimization of manufacturing condition was carried out. From experiments to evaluate the performance of our detector, it was verified that the performance of our detector is equivalent to or better than that of the conventional one.

• Food Science and Biotechnology
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• 제15권6호
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• pp.959-966
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• 2006

The electron-capture detector (ECD) of gas chromatographs (GC) has been used widely in pesticide analysis. However, as ECD relies on radioactive material, it is troublesome to purchase and maintain. Therefore, potent replacements for ECD were investigated. A Pulsed-discharge detector (PDD) for ECD was tested and the analytical results of PDD (ECD mode), ${\mu}ECD$, and nitrogen-phosphorus detector (NPD) were compared for 107 pesticides including organochroline, organophosphorus, pyrethroids etc. The number of pesticides identified at the lowest limit of detection (LOD) was 36, 29, and 2 for PDD, ${\mu}ECD$, and NPD, respectively. The remaining pesticides showed same response to PDD and ${\mu}ECD$. The GC-PDD analysis of pesticides spiked into representative agricultural products (brown rice, spinach, and mandarin oranges) also showed good and/or equivalent recoveries using $GC-{\mu}ECD$.

• 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).

• 한국생물공학회:학술대회논문집
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• 한국생물공학회 2003년도 생물공학의 동향(XII)
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• pp.729-729
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• 2003

• 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.

• 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).

• 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.

• 분석과학
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• 제12권5호
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• pp.408-414
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• 1999

기체 크로마토그래피-전자포획검출기 (gas chromatograph-electron capture detector : GC-ECD)를 이용하여 사람의 혈액 내에 존재하는 homocysteine (Hcy), 관련 화합물인 cysteine (Cys)과 methionine (Met)에 대해 선택적이고 감도 좋은 분석방법에 대하여 연구하였다. 시료는 혈장 내에서 환원과정을 거친 후 ethyl chloroformate (ECF)와 pentafluoropropyl alcohol (PEP-OH) 유도체화 시약을 사용하여 N(O,S)-ethylearhonyl pentafluoropropyl (PEP) ester 유도체를 만들어 추출의 효율을 높이면서 동시에 GC-ECD에 대한 크로마토그래피 성질을 향상시켰다. 생성된 유도체들은 chloroform으로 추출한 후 잔류물을 완전히 건조시키고 hexane으로 추출하여 GC-ECD로 분석하였다. Hcy와 Met는 $5-50{\mu}mol/L$, Cys는 $40-400{\mu}mol/L$ 범위에서 $R^2=0.990$ 이상의 직선상의 상관관계를 나타내었다. 이 작성한 질량곡선을 통해서 5명의 자원자들의 혈액 중에 존재하는 Hcy, Cys, met의 함량을 분석하였다.