• Title/Summary/Keyword: Pyrolysis gas chromatography

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Identification of the Derivated Species from Traditional Coating Films (전통 칠 유래 성분의 확인)

  • Shin, Jeoung Hwa;Ahn, Yun Gyong
    • The Korean Journal of Community Living Science
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    • v.24 no.2
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    • pp.243-249
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    • 2013
  • Identification of coating film species from ancient coating materials is needed to maintaine their surfaces without loss of their original beauty for a long time and understand the historical background of manufacturing techniques. A pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) was applied to identify the origine of films in ancient coating materials. The pyrolysis products, which reflect the source from which they originate were detected distinctively at $500^{\circ}C$. This is a rapid technique that does not require large amounts of sample or any sample preparation. Sesquiterpenes are a class of terpenes that consist of three isoprene units were identified as cadienes, selinenes, cubebenes from the raw material of dendropanax morbifera. On the other hand, alkanes(tetra~heptadecanes), alkenes (tri~heptadecenes), allkyphenols, catechols and fatty acids were detected from the raw material of the lacquer film. Based on these results, the origine of historic coatings artifacts was identified using py-GC/MS by comparison with their pyrolysis products.

Study of Pyrolysis Pattern and Transfer Rate of Organochlorine Pesticide in Tobacco

  • Min, Hye-Jeong;Jang, Seok-Su;Kim, Ick-Joong;Kim, Yong-Ha;Min, Young-Keun
    • Journal of the Korean Society of Tobacco Science
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    • v.29 no.2
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    • pp.118-124
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    • 2007
  • GRLs(Guidance Residue Levels) of agricultural chemicals for tobacco are recommended by the CORESTA Agro-Chemical Advisory Committee guide. In the GRLs list, organochlorine group is one of pesticides commonly used on tobacco cultivation. In this model study, the quantitative correlation in the transfer rate of pesticide residue into tobacco smoke by spiking of organochlorine pesticides to cigarette and pyrolysates were investigated. The spiking concentration referred to the range of GRLs list and the organochlorine pesticides in mainstream smoke were analyzed by GC-MS. For the understanding of the composition variation versus temperature, the behavior of pesticides was investigated by pyrolysis-gas chromatography-mass spectrometry(Py-GC-MS). In this study, the transfer rate of pesticide residue into tobacco smoke at four different spiking concentration and the composition of pyrolysates were analyzed differently. At $10\;{\mu}g/cig$ spiking concentrations, the organochlorine pesticides were transferred into tobacco smoke in $0.02\;{\sim}\;10.19\;%$ each of component and the most of pesticides were pyrolyzed during smoking. It was found that the decomposition compounds from organochlorine pesticides were mainly composed of oxygenated and nitrogenous compounds. This study could estimate that the transfer rate of pesticides into tobacco smoke is very small amount.

Formation of Polybrominated Dibenzo-p-dioxins/Furans (PBDDs/Fs) by the Pyrolysis of 2,4-Dibromophenol, 2,6-Dibromophenol, and 2,4,6-Tribromophenol

  • Na, Yun-Cheol;Hong, Jong-Ki;Kim, Kang-Jin
    • Bulletin of the Korean Chemical Society
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    • v.28 no.4
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    • pp.547-552
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    • 2007
  • This study examined the thermal reactions of 2,4-dibromophenol (diBP), 2,6-diBP and 2,4,6-triBP. The products obtained under pyrolytic conditions were analyzed by gas chromatography/mass spectrometry (GC/MS). 2,7-dibromodibenzo-p-dioxin (diBDD) was the major compound produced from the thermal reaction of 2,4-diBP. In addition, monoBDD and triBDDs were obtained through a process of debromination and bromination, respectively. The pyrolysis of 2,6-diBP and 2,4,6-triBP produced two major brominated dioxin isomers through direct condensation and a Smiles rearrangement. The two ortho-Brs in 2,6-diBP and 2,4,6-triBP mainly led to the production of dioxins, whereas in addition to 2,7-diBDD, 2,4-diBP produced two furans as minor products, 2,8-dibromodibenzofuran (diBDF) and 2,4,8-triBDF, through the intermediate dihydroxybiphenyl (DOHB). The maximum yield of the major dioxins was obtained at 400 oC, and decomposition by debromination at 500 oC resulted in less substituted bromodioxins.

Analysis of Minor Additives and Polymer in Used-stripper Using Pyrolysis-Gas Chromatography/Mass Spectrometry and Electrospray Mass Spectrometry

  • Koo, Jeong-Boon;Park, Chang-Hyun;Han, Cheol;Na, Yun-Cheol
    • Bulletin of the Korean Chemical Society
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    • v.30 no.2
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    • pp.368-372
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    • 2009
  • The trace polymer and additives in used stripper solutions were analyzed by a combination of Py-GC/MS and ESI-MS. In the comparison of the pyrolysates produced by the pyrolysis of the pure stripper and photoresist at $500{^{\circ}C}$, the presence of novolac polymer in the used stripper was confirmed by the presence of the characteristic peaks of its pyrolysates, such as those of the methylphenol, di-methylphenol and methylenebis(methylphenol) isomers. The intact trace polymer was measured by ESI-MS, which showed the distribution of oligomers at intervals of 120 Da, indicating di-methylphenol to be the repeat unit. Additional MS/MS measurements demonstrated that the end group is methylphenol and the repeat groups are di-methylphenol. Some modified oligomers caused by the methylation or di-methylation of the repeat unit were also identified. Although the polymer is only present at a trace level in the used stripper, these combined analytical methods provided the means to qualify the stripper solution through the identification and structural determination of the polymer.

Synthesis of Methyl Alcohol and Alternative Gases for Petroleum by Thermochemical Gasification of Waste Lignocellulosic Materials (I) - Thermochemical Conversion of Sawdust, Ricestraw and Ricehusk Using Alkali Salts as Catalyst - (목질(木質) 폐재(廢材)의 열(熱)-화학적(化學的) 방법에 의한 메틸알콜과 대체(代替)에너지 가스의 합성(合成)(I) - 알카리염(鹽)을 촉매로 사용한 톱밥, 볏집 그리고 왕겨의 열화학적(熱化學的) 분해(分解) -)

  • Lee, Byung-Guen
    • Journal of the Korean Wood Science and Technology
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    • v.14 no.2
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    • pp.21-28
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    • 1986
  • A quartz type gasification reactor was designed and used for pyrolysis and gasification of sawdust, ricestraw and ricehusk. The initial reaction temperature was 350$^{\circ}C$, and up to 550$^{\circ}C$ to complete pyrolysis and gasification reaction. In order to examine the effect of catalyst on reaction temperature, $K_2CO_3$ and $Na_2CO_3$ as catalyst were also used. The product gas mixtures are identified to be CO, $CO_2$, $CH_4$ and $CH_3CHO$ etc. by Gas Chromatography and Mass Spectrometer. The highest gas volume of the gasified sawdust at 550$^{\circ}C$ amounts to 1800ml/g of sawdust, even though the yield and composition of this product gas are depending on the reaction temperature of the reactor and catalyst used.

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Extraction Characteristics of Dried Asian Lacquer by Solvents Before and After UV Degradation (자외선 열화 전후 건조 옻의 용매별 용출 특성)

  • Park, Jongseo;Schilling, Michael R.;Khanjian, Herant;Heginbotham, Arlen
    • Journal of Conservation Science
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    • v.36 no.2
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    • pp.103-111
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    • 2020
  • To compare the cleaning effect of solvents such as water and ethanol used to clean lacquer relics, the components extracted with various solvents were analyzed. A freshly dried lacquer sample and a lacquer sample exposed to ultraviolet radiation for 24 days were treated with water, ethanol, acetone, and hexane, and the dissolved material was detected by pyrolysis-gas chromatography-mass spectrometry. The amount extracted was significantly higher in acetone and ethanol than in hexane, a nonpolar solvent. Water, a highly polar solvent, was relatively efficient for extracting low-molecular-weight materials. After experiencing 24 days of ultraviolet radiation, the lacquer exhibited a significant increase of extracted materials compared with the nonexposed one. This may be due to the degradation of the urushiol chain in the form of polymers, resulting in the formation of low-molecular-weight polar substances, including dicarboxylic acids. In addition to the deterioration status of lacquer relics, such solvent extraction properties will be a crucial consideration in selecting the appropriate cleaning solvent.

Research Trend on the Accumulation Routes of Microplastics in Soil and Their Analytical Methodologies (토양 내 미세플라스틱의 축적경로 및 분석기법 연구 동향)

  • Choi, Hyung-Jun;An, Jinsung;Choi, Suk Soon
    • Applied Chemistry for Engineering
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    • v.31 no.4
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    • pp.360-367
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    • 2020
  • In this study, the accumulation and distribution routes of microplastics in soil environment were examined, and their analytical methodologies were summarized. Density separation and removal process of inhibition materials were introduced for the separation of microplastics in soil and the basic principles and limitations of quantitative and qualitative analyses including pyrolysis gas chromatography mass spectrometry, µ-Raman spectrometry, fourier transform infrared spectrometry, and microscopes were investigated. Chemical extraction methods for the analysis of mediated hazardous substance (additives and sorbed matters) in microplastics were also discussed with focusing on in vitro bioaccessibility assay for the human oral exposure route. Based on the described methodologies for the analysis of microplastics in soil, it is expected that these methods enable to select appropriate analysis techniques in consideration of medium state, contamination level and sample quantity.

Analysis of Automotive Paints using Pyrolysis-Gas Chromatography (열분해-가스크로마토그라피에 의한 자동차 페인트 분석)

  • Shon, Sung-Kun;Park, Ha-Sun;Lee, Jin-Sook;Hong, Sung-Wook;Park, Sung-Woo;Cho, Sung-Hye
    • Analytical Science and Technology
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    • v.13 no.1
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    • pp.101-107
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    • 2000
  • The automotive paints could be generally differentiated by color, layer sequence and chemistry of the paint layers comprising each of the topcoat and the primer system. The successful identification of hit-andrun a and traffic accidental vehicles from evidential paint fiagments is greatly facilitated with a comprehensive laboratory collection of reference paint samples and the technique for direct analysis without sample preparation. The Pyrolysis-Gas Chromatography(PGC) is a precise and reliable method for performing both quantitative and qualitative analysis of polymeric materials and forensic samples. Our Forensic Laboratory is conducting the examination and identification of 73 reference paint samples; 4 colors of each domestic automotive make that is popular in Korea, by Curie Point Pyrolyzer(JHP-3) and GC with capillary column(ultra alloy-5). This method can be used not only to compare paint traces with their suspected sources, but also to identify the type, make and model of the automotive car.

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Synthesis of Methane-rich Gases(Alternative Energy) by Thermochemical Gasification from Waste Municipal and Lignocellulosic Materials (목질 폐재와 가정용 쓰레기의 열-화학적 분해에 의한 고수율 메탄가스(대체연료)의 합성)

  • Lee, Byung-Guen;Lee, Sun-Haing
    • Journal of the Korean Wood Science and Technology
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    • v.17 no.2
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    • pp.13-19
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    • 1989
  • Two different quartz types of gasification reactor were used for pyrolysis and gasification of sawdust, ricestraw, ricehusk and municipal wastes which contain only cellulosics., operating at 1 atmospheric and vacuum pressure respectively. Also a stainless steel autoclave gasification reactor was used which is possible to use up to 100 atmospheric pressures and $800^{\circ}C$ of reaction temperature to complete pyrolysis and gasification reaction. The catalysts used in this reaction w- ere $K_2CO_3$, $Na_2CO_3$, Ni and Ni-$K_2CO_3$ as CO-Catalyst. The product gas mixtures were identified to be CO, $CO_2$, $C_3H_3$, $CH_4$ and $CH_3CHO$ etc. by Gas Chromatography and Mass Spectrometry. The pressurized gasification reaction shows significant increase in terms of methane composition and yield of product gases, comparing with those from unpressurized gasification reactions. The total volume of product gas mixtures amounts to 1600-1800ml per1gof waste of waste lignocellulosics or municipal waste, and the metane content of the gas mixtures reached to 40%, when $800^{\circ}C$ of reaction temperature and 100 atmospheric pressures with Ni-$K_2CO_3$ as CO-catalyst in the pressurized gasification reaction were used. This results show that the product gas mixtures containing 40% of methane call be used for alternative enegy source.

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Composition of the Adhesive Used for Fixing Glass Eyes of the Stone Standing Maitreya of Daejosa Temple, Buyeo (Treasure No. 217)

  • Park, Jongseo;Lee, Sunmyung
    • Journal of Conservation Science
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    • v.35 no.4
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    • pp.295-307
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    • 2019
  • In the process of the conservation treatment of the glass eyes of the stone standing Maitreya of Daejosa temple, Buyeo (Treasure No. 217), a blackish material, expected to be the adhesive for fixing the glass eyes, was collected and analyzed. Infrared spectroscopy and pyrolysis/gas chromatography/mass spectrometry (pyrolysis/GC/MS) were employed to identify the organic material in the sample. The IR analysis revealed the presence of materials such as apatite or bone black. The pyrogram of the sample was similar to that of Asian lacquer, among traditional adhesives. In particular, the pyrolysis/GC/MS analysis with online methylation detected 1,2-dimethoxy-3-pentadecylbenzene, methyl 7-(2,3- dimethoxyphenyl) heptanoate, and methyl 8-(2,3-dimethoxyphenyl)octanoate. These are known to be the pyrolysis products of catechol and its oxidation product, which indicated the presence of Asian lacquer in the sample. X-ray diffraction, X-ray fluorescence, and thermal gravimetry analysis showed that the sample contained ca. 60% inorganic substances, including apatite. Radiocarbon dating of the sample suggested that the blackish material was applied between the late 13th and early 15th century, revealing some discrepancy with the art-historical manufacturing time of the Maitreya. From the above analysis, it was concluded that Asian lacquer and bone ash were used to attach the glass eyes by forming a thick blackish lacquer layer.