• 한국지하수토양환경학회지:지하수토양환경
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• 제15권1호
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• pp.9-18
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• 2010

In this study, Solid-phase micro-extraction (SPME) with Gas Chromatograph using Flame Ionization Detector (GC/FID) was studied as a possible alternative to liquid-liquid extraction for the analysis of Methyl tert-butyl ether (MTBE) and Tertiary-butyl ether (TBA) in water and an optimization condition of trace analysis of MTBE and TBA using the design of experiment (DOE) was described. The aim of our research was to apply experimental design methodology in the optimization condition of trace analysis of fuel oxygenated compounds in soil-phase microextraction with GC/FID. The reactions of SPME were mathematically described as a function of parameters of Temp ($X_1$), Volume ($X_2$), Time ($X_3$) and Salt ($X_4$) being modeled by the use of the partial factorial designs, which was used for fitting 2nd order response surface models and was alternative to central composite designs. The model predicted agreed with the experimentally observed result ($Y_1$(MTBE, $R^2$ = 0.96, $Y_2$ (TBA, $R^2$ = 0.98)). The estimated ridge of the expected maximum responses and optimal conditions for MTBE and TBA were 278.13 and (Temp ($X_1$) = $48.40^{\circ}C$, Volume ($X_2$) = 73.04 mL, Time ($X_3$) = 11.51 min and Salt ($X_4$) = 12,50 mg/L), and 127.89 and (Temp ($X_1$) = $52.12^{\circ}C$, Volume ($X_2$) = 88.88mL, Time ($X_3$) = 65.40 min and Salt ($X_4$) = 12,50 mg/L), respectively.

• 한국지하수토양환경학회지:지하수토양환경
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• 제12권5호
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• pp.73-85
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• 2007

본 연구에서는 액상에서 EGBE, DGBE, DBM, TGME의 효율적인 분석을 위해 이용되던 액상추출법을 대신할 수 있는 방법으로 GC/FID를 이용한 SPME법 실험 연구를 진행하였다. 그리고 실험계획법(DOE)을 사용하여 EGBE를 포함한 디젤첨가제 미량분석의 최적조건을 설명하였다. 실험은 통계분석결과 뿐만 아니라 요인 수의 최적화에 따른 중심합성설계에 의한 완전요인 설계법을 사용하였다. 반응표면분석은 추출 효율이 주 영향인 염농도, 흡착 온도, 흡착 시간과 sonication 시간에 따른 2차 다항식에 의해 설명될 수 있음을 보여주었다. 실험계획법(DOE)을 사용하는 것은 액상 시료에서 디젤첨가제의 정량분석을 개선하는 자료분석법이 될 것이다.

• Bulletin of the Korean Chemical Society
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• 제34권2호
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• pp.531-538
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• 2013

A mass balance method established in this laboratory was applied to determine the purity of an endosulfan-II pure substance. Gas chromatography-flame ionization detector (GC-FID) was used to measure organic impurities. Total of 10 structurally related organic impurities were detected by GC-FID in the material. Water content was determined to be 0.187% by Karl-Fischer (K-F) coulometry with an oven-drying method. Non-volatile residual impurities was not detected by Thermal gravimetric analysis (TGA) within the detection limit of 0.04% (0.7 ${\mu}g$ in absolute amount). Residual solvents within the substance were determined to be 0.007% in the Endosulfan-II pure substance by running GC-FID after dissolving it with two solvents. The purity of the endosulfan-II was finally assigned to be ($99.17{\pm}0.14$)%. Details of the mass balance method including interpretation and evaluating uncertainties of results from each individual methods and the finally assayed purity were also described.

• 분석과학
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• 제20권5호
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• pp.370-382
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• 2007

본 연구에서는 GC/FID를 이용한 SPME법을 적용하여 액상에서 대표적 디젤첨가제인 EGBE, DGBE, DBM, TGME의 미량 분석 가능성을 조사하였다. 또한, 요인배치설계법을 적용하여 EGBE, DGBE, DBM, TGME 미량분석의 최적조건을 도출하였다. 실험은 통계분석결과 뿐만 아니라 요인 수의 최적화에 따른 중심합성설계에 의한 완전요인 설계법을 사용하였으며, 반응표면분석은 추출 효율이 주 영향인염 농도, 흡착 온도, 흡착 시간과 sonication 시간에 따른 2차 다항식에 의해 설명될 수 있음을 보여주었다. 본 연구에서의 결과는 요인배치설계법을 사용하여 액상 시료에서 EGBE, DGBE, DBM, TGME의 정량분석을 개선하는 새로운 자료분석법을 보여주었다.

• Environmental Analysis Health and Toxicology
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• 제15권1_2호
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• pp.53-59
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• 2000

The purpose of this study is the development of the simple and precise determination method of ethyl isocyanate (EIC) and propyl isocyanate (PIC) through derivatization using secondary aliphatic amines by gas chromatography with flame ionization detector. The urea derivatives are quantitatively and simultaneously derived from EIC and PIC with secondary aliphatic amines such as dipropylamine, dibutylamine. and dipentylamine in methylene chloride, and confirmed by thin layer chromatography and gas chromatography with mass selective detector. For GC/FID, according to the increasing carbon atom of the amines, the retention time and peak area of the urea derivatives are increased. The instrumental detection limits for EIC and PIC were about 23.3∼34.8 $\mu\textrm{g}$ and 21.6∼28.9 $\mu\textrm{g}$, respectively.

• 한국산업보건학회지
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• 제33권4호
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• pp.455-463
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• 2023

Objectives: The aim of this study was to develop an air sampling and analytical method for estimating worker exposure to linear carbonate solvents and to evaluate the method. Methods: The target substances were three linear carbonates: DMC, DEC, EMC. GC/FID was used for sample analysis. Laboratory experiments were conducted to determine desorption solvents and sample capacity, and to evaluate storage stability, accuracy, and precision. Results: Coconut Shell Charcoal (CSC, 100/50 mg) was used as the air sampling media, and a desorption solvent of 5% methanol/95% dichloromethane was selected. Recommended sampling capacities were 1~11 ℓ for DMC, 1~18 ℓ for DEC, and 1~24 ℓ for EMC. The stability of three linear carbonates was demonstrated over 30 days in a refrigerator (4℃). Detection limits were determined as follows: DMC 0.26 ㎍/sample, DEC 0.24 ㎍/sample, and EMC 0.25 ㎍/sample. The total coefficient of variation was calculated as DMC 0.064, DEC 0.079, and EMC 0.07. Conclusions: This sampling and analysis method is suitable for estimating personal exposure to linear carbonates in the workplace.

• 한국대기환경학회지
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• 제15권2호
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• pp.121-138
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• 1999

This study was carried out to evaluate the performance of a sampling and analytical methodology for the measurement of selected volatile organic compounds (VOCs) in the ambient air. VOCs were determined by the adsorbent tube sampling and automatic thermal desorption coupled with GC/FID and GC/MSD analysis. Target analytes were aromatic VOCs, including BTEX, 1,3,5-and 1,2,4,-trimethylbenzenes(TMBs), and naphthalene. The methodology was investigatedwith a wide range of performance criteria such as repeatability, linearity, lower detection limits, collection efficiency, thermal conditioning, breakthrough volume and calibration methods using internal and external standards. standards. Stability of samples collected on adsorbent tubes during storage was also investigated. In addition, the sampling and analytical method developed during this study was applied to real samples duplicately collected in various indoor and outdoor environments. Precisions for the duplicate samples and distributed volume samples appeared to be well comparable with the performance criteria recommended by USEPA TO-17. The audit accuracy was estimated by inter-lab comparison of both duplicate samples and standard materials between the two independent labs. The overall precision and accuracy of the method were estimated to be within 30% for major aromatic VOCs such as BTEX. This study demonstrated that the adsorbent sampling and thermal desorption method can be reliably applied for the measurement of BTEX in ppb levels frequently occurred in common indoor and ambient environments.

• 한국지반환경공학회 논문집
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• 제11권5호
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• pp.61-67
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• 2010

본 연구는 GC/FID에서 염화유기용제(PCE와 TCE)와 그 부산물(cis-DCE, VC, 그리고 Ethylene)의 분석을 위하여 액-액추출법의 대안인 SPME방법을 연구하였다. 실험인자로써 fiber의 종류, 흡착 및 탈착시간, headspace의 부피, 염석효과, 그리고 교반효과에 대하여 실험을 실시하였다. 염화유기용제와 부산물의 분석을 위하여 fiber는 CAR/PDMS, 흡착과 탈착시간은 $250^{\circ}C$에서 20분과 5분, 염첨가량 25%와 교반이 병행되었을 때에 최적의 분석조건으로 도출되었다. CAR/PDMS fiber에서 분석물의 추출감도는 PCE>TCE>cis-DCE>VC>Ethylene순으로 조사되었다. 염화유기용제와 부산물의 농도 $10{\mu}g/L$에서 $500{\mu}g/L$까지의 직선상의 상관계수($R^2$)는 0.912에서 0.999로 조사되었으며, $500{\mu}g/L$(5회 분석)일 때에 상대표준편차(% RSD)는 2.1%에서 3.6%로 나타났다. 마지막으로 본 연구에서 염화유기용제와 부산물의 검출한계(LOD)는 $0.5{\mu}g/L$에서 $10{\mu}g/L$로 관측되었다.

• 한국대기환경학회지
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• 제14권5호
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• pp.507-518
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• 1998

A field comparison study was carried out to quantify differences among various sampling and analytical methods for volatile organic compounds (VOCs) at a site in Vlsan in June 1997. Air sampling containers (SUMMA canisters) were used by the Korea Institute of Science and Technology (KIST) and adsorption tubes (carbotrap) were used by Yeungnam University (YN Univ.) for sampling ambient air. Duplicate samples obtained by KIST were analyzed by KIST with a GC-MS system for aromatics and halogenated hydrocarbons and by Atm AA with a GC -FID system for C2∼C9 hydrocarbons, respectively. The adsorption tube samples were analyzed by YN Univ. with a GC-FID system for aromatics. VOC levels for the duplicate canister sampls analyzed by KIST and Atm AA were in good agreement. Concentrations of aromatics by the adsroption tube method were generally higher than those by the canister sampling method by factor of 1.5 to 2.0. Differences between the two sampling methods were discussed.

• Archives of Pharmacal Research
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• 제16권3호
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• pp.175-179
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• 1993

Gas chromoatography with flame ionization detector (FID) along with mass spectrometry (GC/MS) were used for the screening and quantification of methamphetamine (MA) and its major metabolite, amphetamine (AM0, in blood and urine in eleven fatal cases in which MA abuse was suspected. Postmortem blood MA varied from $0.5-30.2\;\mu{g/ml}$, while Am levels ranged from none detected (6 of 11 cases) to 4.8 .mu.g/ml. Additionally, distribution studies were performed in three of these cases in which tissue smaples were available for evaluation. Liver contained the highest ocncentration of MA among the tissu samples. In eight of the eleven cases, when no other direct cause of death was evident (i.e. 3 cases of traumatic dath0, either no blood AM was found or the ratio of MA/AM was 3.4 or greater. These data are consistent with acute MA use followed by death due to acute drug intoxication or by the occurrence of hypersensitivity and reverse seen in cases of chronic drug abuse.