• 한국대기환경학회지
• /
• 제21권2호
• /
• pp.269-274
• /
• 2005

In this work, analytical bias arising from the gas chromatographic determination of sulfur compounds was evaluated by the application of direct loop injection method to the GC/PFPD detection of four sulfur compounds including H$_{2}$S, CH$_{3}$SH, DMS, and DMDS. For the proper evaluation of analytical uncertainties involved in GC calibration, we employed two comparative techniques of calibration at fxed concentration injection (CFCI) vs calibration at fixed volume injection (CFVI) method. The results of our study indicate that CFCI method exhibits very poor sensitivity due to the matrix effect with varying injection volumes. On the other hand, as CFVI method overcomes such limitation, it can be used to obtain very accurate quantification of S compounds at their high concentration levels above a few to a few tens ppb.

• 분석과학
• /
• 제7권3호
• /
• pp.349-359
• /
• 1994

천연가스 중의 부취제 농도를 분석하기 위한 기체 크로마토그래피 방법에 대하여 연구하였다. TBM(tertiarybutylmercaptan) 및 THT(tetrahydrothiophene)를 포함한 8종의 부취제를 OV-101 컬럼상에서 거의 완전히 분리하였다. 수소 유속, 공기 유속 및 검출기 온도와 같이 FPD의 응답에 영향을 미치는 몇 가지 상호 관련된 파라미터들의 최적 조건을 구하였다. TBM과 THT의 검정곡선을 투과한 장치를 이용하여 작성하였다. 이러한 분석방법을 천연가스 공급관 내의 혼합 부취제인 TBM과 THT를 정량하는 데 적용하였다. 부취수준과 부취제 농도와의 상관관계를 구하기 위한 냄새 측정기의 유용성에 대하여 알아보았다.

• 농약과학회지
• /
• 제13권3호
• /
• pp.133-147
• /
• 2009

토양 중 농약잔류량을 신속하고 저렴하게 분석할 수 있는 다성분 동시분석법을 개발하기 위하여 작물체 중 잔류농약분석법 및 개별성분 분석법을 조사하고 확인하여 기기분석 조건을 확립하였고 분배과정의 용매별 효율성을 조사한 결과는 다음과 같았다. 국내사용농약 중 GC로 분석 가능한 성분 180 성분에 대하여 검출기별 감응성 검토결과 ECD의 경우 84 성분 및 NPD의 경우 113 성분이 예상검출한계 $0.01\;mg\;kg^{-1}$ 이하이었으며 ECD와 NPD를 종합하면 148 성분이었다. 검출한계 $0.05\;mg\;kg^{-1}$ 이하인 농약성분은 ECD 137 성분 및 NPD 170 성분이었고, 두 검출기의 결과를 종합하면 179 성분이 예상 검출한계 $0.05\;mg\;kg^{-1}$ 이하이었다. 농약성분 peak의 분리도와 분석소요시간을 고려하여 선정한 기기분석 조건에서의 머무름 시간 분포를 살펴보면 대부분의 성분이 시료주입 후 10 분에서 40 분 사이에 검출되어 적절하게 분포되었으나, 20 분과 30 분사이의 머무름 시간대에는 90 여 성분이 분포하여 많은 성분이 충분히 분리가 되지 않을 것으로 판단되었다. 분배과정의 회수율은 dichlorornethane이 가장 우수하였으며, 그 다음은 ethyl acetate/hexane 혼합용매, ethyl acetate 순으로 각각 시험대상 성분의 90%, 85% 및 81%가 70-120% 범위의 회수율을 나타내었다. 따라서 dichlorornethane을 두 분배용매체계로 대체하는 것이 가능할 것으로 사료된다.

• 한국식품위생안전성학회지
• /
• 제9권1호
• /
• pp.43-48
• /
• 1994

Instrumental determination was performed for the analysis of residues of ethylene oxide(EO), ethylene chlorohydrin(ECH) and ethylene glycol(EG) in white ginseng powders which were deaerated for 30 min after EO fumigation. Gas chromatographic data showed that EO residues were 570 ppm in the immediate samples after deaeration and 170 ppm in the stored ones for 8 days at 30$\pm$1$^{\circ}C$, respectively, showing a decreasing tendency with elapsed time. On the other hand, ECH and EG residues in samples as the secondary products of EO were 17, 650 ppm and 727 ppm stored for one month, and 9, 595 ppm and 221 ppm stored for 3 months, respectively.

• 한국지하수토양환경학회:학술대회논문집
• /
• 한국지하수토양환경학회 1996년도 경북지부 결성 및 추계학술발표회 논문집
• /
• pp.50-53
• /
• 1996

This paper reports the experimental results for the determination of the overall partition coefficient of VOCs in unsaturated soil, A chromatographic method was used for the determination of gaseous partition coefficients to natural soil under various water content conditions. The equilibrium vapor pressure of water over saturated salt solution was used to fix the relative humidity of the air and control the water content of the soil systems. The transport behavior was studied for dichloromethane, trichloroethane and dichlorobenzene pollutants, with log octanol-water partition coefficients(log $K_{ow}$ ) which range from 1.25 to 3.39, or water to soil partitioning which varies by 135 times; water solubility constants which vary by 3 times; and vapor pressures which range from 1 to 362 torr. Water content of the soil had a pronounced effect on the effective partition coefficient(between gas and soil + water stationary phase) as well as on the effective dispersion coefficient.

• Applied Biological Chemistry
• /
• 제34권2호
• /
• pp.149-153
• /
• 1991

Headspace 가스크로마토그라피를 이용한 휘발성 산화생성물 분석으로 대두유의 산화진행도를 객관적으로 평가할 수 있는 방법을 연구하기 위하여, 휘발성 성분의 분리방법으로 GC 주입부에 들어가는 splitless mode liner insert에 Tenax GC를 충전하여 휘발성 산화생성물을 포집 및 용출할 수 있는 방법을 고안하였다. 이 방법을 이용하여 polyethylene 용기에 포장된 대두유를 $60^{\circ}C$에서 400 lux의 형광등을 12시간 주기로 점멸시켜 100일간 저장하고 휘발성 산화생성물의 변화를 분석한 결과와 관능검사 결과와의 상관 분석을 실시하여 headspace 가스크로마토그라피로, pentanal과 hexanal을 분석하면 대두유의 산화 진행도를 회귀식을 이용하여 평가할 수 있음을 알 수 있었다. 따라서 상기의 방법이 저장 은도를 달리한 대두유에도 적용이 가능한가를 알아보기 위하여 저장 온도를 $20^{\circ}C,\;40^{\circ}C$ 및 $60^{\circ}C$로 한 대두유의 pentanal과 hexanal을 가스크로마토그라피로 분석한 결과와 관능검사에 의한 산패취 측정결과와의 상관 분석을 실시한 결과 pentanal(PE), hexanal(HE) 및 $log(PE){\cdot}log(HE){\cdot}log(PE){\times}log(HE)$의 세 가지를 면수로 한 회구식들의 상관 계수 값이 각각 0.941, 0.953 및 0.947로 다같이 높은 값을 보여 저장 은도가 다론 대두유의 경우에는 headspace 가스크로마토그리피로 분석한 pentanal과 hexanal이 대두유의 품질 지표 성분으로 이용 가능함을 알 수 있었다. 또한 널리 쓰이고 있는 산가, 과산화물가와 관능검사에 의한 산패 취 측정 결과와의 상관 분석을 실시한 결과는 상관 계수의 값이 산가는 0.756, 과산화물가는 0.503으로 낮은 값을 보였다.

• 한국지하수토양환경학회:학술대회논문집
• /
• 한국지하수토양환경학회 2003년도 총회 및 춘계학술발표회
• /
• pp.196-200
• /
• 2003

A gas chromatography/mass spectrometric assay method was developed for the simultaneous determination of ethylene glycol monomethyl ether (EGME) and diethylene glycol monomethyl ether (DEGME) in spilled aviation fuels. Ethylene glycol monobutyl ether (EGBE) and ethylene glycol monoethyl ether (EGEE) were used as internal standard and surrogate, respectively. The sample preparation consists of back-extraction with 7 mL of methylene chloride after extraction of 50 mL of fuel with 2 mL of water. The extract was concentrated to dryness and dissolved with 100L of methanol and analyzed by CC-MS (SIM). The peaks had good chromatographic properties by using semi-polar column and the extraction of these compounds from fuel also gave high recoveries of 75 and 85 % with small variations for EGME and DEGME, respectively. Method detection limits were 1.3 ng/mL for EGME and 1.0 ng/mL for DEGME in spilled fuel. The method may be useful for fuel-type differentiation between kerosene and JP-8, which may originate from the storage tank.

• Bulletin of the Korean Chemical Society
• /
• 제22권7호
• /
• pp.685-688
• /
• 2001

A gas chromatography/mass spectrometric assay method has been developed for the simultaneous determination of benzidine (BZ), N-acetyl benzidine (ABZ) and N,N-diacetyl benzidine (DABZ) in rat urine. BZ, ABZ and DABZ were extracted from urine at pH 8 with ethyl ether. Conjugated urinary metabolites were extracted at pH 8 after hydrolysis with 1 M HCl for 30 min at 100 $^{\circ}C.$ The dried extract was dissolved in 100 ${\mu}{\ell}$ of ethylacetate and then injected in gas chromatography-mass spectrometric (GC-MS) system without further purification or modification. BZ, ABZ and DABZ have good chromatographic properties and offer very sensitive response for the EI-MS (SIM) without any derivatization. The recoveries for BZ, ABZ and DABZ were about 98.0, 81.8 and 71.4%, respectively, at pH 8.0 and the concentration of 5.0 ng/mL. The coefficients of variation of BZ and ABZ were less than 9.5% from 0.1 to 100 ng/mL and that of DABZ was less than 13% in the same concentration range. The detection limits of the assay were 0.01 ng/mL for both BZ and ABZ, and 0.05 ng/mL for DABZ in urine or plasma 1.0 mL.

• 한국환경보건학회지
• /
• 제23권1호
• /
• pp.66-73
• /
• 1997

This procedure describes the method for gas chromatographic determination of 31 organophosphorus and 28 organochlorine pesticides in 10g of spinach, tomato and onion. After the pesticides were extracted with several solvents, the amount of coextractives and recovery rates of acephate and methamidophos were calculated. Samples for organochlorine pesticides were cleaned up with florisil solid phase extraction columns. NaBH$_4$ was added to onion extracts, which contained sulfur compound. All the concentrated extracts were analyzed by gas chromatography with ECD and NPD. The smallest amount of coextractives resulted from the spinach samples extracted with 5% MeOH in ethyl acetate. 5% EOH in ethyl acetate had the highest extractability for acephate and methamidophos and gave the best overall performance as an extraction solvent. The ability of 5% EOH in ethyl acetate to extract various organophosphorus and organochlorine pesticides from spinach, tomato and onion was examined. Recovery of 59 insecticides ranged from 58.0% to 110.5%. The average recoveries of fortified spinach, tomato and onion were 90.08%, 94.54% and 84.90%, respectively.

• 약학회지
• /
• 제32권1호
• /
• pp.6-13
• /
• 1988

A gas chromatographic method is described for the determination of volatile free acids(VFAs) in body fluids. VFAs were trace enriched from body fluids by liquid-solid extraction using Chromosorb P as the solid sorbent and ether as the eluant. The enriched VFAs were injected in splitless injection mode onto a HP-20M fused silica capillary column. The flame ionization detector was used as the detector. The present method was applied to the profiling of VFAs in body fluids from patients suffering from the infectious disease, hepatitis. The VFAs concentrations were high in saliva of hepatitis patients and isobutyric acid detected in sera of hepatitis patients compared to healthy subjects.