• Bulletin of the Korean Chemical Society
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• 제35권7호
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• pp.2057-2064
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• 2014

Thermochemical sulfate reduction (TSR) was conducted in autoclave on the system of crude oil and $MgSO_4$ at different temperatures. Gas chromatography pulsed flame photometric detector (GC-PFPD) was used to detected the composition of organic sulfur compounds in oil phase products. The results of the analysis indicate that with increased temperature, the contents of organic sulfur compounds with high molecular weight and thermal stability, such as benzothiophenes and dibenzothiophenes, gradually became dominated. In order to gain greater insight into the formation and distribution of organic sulphur compounds from TSR, positive ion electrospray Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) was used in detecting the detailed elemental composition and distribution of them. The mass spectra showed that the mass range of sulfur compounds was 200-550 Da. Four sulfur class species, $S_1$, $N_1S_1$, $O_1S_1$ and $O_2S_1$, were assigned in the positive-ion spectrum. Among the identified sulfur compounds, the $S_1$ class species was dominant. The most abundant $S_1$ class species increase associated with the DBE value and carbon number increasing which also indicates the evolution of organic sulfur compounds in TSR is from the labile series to the stable one. In pure blank pyrolysis experiments with crude oil cracking without TSR, different composition and distribution of organic sulfur compounds in oil phase products were seen from mass spectra in order to evaluate their pyrolysis behaviors without $MgSO_4$. FT-IR and XRD were used in analyzing the products of solid phases. Two distinct crystallographic phases MgO and $MgSO_4$ are found to coexist in the products which demonstrated the transformation of inorganic sulfur compounds into organosulfur compounds exist in TSR.

• 보존과학회지
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• 제34권5호
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• pp.369-377
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• 2018

경북 경산에 위치한 원삼국시대 고분인 임당1호분에서 출토된 칠초 철제 고리자루칼의 칠편에 대해 칠의 구성성분과 풍화상태를 확인하기 위해 열분해/GC/MS법으로 유기물을 분석하였다. 직접 열분해/GC/MS법에서 칠편과 원주산 건조옻이 대체적으로 유사한 크로마토그램을 보였다. THM(thermally assisted hydrolysis and methylation)-열분해/GC/MS법의 경우 칠편에서 한국에 자생하는 옻나무 종의 특징적인 성분(1,2-dimethoxy-3-pentadecylbenzene 등)이 관찰되었다. 또한, dimethyl nonanedioate 등 건성유에서 비롯되는 것으로 보이는 성분도 검출되었다. 칠편에서 산화된 catechol 성분이 다량 검출되는 것으로 보아 칠의 열화가 우루시올 성분의 산화와 관련 있을 것으로 추정된다. 이로부터 임당1호분 고리자루칼 칠은 옻과 건성유를 사용하였고 오랜 시간의 경과로 산화가 많이 진행된 상태인 것으로 판단된다.

• 한국대기환경학회지
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• 제2권2호
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• pp.60-65
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• 1986

Atmospheric particulates were collected at a site near the front gate of the Yonsei University using nine stages Andersen air sampler and the distribution of seasonal particle size was investigated. Rubber, Pb and Zn contents of the collected particulates in each stage were determined. Particle size distribution of atmospheric particulate, which was made by concentration distribution curve method, was usually divided into two groups, course (particles larger than 1 - 2 $\mu m in diameter$) and fine (particles smaller than 1 - 2 \mu m in diameter$) groups, regardless of sampling period. More than 80 percent of the total rubber contents in atmospheric particulates were larger than $5 \mu m$ in diameter, meaning that most of rubber particles were originated from tire tread. After benzene extraction for 4 hrs, the extracts were analyzed by Curie-point pyrolysis gas chromatography for rubber content. Pb and Zn contents were determined by atomic absorption spectroscopy. The annual average concentration of rubber particles was $4.2 \mu g/m^3$, which corresponded to 2.2% of the annual average total suspended particulates. Average concentration of styrene brtadiene rubber was about five times that of natural rubber. Annual average concentrations of Pb and Zn were $1.2 \mu g/m^3 and 0.4 \mu g/m^3$ respectively, which corresponded to about 0.7% and 0.2% of the annual average total suspended particulates.

• 한국철도학회:학술대회논문집
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• 한국철도학회 2008년도 추계학술대회 논문집
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• pp.406-415
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• 2008

Recently, the amount of thermosetting plastic wastes have increased with the production of reinforced plastic composites and causes serious environmental problems. The epoxy composites, one of the versatile thermosetting plastics with excellent properties, cannot be melted down and remolded as what is done in the thermoplastic industry. In this research, a series of experiments that recovers carbon fibers from carbon fiber reinforced epoxy composites for train body was performed. We experimentally examined various decomposition processes and compared their decomposition efficiencies and mechanical property of recovered carbon fibers. For the prevention of tangle of recovered carbon fibers, each composites specimen was fixed with a Teflon supporter and no mechanical mixing was applied. Decomposition products were analyzed by scanning electron microscope (SEM), gas chromatography mass spectrometer (GC-MS), and universal testing machine (UTM). Carbon fibers could be completely recovered from decomposition process using nitric acid aqueous solution, liquid-phase thermal cracking and pyrolysis. The tensile strength losses of the recovered carbon fibers were less than 4%.

• 한국산업보건학회지
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• 제34권1호
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• pp.14-17
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• 2024

Objectives: This is a case of air exposure assessment conducted after researchers complained of headaches and odor due to residual substances from fire extinguishing agents spread throughout the laboratory due to a malfunction of the fire extinguishing facility. Methods: A component analysis was conducted on the residual substances of a fire extinguishing agent spread in a laboratory using Py-GC-MS (pyrolysis gas chromatography mass spectrometry) at the research institute's own central equipment research center. As a result of the component analysis, several types of substances were detected. Among these, five types of substances subject to work environment measurement in the aromatic hydrocarbon series, which can affect headaches and odor, were selected as substances subject to exposure assessment in the air, and the measurement and analysis methods of the target substances were conducted in accordance with the KOSHA Guide for each substance. Conclusions: The measurement results showed that all 5 types of substances were not detected at locations A, B, and C. This is believed to be the result of the residual substances in the fire extinguishing agent being measured when approximately two months had elapsed after being exposed to the test bench, and the substances already exposed had volatilized and disappeared. In this survey, it is believed that the measurement process is more important than the measurement results.

• 한국근적외분광분석학회:학술대회논문집
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• 한국근적외분광분석학회 2001년도 NIR-2001
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• pp.1516-1516
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• 2001

During the recent years, wine analysis has played an increasing role due the health benefits of phenolic ingredients in red wine [1]. On the other hand there is the need to be able to distinguish between different wine varieties. Consumers want to know if a wine is an adulterated one or if it is based on the pure grape. Producers need to certificate their wines in order to ensure compliance with legal regulations. Up to now, the attempts to investigate the origin of wines were based on high-performance liquid chromatography (HPLC), gas chromatography (GC) and pyrolysis mass spectrometry (PMS) [l,2,3]. These methods need sample pretreatment, long analysis times and therefore lack of high sample throughput. In contradiction to these techniques using near infrared spectroscopy (NIRS), no sample pretreatment is necessary and the analysis time for one sample is only about 10 seconds. Hence, a near infrared spectroscopic method is presented that allows a fast classification of wine varieties in bottled red wines. For this, the spectra of 50 bottles of Cabernet Sauvignon, Lagrein and Sangiovese (Chianti) were recorded without any sample pretreatment over a wavelength range from 1000 to 2500 nm with a resolution of 12 cm$\^$-1/. 10 scans were used for an average spectrum. In order to yield best reproducibility, wines were thermostated at 23$^{\circ}C$ and a optical layer thickness of 3 mm was used. All recorded spectra were partitioned into a calibration and validation set (70% and 30%). Finally, a 3d scatter plot of the different investigated varieties allowed to distinguish between Cabernet Sauvignon, Lagrein and Sangiovese (Chianti). Considering the short analysis times this NRS-method will be an interesting tool for the quality control of wine verification and also for experienced sommeliers.

• 보존과학회지
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• 제32권1호
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• pp.21-32
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• 2016

아교는 나전, 목가구, 단청 등 문화재에 접착제 및 교착제로 광범위하게 사용돼 온 전통재료이다. 아교의 분석과 확인은 주로 IR에 의한 작용기의 확인을 통해 이루어졌으나 몇 가지 물질이 섞여 있는 경우 밴드의 중복 등에 의해 명확하게 아교를 확인하는데 어려움이 있다. 열분해/GC/MS분석은 소량의 시료로 열분해 산물의 화학성분을 알 수 있어 아교 등 고분자 재료의 성분을 분석하는데 유용하다. 본 연구에서는 단청 시편에서 아교를 이 방법으로 확인하고자 하였다. 우선, 단청 채색에 사용되는 아교, 동유에 대한 열분해/GC/MS 분석을 실시하여 주요하면서 특징적인 열분해산물을 확인하였다. 또한, 뇌록을 칠한 단청시편을 제작하여 열충격 시험과 인공 풍화 시험 후에 분석을 했을 때 약화가 되긴 하였지만 아교의 특징적인 peak의 검출이 가능하였다. 이로부터, 단청과 같이 다양한 재료와 풍화상태로 구성된 문화재에서 아교의 검출이 열분해/GC/MS로 가능함을 확인하였다. 아울러, 단청 시편을 IR로 분석하여 IR과 열분해/GC/MS 분석 간에 아교 검출 능력을 비교하였다.

• 공업화학
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• 제28권4호
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• pp.490-494
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• 2017

최근 차량 증가와 더불어 이에 따른 사고 또한 증가하고 있는 추세로써 대부분의 사고차량에서 도색작업이 반드시 요구되고 있다. 통상적인 차량 도색시 다량의 유기용제가 사용되어 환경문제가 대두되고 있으며 이에 대처하기 위해 최근 수용성 도료가 국내에서도 개발되고 그 사용이 증가하고 있다. 그러나 수용성 도료의 경우 도장 작업비용이 고가이기에 정비공장에서 보험금 과다청구의 수단으로 악용하는 사례 또한 적지 않다. 본 연구에서는 수용성 도료를 사용하였는지 여부를 규명하기 위해 수용성 도료에 사용되는 비이온성 계면활성제 성분인 Surfynol 104 성분을 지표물질로 하여 퀴리포인트를 이용한 열분해-기체크로마토그래피/질량분석법(Py-GC/MS)으로 분석하였다. 분석결과 도색작업이 완료된 실제 차량 페인트에서 동위원소 치환된 fluoranthene-d10을 내부표준물질로 하여 표준물첨가법(standard addition method)으로 약 0.38%의 계면활성제 성분이 검출되었다.

• Asian Journal of Atmospheric Environment
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• 제6권1호
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• pp.53-66
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• 2012

A comparison of analytical approaches for Levoglucosan ($C_6H_{10}O_5$, commonly formed from the pyrolysis of carbohydrates such as cellulose) and used for a molecular marker in biomass burning is made between the four different analytical systems. 1) Spectrothermography technique as the evaluation of thermograms of carbon using Elemental Carbon & Organic Carbon Analyzer, 2) mass spectrometry technique using Gas Chromatography/mass spectrometer (GC/MS), 3) Aerosol Mass Spectrometer (AMS) for the identification of the particle size distribution and chemical composition, and 4) two dimensional Gas Chromatography with Time of Flight mass spectrometry (GC${\times}$GC-TOFMS) for defining the signature of Levoglucosan in terms of chemical analytical process. First, a Spectrothermography, which is defined as the graphical representation of the carbon, can be measured as a function of temperature during the thermal separation process and spectrothermographic analysis. GC/MS can detect mass fragment ions of Levoglucosan characterized by its base peak at m/z 60, 73 in mass fragment-grams by methylation and m/z 217, 204 by trimethylsilylderivatives (TMS-derivatives). AMS can be used to analyze the base peak at m/z 60.021, 73.029 in mass fragment-grams with a multiple-peak Gaussian curve fit algorithm. In the analysis of TMS derivatives by GC${\times}$GC-TOFMS, it can detect m/z 73 as the base ion for the identification of Levoglucosan. It can also observe m/z 217 and 204 with existence of m/z 333. Although the ratios of m/z 217 and m/z 204 to the base ion (m/z 73) in the mass spectrum of GC${\times}$GC-TOFMS lower than those of GC/MS, Levoglucosan can be separated and characterized from D (-) +Ribose in the mixture of sugar compounds. At last, the environmental significance of Levoglucosan will be discussed with respect to the health effect to offer important opportunities for clinical and potential epidemiological research for reducing incidence of cardiovascular and respiratory diseases.

• 대한화학회지
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• 제16권5호
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• pp.314-319
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• 1972

N-methyl-p-aminophenol은, 酸素存在下, 철-킬레이트(Fe(III)-EDTA) 水溶液中에서 酸化重合하여 黑色의 Oligo-(N-methyl-p-aminophenol)을 定量的으로 生成한다. 이 酸化重合過程에서 單量體中의 N에 結合된 $CH_3$ group이 일부 脫離되는데, 이것은 oligo-(N-methyl-p-aminophenol)을 아세톤처리하여 얻은 아세톤 可溶部와 不溶部의 赤外線스펙트럼에서 ${\delta}\;asym\;CH_3\;1460\;cm^{-1}$ 및 ${\delta}\;sym\;CH_3\;1380\;cm^{-1}$의 吸收가 候者의 경우 현저히 弱化된 것으로 明白하다. $N_2$氣流中에서 每分 $2^{\circ}C$의 上昇速度로 行한 TGA分析結果, $600^{\circ}C$에서 약 40%의 重量損傷을 나타내며, $CH_3$ 置換基가 없는 p-aminophenol보다 耐熱性이 떨어진다. 또한 이 生成올리고머의 He 氣流中에서 행한 熱分解反應에서의 生成物은 單量體인 N-methyl-p-aminophenol과 물이 確認되었고 分解가스로부터는 gas chromatography에서 $H_2,\;CO,\;CO_2$등이 確認되었다. 生成올리고머의 熱處理에서는 일부는 1次元的인 構造가 切斷되어 單量體로 分解되지만, 대부분은 melt polycondensation이 일어나 더 큰 重合體로 변함과 동시에 熱에 安定한 環式構造로 변하여 감이 確認되었다