• 제목/요약/키워드: Differential scanning calorimetry (DSC)

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Camptothecin 유도체의 결정형 (Crystal Form of A Camptothecin Derivative)

  • 손영택;문현영
    • Journal of Pharmaceutical Investigation
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    • 제32권2호
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    • pp.81-85
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    • 2002
  • Three polymorphic modifications of CKD-602, water soluble derivative of camptothecin, were obtained by the recrystallization from different organic solvents and characterized by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and X-ray powder diffraction (XRPD). The major endothermic peaks of the DSC curve of Form 1, Form 2 and Form 3 was shown at $268.71^{\circ}C$, $247.83^{\circ}C$, $244.76^{\circ}C$, respectively. Form 2 was elucidated to be an acetic acid solvate and Form 3 was elucidated to be a methanol solvate. The dissolution patterns of these three modifications were also checked in distilled water at $37{\pm}0.5^{\circ}C$, for 30 minutes. The polymorphic modifications showed differences in the dissolution rate. The dissolution rate of Form 1 was faster than that of other polymorphic modifications. When stored at different relative humidity over the period of 3 months, all of the polymorphic modifications did not undergo transformation.

Effects of Cereal Powders with Dietary Fibers on Retrogradation Properties of Jeungpyun, a Korean Traditional Fermented Rice Cake

  • Park, Mie-Ja;Kim, Hye Young L.
    • 한국환경보건학회지
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    • 제29권4호
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    • pp.48-54
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    • 2003
  • This study investigated retrogradation properties of Jeungpyun substituted for cereals with dietary fibers of 60% of brown rice, and barley. Quality changes during storage periods of the functional Jeungpyun, were studied using $\alpha$-amylase iodine enzyme digestion methods, X-ray diffraction patterns, and differential scanning calorimetry (DSC). The barley substituted samples showed significantly lower retrogrdation rates than those of control when examined by $\alpha$-amylase method. The Relative crystallity by X-ray diffraction patterns had typical A type in all samples with appealing big crystallity around its diffraction angle 23$^{\circ}$degrees as storage periods were increased. The brown rice and barley Jeunpyun made smaller crystallity than that of control, representing slower retrogradation rates. The batter controls had significantly lower ΔH than the other compared samples when measured by DSC, but had significantly higher ΔH after 30 days of storage, implying that the control required more energy for regelatinization after the 30 days of storage.

Studies on thermal and swelling properties of Poly (NIPAM-co-2-HEA) based hydrogels

  • Shekhar, Suman;Mukherjee, M.;Sen, Akhil Kumar
    • Advances in materials Research
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    • 제1권4호
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    • pp.269-284
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    • 2012
  • Thermoresponsive hydrogels based on N-Isopropylacrylamide (NIPAM) and 2-Hydroxyethylacrylate (HEA) were prepared by free radical polymerization. The hydrogels were characterized by elemental (CHN) analysis, differential scanning calorimetry (DSC) and thermo gravimetric analysis (TGA). DSC thermogram showed two endothermic transitions which are due to hydration of water present in different environments. One near $0^{\circ}C$ called melting transition of ice and was used to calculate the quantitative determination of the amounts of freezing and non freezing water. The other transition above the ambient temperature was due to the combination of hydrophobic hydration and hydrophilic hydration which changes with the copolymer compositions. Swelling and deswelling studies of the hydrogels were carried out using the aqueous media, salt and urea solutions. The experimental results from swelling studies revealed that copolymers have lower rates of swelling and deswelling than the homopolymer.

PSE돈육 드립의 열안정성에 관한 연구 (Studies on the Thermal Stability of Free Drip Released from PSE Pork Muscle)

  • 김천제
    • 한국축산식품학회지
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    • 제20권2호
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    • pp.146-151
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    • 2000
  • The objective of this study was to investigate the characteristics on the thermal denaturation of free drip released from pork loin during chilled storage using DSC(differential scanning calorimetry). DSC thermogram of drip released from normal pork(NORD) was characterized by a minor peak and two major peaks with temperature maxima at $61.5^{\circ}C$, $71.7^{\circ}C$ (associated with sarcoplasmic proteins) and $84.3^{\circ}C$ (associated with protein-protein interaction and aggregation). In the denaturation temperature of drip released from PSE pork (PSED), the peak(Tmax) at $59.0^{\circ}C$ was reduced by $2.5^{\circ}C$. When the thermograms were divided into segments correponding to the three peaks, $\Delta$H2 was shown to be reduced by 10% in PSED as compared to NORD. With the decrease in the solubility of sarcoplasmic proteins in PSE muscle, there was a corresponding increase the drip loss during the storage.

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Thermal Stability of Lithiated Silicon Anodes with Electrolyte

  • Park, Yoon-Soo;Lee, Sung-Man
    • Bulletin of the Korean Chemical Society
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    • 제32권1호
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    • pp.145-148
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    • 2011
  • The thermal behavior of lithiated Si anodes has been investigated using differential scanning calorimetry (DSC). In particular, the effect of Si particle size on the thermal stability of a fully lithiated Si electrode was investigated. For DSC measurements, a lithiated Si anode was heated in a hermetically sealed high-pressure pan with a polyvinylidene fluoride (PVDF) binder and a 1 M $LiPF_6$ solution in an ethylene carbonate (EC)-diethyl carbonate (DEC) mixture. The thermal evolution around $140^{\circ}C$ increases with lithiation and with decreasing particle size; this phenomenon is attributed to the thermal decomposition of the solid electrolyte interface (SEI) film. Exothermic peaks, following a broad peak at around $140^{\circ}C$, shift to a lower temperature with a decrease in particle size, indicating that the thermal stability of the lithiated Si electrode strongly depends on the Si particle size.

Crystal Form of Olmutinib

  • Lee, Chang-Yeob;Sohn, Young-Taek
    • 대한화학회지
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    • 제63권1호
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    • pp.7-11
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    • 2019
  • Olmutinib, N-[3-({2-[4-(4-methylpiperazine-1-yl)aniline]thieno[3,2-d]Pyrimidin-4-yl}oxy)phenyl]prop-2-enamide dihydrochloride monohydrate, $Olita^{TM}$ is an oral, third-generation epidermal growth factor receptor tyrosine kinase inhibitor (EGFR TKI) that was developed by Boehringer Ingelheim and Hanmi Pharmaceutical Co. Ltd for the treatment of non-small cell lung cancer (NSCLC). The aim of this work was to investigate the existence of polymorphs and pseudopolymorphs of olmutinib. Three crystal forms of olmutinib have been isolated by recrystallization and characterized by differential scanning calorimetry (DSC), thermogravimetric (TG) analysis and powder X-ray diffractometry (PXRD). From the DSC and TG data it was confirmed that Form 1 is monohydrate, Form 2 is dihydrate, Form 3 is 1.5 hydrate. The PXRD patterns of three crystal forms were different respectively. After storage of 1 month at $2^{\circ}C$, 24% RH (Relative Humidity), Form 1, Form 2, and Form 3 were not transformed.

혼합 액체 연료의 화학반응 인자 계측에 관한 실험적 연구 (An Experimental Study on Measurement of Chemical Kinetic Parameters of a Liquid Fuel with Various Components)

  • 최효현;임준석;김철진;손채훈
    • 한국연소학회지
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    • 제16권3호
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    • pp.21-26
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    • 2011
  • Thermal analyses are conducted to measure chemical kinetic parameters of an unknown liquid fuel with various components. Thermal Analyses are divided into two different methods such as TGA(Thermo-Gravimetric Analysis) and DSC(Differential Scanning Calorimety). Non-isothermal experimental results are analyzed by adopting TGA and they are filtered by Freeman-Carroll method. As a results of the analysis, chemical parameters of the activation temperature and the reaction order are measured to be 6128.2 K and 1.4, respectively. Furthermore, the chemical kinetic parameters are obtained by a variety of mathematical processing methods. It has been found that they show a little difference depending on the processing method.

양이온성 계면활성제로 표면개질된 몬모릴로나이트의 탈수 특성 (Dehydration Characteristics of Cationic Surfactant-Modified Montmorillonite)

  • Seung Yeop Lee;Soo Jin Kim
    • 한국광물학회지
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    • 제15권4호
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    • pp.305-314
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    • 2002
  • HDTMA로 표면개질된 몬모릴로나이트의 탈수현상을 X-선 회절분석기와 시차주사열량측정 기(DSC)로 조사하였다 열에 의한 HDTMA-몬모릴로나이트의 탈수작용은 유기점토의 팽창거동에 영향을 주었다. HDTHA-몬모릴로나이트의 기저d(001)두께/온도변화 곡선은 크기가 다른 2개의 팽창피크를 보여주었다. 이것은 일차적으로 계면활성제의 정렬에 의한 점토광물의 층간팽창이 10$0^{\circ}C$ 부근에서 발생하고 알킬고리의 이차적인 수직배열에 의한 층간팽창이 20$0^{\circ}C$ 부근에서 일어났음을 가리킨다. 따라서, 이러한 결과는 유기점토의 탈수작용에 의해 점토 규산염층에 상대적으로 수직적인 알킬고리의 배열이 활성화되며, 소규모의 층간팽창을 야기한다는 것을 지시한다.

임게전류밀도 향상을 위한 Cu/NbTi다층박막과 초전도 선재에서의 계면반응 (Interfacial reactions in Cu/NbTi multilayer thin films and superconducting wires)

  • 심재엽;백홍구;하동우;오상수;류강식
    • E2M - 전기 전자와 첨단 소재
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    • 제8권4호
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    • pp.478-486
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    • 1995
  • Cu/NbTi multilayer thin films and superconducting wires were fabricated and heat treated with conventional annealing and analyzed by differential scanning calorimetry (DSC) as a basic study for the enhancement of Jc. Interfacial reactions of Cu/NbTi multilayer thin films and superconducting wires were investigated with optical microscope, SEM, and XRD. According to the effective heat of formation (EHF) model, CU$\_$3/Ti was predicted as a first phase. However, considering the crystalline structure and thermodynamics, CuTi was predicted as a first phase. According to the results of DSC and XRD, CU$\_$2/Ti was found to be the first phase, followed by the formation Of CU$\_$4/Ti. The difference in first crystalline phase between the experimental result and the predicted one was discussed. In case of Cu/NbTi superconducting wires, the compounds formed at the Cu/NbTi interface grew with annealing time and the amount of compounds formed in Nb-47wt%Ti alloy was larger than that in Nb-50wt%Ti alloy. It seemed that the incubation time for the formation of compounds in Nb-50wt%Ti alloy was longer than that formed in Nb-47wt%Ti alloy. Also, the diffusion was the rate controlling step for the growth of compounds in all specimens. These compounds were formed at 500-600.deg. C for I hour annealing and, thus, the drawing time below I hour must be required to minimize the growth of compounds for the enhancement of Jc.

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다양한 아민 단량체로 합성한 무색투명 폴리이미드 필름 특성 (Characterization of Colorless and Transparent Polyimide Films Synthesized with Various Amine Monomers)

  • 최일환;장진해
    • 폴리머
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    • 제34권5호
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    • pp.480-484
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    • 2010
  • 무수산인 4,4'-(4,4'-isopropylidene-diphenoxy)bis(phthalic anhydride)(BPADA)와 아민계인 2,2'-bis(trifluoromethyl)benzidine(TFB), bis(3-aminophenyl)sulfone(APS), 4,4'-methylene-bis-(2-methylcyclohexylamine)(MMCA), bis[4-(3-aminophenoxy)phenyl]sulfone(BAPS)에 melamine을 각각 5 몰%로 반응시켜 N,N'-dimethylacetamide(DMAc) 용매 속에서 폴리아믹산(poly(amic acid), PAA)들을 얻었다. 용액 상태의 PAA를 캐스팅하여 각각 다른 반응 온도에서 열처리를 통해 무색 투명한 폴리이미드(PI) 필름을 얻었다. PI의 열적 성질, 광학적 특성을 다양한 아민 구조의 변화에 따라 조사하였으며, 열적 성질은 differential scanning calorimetry(DSC), thermogravimetric analysis(TGA), thermomechanical analysis(TMA)를 이용해 측정하였고, 광학적 투명도는 색차계(spectrophotometry)를 이용하였다. 제조된 모든 필름의 열 팽창계수는 $48.53-64.24ppm/^{\circ}C$ 사이의 값을 얻었으며, 모든 필름 시료의 노란색 지수(yellow index, YI)는 3 이하를 나타내었다.