• Title/Summary/Keyword: 열분해/GC/MS

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Characterization of Degradation features and Degradative Products of Poplar Wood(Populus alba${\times}$glandulosa) by Flow Type-Supercritical Water Treatment (초임계수에 의한 현사시 목분의 분해특성 및 분해산물 분석)

  • Choi Joon-Weon;Lim Hyun-Jin;Han Kyu Sung;Kang Ha-Young;Choi Don-Ha
    • Journal of Korea Foresty Energy
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    • v.24 no.1
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    • pp.39-46
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    • 2005
  • In this study, the possibility of sugar conversion of poplar wood(Populus $alba{\times}rglandulosa$) and their degradation features of major wood components were characterized using flow type supercritical water treatment system. The finely ground poplar wood meals were treated for 2min. under subcritical condition$(23MPa,\;275^{\circ}C\;and\;325^{\circ}C)$ and supercritical condition $(23MPa,\;375^{\circ}C\;and\;415^{\circ}C)$. respectively. The degradation products of poplar wood meals appeared brownish colors, including undegraded solids. Increasing the temperature of the system, the degradation rate of poplar wood meals was accelerated and reached up to $94\%\;at\;375^{\circ}C$. The total amount of reducing sugars in degradation products determined by DNS method were gradually lowered when the temperature condition became severe. This indicated that the reducing sugars formed were further degraded to kan derivatives by certain side reaction such as pyrolysis under higher temperature. In order to characterize degradation features of lignin, the degradation products were extracted with ethylacetate and the organic phases were subjected to GC-MS analysis. Main lignin degradation products were identified to vanillin, guaiacol, syrinaldehyde, 4-prophenyl syringol and dihydrosinapyl alcohol, which could be formed by the cleavage of ether linkages in lignin polymers by high temperature condition.

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Instrumental Analysis of Deposits on Paper Machine and Holes/Spots in Paper (제지공정 침착이물질 및 종이내 불순물 성분의 기기분석)

  • Ma, Geum-Ja;Lee, Bok-Jin
    • Applied Chemistry for Engineering
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    • v.9 no.1
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    • pp.135-140
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    • 1998
  • The constituents of deposits on paper machine and holes/spots in paper have been analyzed by a combination of analytical techniques, such as FTIR, Py-GC-MS, and EDS. FTIR spectroscopy was used prior to Py-GC-MS and EDS analysis, as a preliminary analysis. The analysis of organic components was carried out with a pyrolysis unit connected to a GC-MS, and inorganic components in ash were analyzed by SEM equipped with an EDS analyzer after pyrolysis at $590^{\circ}C$. The deposits on the dryer section were complex pitch, which was the mixture of the organic components of fatty acid ester and starch, and the inorganic components of talc, clay, and calcium carbonate. The complex pitch was estimated to come from the coated broke. We knew the deposits on the metering rod of sym-sizer were associated with the interaction of unstable alkyl keten dimer(AKD) and $CaCO_3$. The compositions of holes or spots varied considerably and were associated with chemical interaction within the system. The holes, spots, and blotches in the finished paper were PE and PP from pulp sources, complex pitch that were caused by the interaction of the different additives in the system, polymer such as flexible PVC that was used for the prop of palette, and hot melt as adhesives that came from the inadequate handling of broke. In addition, we identified that poly(caprolactam) which is used for forming fabrics or press felts, could be mixed with the raw materials by accident and results in streaks on coating.

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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.

A STUDY ON THE PYROLYSIS OF VANILLIN - IDENTIFICATION OF VANILLIN PYROLYTIC PRODUCTS AT $800^{\circ}C$ - (바니린의 열분해에 관한 연구 - $800^{\circ}C$에서 바니린의 열분해 생성물의 확인을 중심으로 -)

  • Kwag, Jae-Jin;Kim, Ok-Chan;Park, Tae-Moo
    • Journal of the Korean Society of Tobacco Science
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    • v.6 no.2
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    • pp.131-139
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    • 1984
  • The pyrolytic behavior of vanillin, a flavorant for manufactured cigarettes, was examined to find its contribution to the smoke composition. Vanillin was pyrolyzed at various temperatures (500-$900^{\circ}C$) in a stream of nitrogen. Pyrolytic products at $800^{\circ}C$ were identified with GC/MS. As increasing temperature, pyrolytic products did not appear with qualitative differences. Component analysis of the resulting products showed that 24 compounds were identified. and phenolic compounds were major products. The pyrolytic pathway of vanillin was also discussed.

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A Study on Catalytic Pyrolysis of Polypropylene with Ni/sand (Ni/sand를 이용한 폴리프로필렌 촉매 열분해 연구)

  • Kim, Soo Hyun;Lee, Roosse;Sohn, Jung Min
    • Clean Technology
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    • v.27 no.3
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    • pp.232-239
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    • 2021
  • In order to develop a novel system named "thermal medium and gas circulation type pyrolysis system," this study was conducted to obtain basic data for process simulation before performing the pyrolysis experiment. Polypropylene (PP) was chosen as model material in the basic pyrolysis experiment instead of waste plastic and fluidized sand (hereinafter referred to as "sand"), and it was used as a heat transfer material in the "thermal medium and gas circulation type pyrolysis system." Ni was impregnated as an active catalyst on the sand to promote catalytic pyrolysis. The basic physical properties of PP were analyzed using a thermogravimetric analyzer, and pyrolysis was performed at 600 ℃ in an N2 atmosphere to produce liquid oil. The distribution of the carbon number of the liquid oil generated through the catalytic pyrolysis reaction was analyzed using GC/MS. We investigated the effects of varying the pyrolysis space velocity and catalyst amount on the yield of liquid oil and the carbon number distribution of the liquid oil. Using Ni/sand, the yield of liquid oil was increased except with the pyrolysis condition of 10 wt% Ni/sand at a space velocity of 30,000 h-1, and the composition of C6 ~ C12 hydrocarbons increased. With increases in the space velocity, higher yields of liquid oil were obtained, but the composition of C6 ~ C12 hydrocarbons was reduced. With 1 wt% Ni/sand, the oil yield obtained was greater than that obtained with 10 wt% Ni/sand. In summary, when 1 wt% Ni/sand was used at a space velocity of 10,000 h-1, the oil yield was 60.99 wt% and the composition of C6 ~ C12 hydrocarbons was highest at 42.06 area%.

Upgrading of Quercus mongollica bio-oil by esterification (에스터화 반응을 이용한 신갈나무 바이오오일 품질 개선)

  • Chea, Kwang-Seok;Lee, Hyung-Won;Jeong, Han-Seob;Lee, Jae-Jung;Ju, Young-Min;Lee, Soo-Min
    • Journal of the Korean Applied Science and Technology
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    • v.35 no.4
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    • pp.975-984
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    • 2018
  • Fast pyrolysis bio-oil has unfavorable properties that restrict its use in many applications. Among the main issues are high acidity, instability, and water and oxygen content, which give rise to corrosiveness, polymerization during storage, and a low heating value. Esterification and azeotropic water removal can improve all of these properties. A 500 g of Quercus mongollica which grounded 0.8~1.4 mm was processed into bio-oil via fast pyrolysis for 2 seconds at $550^{\circ}C$. The esterification consists of treating pyrolysis oil with a high boiling alcohol like n-butanol at $70^{\circ}C$ under reduced pressure (100 hPa). All products are analyzed for water mass fraction, viscosity, higher heating value, pH, FT-IR and GC/MS. The water mass fraction can be reduced by 91.4 % (from 31.5 % to below 2.7 %), the viscosity by 65.8 % (from 36.5 to 12.5 cP) and the higher heating value can be increased by 96.8 % (from 3,918 to 7,712 kcal/kg), the pH by 1.3 (from 2.7 to 4.0). FT-IR and GC/MS analysis indicated that labile acids, aldehydes, ketones and lower alcohols were transformed to stable target products. Using this approach, the water content of the pyrolysis oil is reduced significantly. These improvements should allow the utilization of upgraded pyrolysis liquids in standard boilers and as fuel in CHP (Combined heat and power) plants.

Observation of Interfacial Adhesion in Silica-NR Compound by Using Bifunctional Silane Coupling Agent (양기능성 커플링제 실란에 의한 실리카-천연고무 복합소재의 계면간 결합 고찰)

  • Lee, Jong-Young;Kim, Sung Min;Kim, Kwang-Jea
    • Polymer(Korea)
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    • v.39 no.2
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    • pp.240-246
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    • 2015
  • Formation of a strong 3-dimensional interfacial network structure via chemical reaction between hydroxyl group on silica surface and NR chain by the addition of bis(triethoxysilylpropyl)tetrasulfide (TESPT) into silica-filled NR compound was observed by using Py-GC/MS and SEM. Addition of TESPT into silica-filled NR compound decreased scorch time ($t_{10}$) due to increased sulfur content, and reduced cure rate index (CRI) via continuous reaction between sulfur atoms in TESPT, which acted as a sulfur donor, and activators and/or accelerators. Addition of TESPT in the compound improved processability and mechanical properties of the compound. Overall, we observed that the addition of TESPT into the silica-filled NR compound formed a silica-TESPT-NR network, and thus the degree of crosslinking was increased resulting in improved mechanical properties.

Component Analysis of Softwood Vinegar (침엽수 목초액의 성분분석)

  • ;;;Sano Yoshihiro
    • Journal of Korea Foresty Energy
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    • v.20 no.1
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    • pp.28-34
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    • 2001
  • To analyze chemical compositions of softwood vinegar prepared with continuous carbonized kiln, the chemical compositions were analyzed by GC-MS spectrometry. The results were summarized as follow : 1. The amounts of methylalcohol and acetic acid and of vinegar were 0.12% and 0.8% respectively, and acidity was 0.85 2. Perfume components of vinegar were frufual, 5-meayl-2-furancarboxyaldehyde, 2,3-pentanedione, 2-butanol, 2,3-dihydrofuran, 1-(2-furanyl)-etanone, benzaldehyde, 2-furan carboxyaldehyde and acetic acid. 3 Vinegar prepared from softwood, so that murk amount of guaiacyl compound and phenol derivetives are produced from lignin and extractives was analγzed. 4 The yield of 4-methyl-di-tert-butylphenol was the highest in the nutural and carbonyl and acetic acid in the acid fractions, 3-ethylpentane in the basic fraction, and guaiacol in the phenolic fraction.

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Preparation of Liquefied Cellulose and Analysis of Its Components by GC-MS Spectrometry (액화셀룰로오스의 제조 및 GC-MS에 의한 그 성분 분석)

  • 조국란;황병호;공영토;도금현
    • Journal of Korea Foresty Energy
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    • v.19 no.2
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    • pp.86-92
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    • 2000
  • The liquefactions of $\alpha$-cellulose(Sigma Chemical, C-8002, 47H0383) was prepared in the presence of phenol using sulfuric acid as a catalyst under $N_2$ gas protection at $180^{\circ}C$ for 60minutes to examine its components. The ratio of $\alpha$-cellulose to phenol was 1: 6.2(w/w), and that to sulfuric acid was 1: 0.05(g/$m\ell$). The yields of liquefaction were calculated after the liquefied mixtures were passed through 1G4 glass filter. The luquefied product of $\alpha$-cellulose was analyzed using GC-MS Spectormeter. The 12 compounds identified by GC-MS Spectrometer, of which peak area covers 54% as 2,4-dimethyl phenol, p-isopropyl phenol, 1-ethyl-3,5-dimethyl benzene, o-isopropyl phenol, (E)-2,4\` dihydroxy-stilbene, 2,2\`-methylene-bisphenol, 4,4\`-methylenebisphenol, 3-methyl-2-hydroxyphenyl-(E)-2-hydroxyl-4\`-methoxy-stilbene, 1-phyenyl-1-(4\`hydroxyphenyl)methanol phenol derivatives. From this results, the reaction pathways of the liquefaction of cellulose were proposed through electrophilic substitution reaction. Phenol as a solvent might react with the reaction intermediates as well in the cellulose liquefaction.

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Direct Analysis of Organic Additives in Cured Rubber by Pyrolysis-Gas Chromatography/Mass Spectrometry (열분해-가스크로마토그래피/질량분석법에 의한 가황고무중의 유기첨가제의 직접분석)

  • Kim, Seung Wook;Heo, Gwi Suk;Lee, Gae Ho
    • Journal of the Korean Chemical Society
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    • v.41 no.10
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    • pp.524-534
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    • 1997
  • Analysis of additives in cured rubber is often a difficult task for analytical chemists because of a wide variety of complex components. Conventional analyses of additives and rubbers have been done in multistep, off-line processes with large sample size and extensive sample preparations. The coumarone-indene resin, resorcinol-formaldehyde resin, and prevulcanization inhibitor have been characterized by their pyrolysis pathways and mass spectra of characteristic pyrolyzates. Pyrolysis Gas Chromatography/Mass Spectrometry (Py-GC/MS) was used in the identification of additives without any sample pretreatment. This result shows that several organic additives in cured rubber can be directly analyzed.

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