• Title/Summary/Keyword: thermal degradation products

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Characterization of Thermal Products of Alpha-Tocopherol

  • Chung, Hee-Young
    • Preventive Nutrition and Food Science
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    • v.9 no.4
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    • pp.295-299
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    • 2004
  • Alpha-tocopherol was thermally oxidized and degraded at high temperatures and the resulting products were chromatographically separated and identified by LC-MS. Alpha-tocopherol dissolved in glycerol was heated at 200^{\circ}C for 30 min. The thermal products were separated by hexane extraction and analyzed by HPLC using a reversed phase $\mu$-Bondapak $C_{18}-column$ with two kinds of elution solvents: a mixture of acetonitrile and methanol (3:2), and of acetonitrile, methanol, 2-propanol, chloroform and methylene chloride (3:2:5:0.5:0.5) in a gradient mode. The isolated thermal. products of alpha-tocopherol were more viscous than alpha-tocopherol, and dark brown in color. Major thermal degradation products of alpha-tocopherol were identified by LC-MS, and the structures of thermal products were proposed. Alpha-tocopherol and its thermal degradation products were degraded into fragments, mainly at the non-aromatic parts. The degradation products of alpha-tocopherol. were combined with oxidized product (tocopherylquinone) to make thermal. products through dimerization.

Kinetics of Thermal Degradation of Polypropylene/Nanoclay/Wood Flour Nanocomposites

  • Mohan, D. Jagan;Lee, Sun-Young;Kang, In-Aeh;Doh, Geum-Hyun;Park, Byung-Dae;Wu, Qinglin
    • Journal of the Korean Applied Science and Technology
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    • v.24 no.3
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    • pp.278-286
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    • 2007
  • As a part of enhancing the performance of wood-plastic composites (WPC), polypropylene (PP)/ nanoclay (NC)/ wood flour (WF) nanocomposites were prepared using melt blending and injection molding process to evaluate their thermal stability. Thermogravimetric analysis (TGA) was employed to investigate thermal degradation kinetics of the nanocomposites both dynamic and isothermal conditions. Dynamic scans of the TGA showed an increased thermal stability of the nanocomposites at moderate wood flour concentrations (up to 20 phr, percentage based on hundred percent resin) while it decreased with the addition of 30 phr wood flour. The activation energy $(E_a)$ of thermal degradation of nanocomposites increased when nanoclay was added and the concentration of wood flour increased. Different equations were used to evaluate isothermal degradation kinetics using the rate of thermal degradation of the composites, expressed as weight loss (%) from their isothermal TGA curves. Degradation occurred at faster rate in the initial stages of about 60 min., and then proceeded in a gradual manner. However, nanocomposites with wood flour of 30 phr heated at $300^{\circ}C$ showed a drastic difference in their degradation behavior, and reached almost a complete decomposition after 40 min. of the isothermal heating. The degree of decomposition was greater at higher temperatures, and the residual weight of isothermal degradation of nanocomposites greatly varied from about 10 to 90%, depending on isothermal temperatures. The isothermal degradation of nanocomposites also increased their thermal stability with the addition of 1 phr nanoclay and of wood flour up to 20 phr. But, the degradation of PP100/NC1/MAPP3/WF30 nanocomposites with 30 phr wood flour occurs at a faster rate compared to those of the others, indicating a decrease in their thermal stability.

Characterization of Thermal Degradation of Polytrimethylene Terephthalate by MALDI-TOF Mass Spectrometry

  • Jang, Sung-Woo;Yang, Eun-Kyung;Jin, Sung-Il;Cho, Young-Dal;Choe, Eun-Kyung;Park, Chan-Ryang
    • Bulletin of the Korean Chemical Society
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    • v.33 no.3
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    • pp.833-838
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    • 2012
  • The thermal degradation products of polytrimethylene terephthalate (PTT) obtained by heating the sample in the temperature range of $250-360^{\circ}C$ under non-oxidative conditions was characterized using MALDI-TOF (matrix assisted laser desorption/ionization) mass spectrometry. The structures of the degradation products were determined and the relative compositions were estimated. The MALDI-TOF mass spectra of the thermally degraded PTT sample showed three main series of oligomer products with different end groups, which were carboxyl/carboxyl, carboxyl/allyl, and allyl/allyl. In contrast to the thermal degradation of polyethylene terephthalate (PET), the oligomers containing terephthalic anhydrides were not detected, whereas the formation of oligomers containing the unsaturated allyl ester group was confirmed by mass assignment. From these results, it was concluded that the thermal degradation of PTT proceeds exclusively through the ${\beta}$-CH hydrogen transfer mechanism, which is in accordance with the proposed reaction mechanism for the thermal degradation of polybutylene terephthalate (PBT).

Formation Kinetic Study of Thermal Products of Tocopherols

  • Chung, Hae-Young
    • Preventive Nutrition and Food Science
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    • v.12 no.3
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    • pp.131-134
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    • 2007
  • The kinetic analyses for thermal products of alpha-, gamma- and delta-tocopherols during heating as functions of temperature and time were studied. Alpha-, gamma- and delta-tocopherols dissolved in glycerol were heated at $100{\sim}200^{\circ}C$ for $5{\sim}60$ min. The thermal products were separated by hexane extraction and analyzed by HPLC using a reversed phase ${\mu}-Bondapak$ $C_{18}-column$ with two kinds of elution solvents in a gradient mode. The formation kinetics of thermal products of tocopherols followed a first-order kinetic model. The formation rate of thermal products of tocopherols was dependent on heating temperatures and heating times. The activation energy and enthalpy for the thermal products of ${\gamma}-and$ ${\delta}-tocopherols$ were higher than those for ${\alpha}-tocopherol$ as in the case of the oxidative degradation kinetics of tocopherol. The magnitude order of the activation energy was ${\gamma}->{\delta}->{\alpha}-tocopherol$.

Thermal Degradation of Aqueous MEA Solution for CO2 Absorption by Nuclear Magnetics Resonance (핵자기공명분석법을 이용한 수용성 아민 CO2 흡수제인 MEA의 열적변성 분석)

  • CHOI, JEONGHO;YOON, YEOIL;PARK, SUNGYOUL;BAEK, ILHYUN;KIM, YOUNGEUN;NAM, SUNGCHAN
    • Transactions of the Korean hydrogen and new energy society
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    • v.27 no.5
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    • pp.562-570
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    • 2016
  • At the carbon dioxide capture process using the aqueous amine solution, degradation of absorbents is main factor to reducing the process performance. Also, degradation mechanism of absorbent is important for understanding the environmental risk, route of degradation products, health risk etc. In this study, the degradation products of MEA were studied to clarify mechanism in thermal degradation process. The degradation products were analyzed using a $^1H$ NMR (nuclear magnetic resonance) and $^{13}C$ NMR. The analysis methods used in this study provide guidelines that could be used to develop a degradation inhibitor of absorbent and a corrosion inhibitor.

Thermal Degradation Pattern of Tocopherols on Heating without Oxygen in a Model Food System (모델식품계에서 무산소 가열시 토코페롤의 열분해 패턴)

  • 정혜영
    • The Korean Journal of Food And Nutrition
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    • v.11 no.6
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    • pp.635-639
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    • 1998
  • The thermal degradation pattern of $\alpha$-, ${\gamma}$-and $\delta$-tocopherols in glycerol was investigated during heating at 100~25$0^{\circ}C$ for 5-60 min in the absence of oxyge. The tocopherols and thermally decomposed products were separated by HPLC with a reversed phase $\mu$-Bondapak C18-column. The degradation pattern of $\alpha$-tocopherol during the heating in the absence of oxygen was different from those of ${\gamma}$-and $\delta$-tocopherols. But the degradation patterns of ${\gamma}$-and $\delta$-tocopherols were similar to each other. The residual content of $\alpha$-tocopherol during the heating in the absence of oxygen decreased to the range 12~65% and those of ${\gamma}$-and $\delta$-tocopherols decreased to the range 4~96%. The thermal degradation of tocopherols in the absence of oxygen was less than that in the presence of oxygen.

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Studies on Polyacrylonitrile (2) Thermal Degradation of Polyacrylonitrile (폴리아크릴로니트릴에 關한 硏究 (第 2 報) 폴리아크릴로니트릴의 熱分解에 關하여)

  • ICK SAM NOH
    • Journal of the Korean Chemical Society
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    • v.11 no.2
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    • pp.70-76
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    • 1967
  • Structural changes attending polyacrylonitrile(PAN) upon heating and treating with nucleophilic reagents have been studied for some time and a few authors have studied on the thermal degradation, particularly on the characterization of degradation products in PAN. It is the purpose of this paper to report the kinetic study on the thermal degradation above $250^{\circ}C$ and make some suggestions as to the degradation process and mechanism in PAN. The degradation process in PAN is considered that three reactions are combined in two steps. Random chain scission accompanying the naphthylidine-type ring formation is the first step and the degradation of naphthylidine-type ring occurred as the next step. The reactions in the first step are competitive so that the maximum weight loss on pyrolysis of PAN, under such a condition that the degradation of naphthylidine-type ring is negligible, is depended on the relative reaction rate of these two competitive reactions.

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Thermal Stability of Polypropylene-Based Wood Plastic Composites by The Addition of Ammonium Polyphosphate (폴리인산염 첨가에 의한 폴리프로필렌 기반의 Wood Plastic Composites 열안정성)

  • Chun, Sang-Jin;Lee, Sun-Young
    • Journal of the Korean Wood Science and Technology
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    • v.42 no.6
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    • pp.682-690
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    • 2014
  • In order to improve the thermal stability of wood plastic composites (WPC), thermal degradation behavior of WPC in this study was investigated by the addition of wood flour and fire retardant after hybridization of wood flour and ammonium polyphosphate (APP) into polypropylene (PP) matrix. Thermal degradation behavior of all formulations was analyzed with thermogravimetric analyzer under nitrogen environment at heating rate of $10^{\circ}C/min$. As the thermal degradation temperature of wood flour is lower than that of PP, char layer formed by the wood flour decreases the speed of heat transfer to PP. In addition, the char layer increases the 2nd thermal degradation temperature and decreases the 2nd thermal degradation speed. The WPC treated with APP increases the 1st and 2nd degradation temperatures. In the case of WPC with high loading level of wood flour, the 1st thermal degradation temperature and 2nd thermal degradation rate were increased by the addition of APP, and then the amount of remnants at high temperature was increased by the increase of the APP loading level. In the case of WPC treated with APP, the amount of the remnants at high temperature was increased with the increase of wood flour content from 10 wt% to 50 wt%, indicating that char formation of the APP and wood flour occurred at the same time, resulting in high thermal stability effect by the increase of wood flour content.

GC-MS Analysis of Amur Cork Tree Extract and Its Degradation Products

  • Ahn, Cheun-Soon
    • Journal of the Korean Society of Clothing and Textiles
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    • v.34 no.6
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    • pp.1042-1052
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    • 2010
  • The Degradation of amur cork tree extract is investigated by GC-MS after treating the dye with three thermal degradation systems of, room temperature (RT), $4^{\circ}C$ refrigeration (LT), $100^{\circ}C$ oven (OV), and $H_2O_2$/UV/$O_2$ (PER) degradation system for 0-24 days. It was found that PER degradation system represented the highest intensity of degradation treatment followed by OV treatment among the four degradation parameters. The possible fingerprint products of amur cork tree dye, that yielded 68% (or higher) reliability in the NIST spectral match, were isobenzofuran-1,3-dione,4,5-dimethoxy- (8.37 min, PER only), 1,3-dioxolo[4,5-g]isoquinolin-5(6H)-one,7,8-dihydro (9.41 min, PER only), canthine-6-one (10.24 min, RT, LT, OV only), and dihydroberberine (15.05 min, RT, LT, OV, PER) in the order of higher to lower possibility of detection. Unknown products 7 (13.43 min) and 8 (16.35 min) are two other possible fingerprint products of amur cork tree dye that require future identification.

Effect of Reaction Temperature Program on Thermal Degradation of Low-quality Pyrolytic Oil for Bench-scale Continuous Reaction System (벤치 규모 연속반응시스템에서 저급 열분해유 분해반응에 대한 반응온도 프로그램의 영향)

  • Lee, Kyong-Hwan;Nam, Ki-Yun
    • Clean Technology
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    • v.15 no.3
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    • pp.186-193
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    • 2009
  • The characteristics of product materials obtained from thermal degradation of low-qualify pyrolytic oil were investigated in this study. The reactants were produced by pyrolysis of mixed plastic waste with film type in a commercial rotary kiln reaction system. The properties of reactants were measured by elemental analysis, calorimetry analysis and SIMDIST analyst. The result of degradation experiments with different reaction temperature programs was discussed through product yields, cumulative yields and production rates of oil products. The multi-step reaction temperature program resulted in higher yields of product oils and lower yields of residues than one-step reaction temperature program. The product characteristics such as production yield and the rate of oil products etc. were influenced by reaction temperature program in the continuous thermal degradation.