• Analytical Science and Technology
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• v.11 no.5
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• pp.321-331
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• 1998

The separation and sample extraction methods of 19 polycyclic aromatic hydrocarbons (PAHs) in water samples were investigated by gas chromatography/mass spectrometry (GC/MS) and some extraction methods involved liquid-liquid extraction, disk extraction and solid-phase extraction methods. The separation of 19 PAHs was possible by partial variation of oven temperature of GC/MS in temperature range $80{\sim}310^{\circ}C$. Extraction procedures of PAHs in water samples were somewhat modified and compared as extraction recoveries and the simplicity of methods. Extraction recoveries of PAHs were 71.3~109.5% by liquid-liquid extraction method. By using disk extraction, good extraction recoveries (80.7~94.9%) were obtained in case of $C_{18}$ disk extraction method by filtration. And extraction recoveries of PAHs by $C_{18}$ solid-phase were in the range of 51.8~77.9%. Method detection limits (S/N=5) of 19 PAHs were in the range of 0.25~6.25 ppb by liquid-liquid extraction and solid-phase extraction and 0.05~1.25 ppb by disk extraction methods.

• Environmental Analysis Health and Toxicology
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• v.18 no.1
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• pp.45-55
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• 2003

The alkylphenols, chlorophenols and bisphenol A were determined by gas chromatography/mass spectrom-etry-selected ion monitoring (GC/MS-SIM) mode followed by two work-up methods for comparison; isoBOC derivatization method and TBDMS derivatization method. Eleven phenols in paper samples were extracted with acetonitrile. Also, solid -phase extraction (SPE) with XAD -4 and subsequent conversion to isobutoxycarbonyl derivatives or tert.-butyldimethylsilyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The SIM responses were linear with the correlation coefficient varying 0.9717 ∼ 0.9995 (isoBOC derivatization), and 0.9842 ∼ 0.9980 (TBDMS derivatization). The recoveries were 82.4 ∼ 108.8％) by area ratio of phenanthrene -d$\_$10/ vs bisphenol A-d$\^$l6/. (isoBOC derivatization and TBDMS derivatization) The range of concentrations was respectively, 0.95 ∼ 1.44 ng/g in 2,4-dichlorophenol, 1.01 ∼ 1.17 ng/g in t-butylphenol,2.17 ∼ 5.84 ng/g in pentachlorophenol, 12.68 ∼ 14.88 ng/g in nonylphenol and 30.84 ∼ 153.72 ng/g in bisphenol A.

• Analytical Science and Technology
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• v.16 no.6
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• pp.458-465
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• 2003

The HS (headspace)-SPME (Solid phase microextraction) as rapid and simple method was performed for the determination of volatile fatty acids (VFAs) from the aqueous samples. In-fiber derivatization of VFAs with 1-Pyrenyldiazomethane (PDAM) was applied to improve their sensitivity of detection. In SPME procedure, typical parameters such as effects of solution pH, and salting out reagent and ultrasonication were investigated to improve the extraction efficiency. Based on the developed method, VFAs in wastewater samples were determined by gas chromatography / mass spectrometry-selected ion monitoring (GC/MS-SIM) mode.

• Environmental Analysis Health and Toxicology
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• v.20 no.1
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• pp.47-55
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• 2005

본 연구는 GC/MS를 이용하여 수질, 토양 및 저질 시료 중의 benzo(a)pyrene(BaP)을 분석하는 방법을 확립하고자 하였다. BaP은 수질 시료(100mL)에서 n-hexane으로 추출하였으며, 토양 및 저질 시료(l0g) 에서는 먼저 메탄올로 추출한 후 hexane으로 다시 추출하여 농축시켜 분석하였다. 수질 시료 중의 BaP 회수율은 94.8% 이상이었으며 토양에서의 회수율은 약 93％를 보였고 재현성은 10.49% 이하였다. 검정 곡선은 상관계수(R²)값이 수질과 토양 모두에서 0.996 이상의 좋은 직선성을 보여주었다. 토양 시료의 경우 35지역 중 6지역의 토양에서 0.5～223.5㎍/kg의 농도 범위로 BaP가 검출되었으며 수질과 저질 시료에서는 모든 지역에서 검출한계 이하로 나타났다. 이 분석방법은 환경 중에 미량으로 존재하는 BaP의 분석과 모니터링에 유용하게 사용할 수 있는 적합한 방법이라 사료된다.

• Korean Journal of Heritage: History & Science
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• v.55 no.4
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• pp.166-177
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• 2022

The Shiveet Khairkhan is located on Tsengel Som in the middle of Bayan-ulgi Aimag in the Altai region. Various remains have been identified, and it has been found to be an important area of the Eurasian steppe. In this study, the characteristics of textile fibers and dyes excavated from the tombs of the 1st~3rd century Xianbei period in the sites of Shiveet Khairkhan, Mongolia were investigated. As a result of analysis using optical microscopic observation and attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR) for fiber identification, green and yellow fabrics were identified as silk fabrics. To investigate the properties of the dye, the surface reflectance of the dyed fabric was measured using an fiber optic reflectance spectrophotometer for non-destructive analysis. The green fabric appeared similar to the reflection spectrum of indigo dye. In addition, as a result of component analysis using gas chromatography-mass spectrometry, isatin and indigotine were detected. Isatin and indigotine are characteristic components of indigo dye, and it was found that the green fabric of the tombs of the Xianbei period was dyed using indigo dye. It was difficult to identify the type of dye in the yellow fabric as a result of reflectance spectrum and gas chromatography analysis. Indigo plants are a dye used for blue dyeing from thousands of years ago, and many species are distributed around the world. It was confirmed that the fabric was relatively well preserved and indigo dye was used for the green Jikryeongui (garment with a straight collar) in the ancient tomb of the Xianbei period about 1,800 years ago, even though it was buried for a long time. Scientific investigation of textile cultural heritage is an essential process for conservation treatment, restoration, exhibition, and the creation of a conservation environment. It is expected that related research will be activated in the future and will be helpful in interpreting the living culture at the time, preserving textiles, and a conservation environment.

• Environmental Analysis Health and Toxicology
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• v.20 no.2 s.49
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• pp.123-131
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• 2005

본 연구는 GC/MS를 이용하여 수질, 토양 및 저질 시료 중의 4-Nitrotoluene(4-NT)을 분석하는 방법을 확립하고자 하였다. 4-NT은 수질 시료(100mL)에서 n-hexane으로 추출하였으며, 토양 및 저질 시료(10g)에서는 먼저 메탄올로 추출한 후 hexane으로 다시 추출하여 농축시켜 분석하였다. 수질 시료 중의 4-NT의 회수율은 $99.1\%$ 이상이였으며 토양에서의 회수율(recovery)은 약 $110\%$를 보였고 재현성 (relative standard deviation)은 $11.99\%$ 이하였다. 검정곡선은 상관계수$(R^2)$값이 수질과 토양 모두에서 0.994이상의 좋은 직선성을 보여주었다. 본 연구에서 채취한 수질 43개 지역, 토양 35개 지역 및 저질 11개 지역의 모든 시료에서 4-NT은 검출한계 이하로 나타났다. 이 분석방법은 환경 중에 미량으로 존재하는 4-NT의 분석과 모니터링에 유용하게 사용할 수 있는 적합한 방법이라 사료된다.

• Analytical Science and Technology
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• v.7 no.1
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• pp.65-78
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• 1994

The herbicide mixture of 7 triazines and 9 phenoxyalkanoic acid esters was simultaneously separated and determinated with the selected ion monitoring by using gas chromatography/mass spectrometry. The extraction recoveries of those herbicides from the reagent water were studied for the organic solvent extraction(LLE) with methylene chloride. The calibration curves of them showed good linearity over the concentration range of 0.2~0.5ng/ml and the detection limits were 0.2~0.5ng/ml for 100ml of water. This analytical method could be applied to the drinking water and biological sample.

• Journal of the Korean Chemical Society
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• v.39 no.7
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• pp.513-523
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• 1995

Polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs) are the most concerned toxic organic pollutants to human. Because of their extremely high toxicity and uncertain genotoxic potential, their determination in environmental and biological samples is of great interest. Municipal solid waste incinerator facilities have been reported as the major contributors of dioxins and furans to the environment, and their formation from combustion is a universal phenomenon, everywhere. In this study dioxins and furans were analyzed from the bottom ash produced during combustion in an municipal waste incinerator located in Seoul. The EPA method was modified for sample pretreatment: the soxhlet method was used for extraction and clean-up procedures were performed by using silica and basic alumina, excluding active-carbon. The extract was then analyzed by HRGC/HRMS. A general trend of increase in the amounts of 6∼7 chlorine-substituted dioxins and furans was observed. Total dioxins, furans and 2,3,7,8-TCDD were determined as 8.05 ng/g, 4.75 ng/g, and 6.93 pg/g, respectively.

• Applied Chemistry for Engineering
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• v.20 no.2
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• pp.177-185
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• 2009

The failure analysis of scales deposited on automotive thermostat housing has been carried out. Observations using energy dispersive spectroscopy and electron probe micro analyzer indicate that the main components of scales are some of additives of coolant used. For a detailed investigation of organic matters pyrolysis-GC/MS is employed. The result shows that the main organic component is benzoic acid and furthermore, a small amount of acetophenone, benzene and phenyl group is detected. Based on the results of failure analysis performed, the scales on automotive thermostat housing appear due to the deposition of coolant components, followed by crevice corrosion, into gap between housing and rubber horse. New accelerated test methodology, which could mimic the scale formation and the crevice corrosion on thermostat housing, is developed considering the above results. In order to reproduce the real operating conditions, the accelerating factors, i.e. temperature and humidity, are changed and programmed. The reproducibility of the accelerated test proposed is confirmed after analyzing the scales obtained from the accelerated test.

• Analytical Science and Technology
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• v.9 no.4
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• pp.392-398
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• 1996

Eleven organic chemical substances, tetrachloroethylene, ethyl benzene, p-xylene, o-xylene, isopropyl benzene, n-propyl benzene. 1,2,4-trimethyl benzene, 1,3,5-trimethyl benzene, p-isopropyl toluene. see-butyl benzene, and naphthalene, which have hazardously influenced to human, were extracted from untreated wastewater collected at 26 companies of 8 types industry in the basin of Kwangju stream. Their structures were elucidated by Gas Chromatography/Mass Spectrometry(GC/MS) and in comparison with each standard reagents.