• Title/Summary/Keyword: Pyrolysis mass spectrometry

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Polyhydroxyamic Acid from 3,3′ - Dihydroxybenzidine and Pyromellitic Dianhydride as a Fire-safe Polymer

  • Park, Seung Koo;Farris, Richard J.;Kantor, Simon W.
    • Fibers and Polymers
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    • v.5 no.2
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    • pp.83-88
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    • 2004
  • In order to assess the potential of the hydroxy-containing polyamic acid (PHAA) synthesized from 3,3'-dihydroxy benzidine and pyromellitic dianhydride for a fire-safe polymer, the cyclization pathway of PHAA has been investigated using a model compound prepared from 2-aminophenol and phthalic anhydride. The reaction was monitored. by $^1{H-nuclear}$ magnetic resonance. N-(2-hydroxyphenyl) phthalamic acid is converted to N-(2-hydroxyphenyl) phthalimide at ca. 175$^{\circ}C$, showing endothermic reaction. The imide structure is rearranged to the benzoxazole structure over ca. $400^{\circ}C$. These results are similar with that of PHAA. According to pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) data, water and carbon dioxide are released during the cyclization and rearrangement reaction. One DMAc molecule is complexed with one carboxyl acid group in PHAA, which accelerates the imidization process to release more easily the flame retardant, water.

Analytical Methods of Levoglucosan, a Tracer for Cellulose in Biomass Burning, by Four Different Techniques

  • Bae, Min-Suk;Lee, Ji-Yi;Kim, Yong-Pyo;Oak, Min-Ho;Shin, Ju-Seon;Lee, Kwang-Yul;Lee, Hyun-Hee;Lee, Sun-Young;Kim, Young-Joon
    • Asian Journal of Atmospheric Environment
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    • v.6 no.1
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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.

Study on Qualitative Analysis for Lacquer Mixed with Some Additives by Pyrolysis‐Gas Chromatography/Mass Spectrometry (Py-GC/MS 분석법을 이용한 첨가물 혼합 옻칠 접착제의 정성분석)

  • Kim, Ji Eun;Yu, Ji A;Chung, Yong Jae
    • Journal of Conservation Science
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    • v.33 no.1
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    • pp.51-59
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    • 2017
  • Lacquer has been used as a natural paint or adhesive in Korea since 2nd century B.C. It has been found to have been used as an adhesive as mentioned in old records and as seen in excavated relics, It was also mixed with flour, animal glue, or fish glue to produce lacquer adhesives. Qualitative analysis and evaluation of the applicability of lacquer and additives was performed in this study. The results of EGA analysis for lacquer additives confirmed that the pyrolysis temperature of lacquer, glucose glue, and animal glue. On the basis of this result, raw lacquer sample was checked that pyrolysis product that originated from urushiol side chain (R group). Components originating from glucose and amino acid were detected in glutinous rice paste and animal glue samples. In this study, the optimum pyrolysis temperature for each lacquer and additive mixture was determined from basic qualitative analysis data. By performing the qualitative analysis of each mixture, the applicability of this technique for analyzing real relics was evaluated.

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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Organic Material Analysis of a Lacquered Wooden Sheath of Long Sword with Ring Pommel Excavated in Imdang Ancient Tomb (경산 임당고분 출토 철제 고리자루칼 칠의 유기물 분석)

  • Park, Jongseo;Cho, Ha-nui;Lee, Jae-sung
    • Journal of Conservation Science
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    • v.34 no.5
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    • pp.369-377
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    • 2018
  • In order to examine the constituents and weathered state of a lacquer specimen, analysis of the organic materials was conducted using py/GC/MS(pyrolysis-gas chromatography-mass spectrometry). The samples were obtained from the lacquered wooden sheath of a long ring-pommel sword excavated in the Imdang No.1 ancient tomb constructed around the Proto-Three Kingdoms period. In direct py/GC/MS, the sample and the dried Asian lacquer showed similar chromatograms, while the characteristic compounds of Asian lacquer such as 1,2-dimethoxy-3-pentadecylbenzene were observed in THM(thermally assisted hydrolysis and methylation)-py/GC/MS. In addition, compounds like dimethyl nonanedioate, which presumably originated from drying oil, were also detected. Furthermore, the detection of oxidized catechols in considerable amount indicated that the degradation of lacquer is estimated to result from the oxidation of urushiol. Therefore, it is suggested that the lacquered wooden sheath was prepared using Asian lacquer and drying oil, and that the lacquer layer was considerably oxidized over the long burial time.

Research on Pyrolysis Properties of Waste Plastic Films (폐플라스틱 필름의 열분해특성에 대한 연구)

  • Kim, Young-Min;Lee, Boram;Han, Tae Uk;Kim, Seungdo;Yu, Tae-U;Bang, Byoung Yeol;Kim, Joug-Su;Park, Young-Kwon
    • Applied Chemistry for Engineering
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    • v.28 no.1
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    • pp.23-28
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    • 2017
  • Pyrolysis characteristics of waste plastic films were investigated by using a thermogravimetric analysis and pyrolyzer-gas chromatography/mass spectrometry. Thermogravimetric analysis results revealed that the pyrolysis of waste plastic films can be divided into two distinct reactions; (1) the decomposition reaction of starch at between 200 and $370^{\circ}C$ and (2) that of other plastic polymers such as PS, PP, PE at between 370 and $510^{\circ}C$. The kinetic analysis results obtained by using the revised Ozawa method indicated that the apparent activation energy of the pyrolysis reaction of waste plastic films was also changed dramatically according to the different decomposition reactions of two major waste plastic film components. Py-GC/MS results also revealed that the typical pyrolyzates of each polymer in waste plastic films were levoglucosan (starch), terephthalic acid (PET), styrene monomer, dimer, and trimer (PS), methylated alkenes (PP), and triplet peaks (PE) composed of alkadiene/alkene/alkane. The phthalate, used as a polymer additive, was also detected on the pyrogram of waste plastic films mixture.

Example of Air Exposure Assessment for Fire Extinguishing Agent Residues (소화약제 잔류물질에 대한 공기 중 노출평가 사례)

  • Daesung Lim
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.34 no.1
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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.

Confirming Animal Glue in Dancheong Sample by Pyrolysis/GC/MS (열분해/GC/MS에 의한 재현 단청 시편에서 아교의 확인)

  • Park, Jong Seo;Kim, Mi Jeong;Kim, Soon Kwan
    • Journal of Conservation Science
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    • v.32 no.1
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    • pp.21-32
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    • 2016
  • Animal glue is a traditional material used extensively as adhesive and binder in mother-of-pearl, wooden structure, traditional painting, etc. Analysis of animal glue is usually performed with IR(infrared spectroscopy) based on the IR absorption of functional group. But, it has a limitation in confirming animal glue when a sample consists of several materials because of overlapping of the absorption band. Py/GC/MS(pyrolysis/gas chromatography/mass spectrometry) is a useful tool in analyzing the constituent of polymeric materials like animal glue by identifying their pyrolysate with very small amount of sample. In this study, confirmation of animal glue in a Dancheong sample was tried with this method. Characteristic pyrolytic compounds of animal glue and tung oil used in Dancheong were identified. Dancheong sample painted with Noerok as a coloring material, animal glue and tung oil was prepared and it was possible to find characteristic peaks of animal glue after thermal degradation and artificial weathering experiment. From this, we found that animal glue can be detected using py/GC/MS in cultural heritage samples consisting of several materials and in different condition. IR was also tried to analyze Dancheong sample and the results were compared with those of py/GC/MS for the detection of animal glue.

Effects of Metal Oxide Addition on Co-pyrolysis of PVC and ABS Mixtures (PVC와 ABS 혼합물의 공열분해에 대한 금속산화물의 첨가 효과)

  • Kim, Hee Taik;Choung, Youn Wook;Lee, Hae Pyeong
    • Applied Chemistry for Engineering
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    • v.16 no.2
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    • pp.296-303
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    • 2005
  • The co-pyrolysis characteristics of polyvinylchloride (PVC) and acrylonitrile butadiene styrene (ABS) mixtures with various mixing ratios and effect of addition of CaO and $Cu_2O$ have been studied using thermogravimetry (TG) and gas chromatograph-mass spectrometry (GC-MS). In an isothermal decomposition conducted at $500^{\circ}C$, the yields of styrene monomers and aromatic compounds increased as the mixing ratio of ABS increased, and the yield of BTX compounds reached its maximum (16.14%) when the mixing ratios of PVC and ABS was 4:1. In an isothermal decomposition added with metal oxides, the maximum yield of liquid product was 73% when CaO [CaO/(PVC+ABS)=0.4] was added and it was 70% when $Cu_2O$ [$Cu_2O$/(PVC+ABS)=0.4] was added, respectively, where HCl contained in the gaseous product was completely removed when added with CaO [CaO/(PVC+ABS)=0.5] and $Cu_2O$ [$Cu_2O$/(PVC+ABS)=1.0]. Therefore, to obtain the highest yield of liquid product it appears to be the reaction condition: the reaction temperature of $500^{\circ}C$ and mixing ratios of CaO and $Cu_2O$ are 0.5 and 1.0, respectively.

Analysis of Waterborne Automotive Refinish Paint for Investigating Insurance Fraud (차량 보수도장 보험사기 규명을 위한 수용성 페인트 성분분석)

  • Lee, Joon-Bae;Lee, Cheon-Ho;Ryu, Seung-Jin;Gong, Bokyoung;Kwon, O-Seong;Kim, Myung-Duck;Kim, Nam Yee;Paeng, Ki Jung
    • Applied Chemistry for Engineering
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    • v.28 no.4
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    • pp.490-494
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    • 2017
  • With increasing the number of vehicles, the accident rate also goes up and the damaged vehicles should be painted as a final repair process. At the painting stage the solvent-based paint causes environmental problems. To overcome these problems waterborne refinish paint is frequently used recently. However, for waterborne refinish, the costs of insurance coverage are too expensive, and insurance reimbursement costs could be burdensome. Because of the high price of aquatic paint treatment, the service shop might charge the malicious service price. In this study, the surfactant of Surfynol 104, which is the component in the paint, was used as an indicator whether the vehicle was painted with waterborne paint. The specimen was quantitatively analyzed to contain 0.38% of the surfactant through the standard addition method with isotope substituted internal standard (IS) of fluranthene-d10 by curie point pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS).