• Title/Summary/Keyword: Differential scanning calorimetry (DSC)

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Thermal and Mineralogical Characterization of Ca-Montmorillonite from Gampo Area (감포지역(甘浦地域) Ca-몬모릴로나이트의 열적(熱的) 및 광물학적(鑛物學的) 특성(特性))

  • Moon, Hi-Soo;Choi, Sun Kyung;Kim, Moon Young
    • Economic and Environmental Geology
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    • v.21 no.2
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    • pp.175-184
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    • 1988
  • Ten under 2 micron size fractions of the montmorillonite from Yongdongri area, Gyeongsangbug-Do were studied using X-ray powder diffraction, cation exchange measurement, differential thermal analysis, thermogravimetric analysis, differential thermal scanning calorimetry and chemical analysis. Montmorillonites occurring at same deposit show limited variation in chemical composition whereas in thermal properties they do not. Their dehydroxylation endothermic peaks are "abnormal" type with a small range of variation of peak temperature reflecting tetrahedral substitution of Al for Si. Data from DSC show that divalent-cation saturated montmorillonite has relatively a higher endothermic heat capacity than monovalent-cation saturated montmorillonite, indicating that cations with higher electronegativity hold more water molecules.

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Thermotropic Polyurethanes Prepared from Diisocyanates and 4,4'-Bis(3-hydroxypropoxy)Biphenyl Containing Mesogenic Unit (4,4'-Bis(3-hydroxypropoxy)Biphenyl와 Diisocyanate 에 의한 열방성 액정폴리우레탄 합성)

  • Lee, Jong Baek
    • Korean Chemical Engineering Research
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    • v.48 no.5
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    • pp.615-620
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    • 2010
  • In this study, five series of novel polyurethanes was synthesized by the polyaddition reaction of diisocyanates such as 2,6-tolylene diisocyanate(2,6-TDI), 2,5-tolylene diisocyanate(2,5-TDI), 2,4-tolylene diisocyanate(2,4-TDI), and 1,4-phenylene diisocyanate(1,4-PDI), hexamethylene diisocyanate(HDI) with 4,4'-Bis(3-hydroxypropoxy)biphenyl (BP3), 4,4'-bis(3-hydroxypropoxy)biphenyl exhibited a smectic type mesophase. Monotropic mesophase was found for all synthesized liquid crystalline polyurethanes except HDI/BP3. In contrast, 1,4-PDI/BP3 without a methyl substituent in the phenylene unit exhibited no explicit mesomorphic behavior, which was confirmed by DSC and polarizing microscopy experiments. Structures of the compound were identified by FT-IR and $^1H$-NMR spectroscopies. Their phase transition temperatures and thermal stability were also investigated by differential scanning calorimetry(DSC), polarized optical microscopy(POM) and x-ray diffraction analysis.

Effect of Trehalose on Stabilization of Cellular Components and Critical Targets Against Heat Shock in Saccharomyces cerevisiae KNU5377

  • PAIK SANG-KYOO;YUN HAE-SUN;IWAHASHI HITOSHI;OBUCHI KAORU;JIN INGNYOL
    • Journal of Microbiology and Biotechnology
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    • v.15 no.5
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    • pp.965-970
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    • 2005
  • In our previous study [14], we found that heat-shock exposure did not stimulate the neutral trehalase activity in Sacchromyces cerevisiae KNU5377, but did in ATCC24858. Consequently, the trehalose content in KNU5377 became 2.6 times higher than that in ATCC24858. Because trehalose has been shown to stabilize the structure and function of some macromolecules, the present work was focused to elucidate the relationship between trehalose content of these strains and thermal stabilities of whole cells, through differential scanning calorimetry (DSC), and to predict critical targets calculated from the hyperthermic cell killing rates. These analyses showed that the prominent DSC transition of both strains gave identical $T_m$ (transition temperature) values in exponentially growing cells, and that the $T_m$ values of critical targets was about $3^{\circ}C$ higher in KNU5377 than in ATCC24858. Both heat-shocked KNU5377 and ATCC24858 cells displayed similar shifts in their DSC transition profiles. On the other hand, the $T_m$ value of the critical target of KNU5377 was decreased by $2.1^{\circ}C$, which was still higher than ATCC24858 showing no changes. In view of these results, the intrinsic thermotolerance of KNU5377 did not appear to result from the stability of entire cellular components, but rather possibly from that of particular macromolecules, including critical targets, even though it should be investigated in more details. Although the trehalose levels in heat-shocked cells are significantly different, as described in our previous study [14], the overall pattern of thermal stabilities and their predicted critical targets in two heat-shocked strains seemed to be identical. These data suggest that the trehalose levels examined before and after heat shock of exponentially growing cells are not closely correlated with the stabilities of whole cells and/or critical targets in both yeast strains.

Rheological Properties During Mixing and Thermal Properties of Polypropylene/Natural Fiber Composites: II. Effects of A Compatibilizer (폴리프로필렌-천연섬유 복합재료의 혼합시 유변학적 및 열적 특성: II. 상용화제의 영향)

  • Kim, Sam-Jung;Yoo, Chong Sun;Ha, Chang-Sik
    • Journal of Adhesion and Interface
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    • v.10 no.1
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    • pp.23-29
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    • 2009
  • We investigated effects of a compatibilizer on the rheological properties during mixing and thermal properties of polypropylene (PP)-natural fiber composites. Two types of natural fibers (cotton fiber and wood fiber) were compared. maleic anhydride grafted PP was used for a compatibilizer. On increasing the amounts of the compatibilizer, the torque values of composites were increased, regardless of the kind of fibers. X-ray diffraction (XRD) and differential scanning calorimetry (DSC) results showed a slight increase in the degree of crystallinity with adding the compaibilizing agent, while the effects of the kind of fibers were marginal. It may be considered, however, the cotton fiber exhibits better interaction with PP-g-MAH than the natural fiber based on the rheographs, DSC, and XRD results.

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Accurate Measurement of the Thermal Conductivity of Electronic Materials Using the Flash Method (섬광법을 이용한 전자재료의 열전도율 정밀측정)

  • Kim, Seog-Kwang
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2008.11a
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    • pp.9-9
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    • 2008
  • 일반적으로 섬광법으로 열전도율을 구하기 위해서는 섬광법으로 열확산계수를 측정하고, 시차주사열량계(Differential Scanning Calorimetry, DSC)로 비열측정을 하며 아르키메데스의 원리를 이용한 용적밀도를 구하여 이들 각각의 값을 사용하여 열전도율을 얻는다. 따라서 열전도율을 정밀하게 측정하기 위해서는 이 세 가지 물성치를 측정할 때 수반되는 오차요인을 종합적으로 검토하여 개선하는 것이 매우 중요하다. 섬광법으로 열확산계수를 측정할 때 시료의 전면에 조사되는 빛의 흡수율을 향상시키고 배면에서의 온도상승의 감지를 증대할 목적으로 시료 양면에 흑연코팅을 하게 된다. 이때 코팅된 흑연이 시료에 부가적으로 열저항을 증가시켜서 열확산계수를 측정하는데 가장 큰 오차요인이 되고 있다. 한편 비열은 대부분 DSC로 측정하는데, 시료와 용기의 열접촉 정도에 따라 큰 오차요인이 되기도 한다. 본 연구에서는 열확산계수를 정밀하게 측정하기 위해서 시료에 부가적인 열저항으로 작용하는 흑연코팅의 두께와 시료배면에서의 온도상승곡선 간의 상관관계를 실험식으로 도출하였으며 이방법은 열확산계수를 정밀하게 측정하는데 매우 유효한 방법임이 입증되었다. 또한 DSC의 접촉에서의 문제점을 해결하기 위해서 시료배면에서의 무차원 시간축(t/$t_{max}$)을 도입하였으며. 무차원 시간축에 따른 온도상승 곡선에서 표준시료와 측정시료의 half time($t_{1/2}$)의 0.5 배와 1.5배 사이 구간을 적분한 뒤 비교하여 열량계산으로부터 비열을 구하는 방법을 새롭게 개발하였으며 기존의 DSC에 비하여 정밀도를 향상시킬 수 있었다. 결론적으로 새롭게 제안된 측정기법들은 열확산계수 및 비열 혹정 시의 근본적인 오차요인을 혁신적으로 해결함으로써 정밀하고 신뢰성 있는 열전도율을 측정할 수 있음을 입증할 수 있었다.

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Comparison of Physicochemical Properties of Legume Starches (두류전분의 이화학적 특성 비교)

  • Kweon, Mee-Ra;Ahn, Seung-Yo
    • Korean Journal of Food Science and Technology
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    • v.25 no.4
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    • pp.334-339
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    • 1993
  • Physicochemical properties such as amylose content, swelling power, gelatinization and DSC of legume starches were investigated. The granule shape of legume starches was oval. The size of cowpea and mung bean were smaller than kidney bean and red bean. The amylose content of mung bean and kidney bean was larger and were $25{\sim}29%$. Swelling power of kidney bean starch was much lower than other starches in all temperature range. In gelatinization temperature by Brabender amylogram, red bean starch was low, but kidney bean starch was rather high. Amylographic hot-paste viscosity and set back of cow pea, mung bean and red bean starches were high. But those of kidney bean starch were very low. DSC results Indicated kidney bean starch gelatinized in higher temperature. From above results, row pea and mung bean starches were similar in granule size and shape, solubility and swelling power, amylogram, and DSC thermogram. But kidney bean starch was very different and red bean starch was slightly different with the physicochemical properties of cow pea and mung bean starches.

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Retrogradation Characteristics of Jeungpyun by Different Milling Method of Rice Flour (쌀가루의 제분방법에 따른 증편의 노화도 특성)

  • Kim, Young-In;Kum, Jun-Seok;Lee, Sang-Hyo;Lee, Hyun-Yu
    • Korean Journal of Food Science and Technology
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    • v.27 no.6
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    • pp.834-838
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    • 1995
  • The relative retrogradation of Jeungpyun investigated with different milling methods of rice flour. The relative retrogradation of Jeungpyun was reduced in order that of W-C, W-P, D-M, D-J in DSC(Differential Scanning Calorimetry) method while W-C, D-M, D-J, W-P in Diastase method. In wet milling method, the relative retrogradation of Jeungpyun by pin mill (W-P) was lower than Jeungpyun by colloid mill (W-C). In dry milling method, the relative retrogration of Jeungpyun by jet mill (D-J) was lower than Jeungpyun by micro mill(D-M). The relative retrogradation of Jeungpyun by DSC method was similar to the diastase method. The relative retrogradation of Jeungpyun was decreased with decreasing particle size and setback value for amylogram and increasing damaged starch.

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Study on Cure Behavior of Low Temperature and Fast Cure Epoxy with Mercaptan Hardener (Mercaptan 경화제에 의한 저온속경화 에폭시의 경화거동에 관한 연구)

  • Eom, Se Yeon;Seo, Sang Bum;Lee, Kee Yoon
    • Polymer(Korea)
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    • v.37 no.2
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    • pp.240-248
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    • 2013
  • The curing behaviors of diglycidyl ether of bisphenol A (DGEBA) with mercaptan hardener were studied by the comparison with amine-adduct type hardener. Curing behaviors were evaluated by DSC at dynamic and isothermal conditions. In the DSC, the dynamic experiments were based on the method of Kissinger's equation, and the isothermal experiments were fitted to the Kamal's kinetic model. Activation energy of epoxy/amine-adduct type hardener was ca. 40 kcal/mol. As the functional group of mercaptan hardener, -SH increased, on epoxy/mercaptan hardeners, the activation energies decreased from 28 to 19 kcal/mol. Epoxy/amine-adduct type hardener was initiated at $90^{\circ}C$ or higher. However, epoxy/mercaptan hardeners reduced the initiation temperatures below $80^{\circ}C$ and shortened the durations of curing reaction within 10 min. We found out that the reaction kinetics of epoxy with mercaptan hardener followed the autocatalytic reaction models, and the maximum reaction rates were shown at the conversions of 20~40%.

Effects of Rice Bran Dietary Fiber Extract on Gelatinization and Retrogradation of Wheat Flour (미강 식이섬유 추출물이 밀가루의 호화 및 노화에 미치는 영향)

  • Kim, Young-Soo;Ha, Tae-Youl;Lee, Sang-Hyo;Lee, Hyun-Yu
    • Korean Journal of Food Science and Technology
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    • v.29 no.3
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    • pp.464-469
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    • 1997
  • Rapid visco-analyzer (RVA) and differential scanning calorimetry (DSC) were used to study the effect of rice bran dietary fiber extract on gelatinization and retrogradation of wheat flour. The addition of rice bran dietary fiber extracts from various heat treated bran into wheat flour caused to increase the pasting temperature, peak viscosity and final viscosity of RVA measurements. For gelatinization measured with DSC, mixtures of wheat flour and rice bran dietary fiber extract had slightly higher To (onset temperature) and Tp (peak temperature) values than those of control (wheat flour), and wheat flour/defatted rice bran dietary fiber extract mixture had the lowest enthalpy value. In comparison with gelatinization, the retrogradation endotherm of mixtures stored at $4^{\circ}C$ up to 4 weeks occurred at about $20^{\circ}C$ lower temperatures than gelatinization endotherm with broader shape and well-defined thermograms with storage time. The retrogradation of wheat flour was retarded greatly by addition of rice bran dietary fiber extract, and there was no big difference between 5% and 10% additions.

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Addition Polymerization of 5-Norbornene-2-carboxylic Acid Esters Using Palladium Catalyst System: Synthesis of Monomers, Effect of Their Stereochemistry on Polymerization Behavior (Palladium 촉매를 이용한 5-Norbornene-2-carboxylic Acid Esters의 부가 중합: 단량체의 합성, 단량체의 Stereochemistry(Endo-, Exo-이성질체)가 고분자의 중합 거동에 미치는 영향)

  • Chung, Hae-Kang;Shim, Hyoug-Sub;Jeon, Seung-Ho;Kim, Ji-Heung;Nam, Sung Woo;Jeon, Boong Soo;Kim, Young Jun
    • Polymer(Korea)
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    • v.39 no.3
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    • pp.487-492
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    • 2015
  • The effects of chemical structure of alkyl groups of norbornene carboxylic alkyl esters(methyl, octyl, 4-chlorobenzyl) and endo/exo ratios of norbornene monomers on activity of palladium catalyst and polymerization behavior were investigated. Norbornene ester monomers were synthesized from the reaction of 5-norborene-2-carboxylic acid and various alcohols. Polymerization catalyst, di-${\mu}$-chloro-bis(-methoxybicyclo[2,2,1]-hept-2-ene)palladium(II) (DCBMP), was synthesized according to the literature procedure and silver hexafluoroantimonate ($AgSbF_6$) was used as a conjugate anion source. Gel permeation chromatography (GPC), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) were the principal techniques for polymer characterization and $^1H$ NMR spectroscopy was used for chemical structures determination of monomers and polymers. For all of the norbonene alkyl esters GPC data showed that when the amounts of endo isomers exceeded those of exo isomers decreased molecular weight polymers were obtained probably due to the decreased catalyst activity. Polymerizations were conducted by varying the monomer/catalyst mole ratios (100:1, 200:1, 300:1). When 300:1 monomer/catalyst ratio was employed it was possible to synthesize high molecular weight ($M_n=27500g/mol$), film forming polymer from exo-norbornene carboxylic acid octyl ester.