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

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Solvent-Polymer Interactions for Stable Non-Aqueous Graphene Dispersions in the Presence of PVK-b-PVP Block Copolymer (PVK-b-PVP 블록 공중합체의 존재 하에서 안정한 비 수계 그래핀 분산액을 위한 용매-고분자 상호작용에 관한 연구)

  • Park, Kyung Tae;Perumal, Suguna;Lee, Hyang Moo;Kim, Young Hyun;Cheong, In Woo
    • Journal of Adhesion and Interface
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    • v.18 no.3
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    • pp.109-117
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    • 2017
  • Poly(N-vinyl carbazole) (PVK) homopolymer, poly(4-vinylpyridine) (PVP) homopolymer, and PVK-b-PVP block copolymer were synthesized by reversible addition-fragmentation chain transfer (RAFT) polymerization and the polymers were used to prepare non-aqueous graphene dispersions with four different solvents, ethanol, N-methyl-2-pyrrolidone (NMP), dichloromethane (DCM), and tetrahydrofuran (THF). $^1H-$ and $^{13}C-NMR$ spectroscopy, size exclusion chromatography (SEC), and differential scanning calorimetry (DSC) were carried out to confirm the chemical structure of the polymers. Stability of graphene dispersions was measured by on-line turbidity measurement. Time-dependent Turbiscan Stability Index (TSI) values were interpreted in terms of surface tension (${\sigma}$) and solubility parameter (${\delta}$) among solvents, polymers, and graphene. It was confirmed that the solubilities of polymer and surface tension between solvent and graphene affected the dispersion stability of graphene. PVK-b-PVP block copolymer could effectively maintain the low TSI values of graphene dispersions in ethanol and THF, which have been known as poor solvents for graphene dispersions. It can also be noted that DCM shows good dispersion stability comparable to NMP, which has been known as the best solvent for graphene dispersion.

Effects of Moisture Content on Recrystallization of Rice Starch Gels (쌀전분겔의 재결정화에 미치는 수분함량의 영향)

  • Baik, Moo-Yeol;Kim, Kwang-Joong;Cheon, Ki-Cheol;Ha, Yeon-Chul;Kim, Wang-Soo
    • Korean Journal of Food Science and Technology
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    • v.29 no.5
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    • pp.939-946
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    • 1997
  • Effects of moisture content on the gelatinization and recrystallization of non-waxy and waxy rice starch gels were investigated by differential scanning calorimetry (DSC). The recrystallization rates of the starch gels containing various moisture contents $(40{\sim}70%)$ were analyzed by Avrami equation. The waxy rice starch had higher gelatinization temperature and enthalpy than non-waxy one. The highest degrees of recrystallization in both rice starch gels stored at $4^{\circ}C$ were shown at 40%, and recrystallizations above 80% moisture content were not found. The degree of recrystallization of waxy one was higher than that of non-waxy one in the range of 40 to 60% moisture content. The Avrami exponents (n) of both rice starch gels were near to 1.0 and the time constant (1/k) was increased with increasing moisture content in the range of 40 to 70% moisture content. The recrystallization rate of waxy rice starch gel was slower than that of non-waxy one. The recrystallization of rice starch gels could be explained by the change of ice melting enthalpy during storage. The Wg's, represented the maximum practical amount of plasticizing water, were about 29.9% and 28.2% for non-waxy and waxy rice starch gels, respectively.

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Synthesis and Characterization of Alkoxy and Alkylamino GAP Copolymer for Energetic Thermoplastic Elastomer (ETPE) (에너지화 열가소성 탄성체에 사용될 수 있는 알콕시 계열과 알킬 아민 계열 GAP Copolymer의 합성 및 분석)

  • Lim, Minkyung;Jang, Yoorim;Kim, Hancheul;Rhee, Hakjune;Noh, Sitae
    • Applied Chemistry for Engineering
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    • v.30 no.1
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    • pp.81-87
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    • 2019
  • In this study, synthetic methods and physical properties for a new class of glycidyl azide polymer (GAP) were investigated for energetic thermoplastic elastomers (ETPE). Four kinds of GAP copolymer polyols were synthesized by introducing nucleophiles such as azide, alkoxide and alkyl amine into poly(epichlorohydrin) (PECH). The GAP copolymer synthetic reaction can be evaluated as an environmental benign and efficient synthetic method due to the simultaneous one-step reaction using two kinds of nucleophiles and the complete consumption of sodium azide. The relative stoichiometric substitution ratio analysis and the progress of reaction were checked and monitored by inverse gated decoupled $^{13}C$ NMR and Fourier transform infrared (FT-IR) spectroscopy. The glass transition temperature and molecular weight were measured by differential scanning calorimetry (DSC) and gel permeation chromatography (GPC) analysis. The synthesized poly($GA_{0.8}-butoxide_{0.2}$), poly($GA_{0.7}-n-butylamine_{0.3}$), poly($GA_{0.7}-dipropylamine_{0.3}$) and poly($GA_{0.7}-morpholine_{0.3}$) had a glass transition temperature ranged from -39 to $-26^{\circ}C$.

Effects of Local Anesthetics on the Fluidity of Synaptosomal Plasma Membrane Vesicles Isolated from Bovine Brain (국소마취제가 Synaptosomal Plasma Membrane Vesicles의 유동성에 미치는 영향)

  • Yun, Il;Han, Suk-Kyu;Baik, Seung-Wan;Kim, Nam-Hong;Kang, Jung-Sook;Chung, Joong-Ki;Lee, Eun-Joo
    • The Korean Journal of Pharmacology
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    • v.24 no.1
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    • pp.43-52
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    • 1988
  • To elucidate the mechanism of action of local anesthetics, the effects of local anethetics on the microenvironment of the lipid bilayers of synaptosomal plasma membrane vesicles (SPMV) isolated from bovine brain and dimyristoylphosphatidylcholine (DMPC) multilamellar liposomes were investigated employing the intermolecular excimer fluorescence technique and differential scanning calorimetry (DSC). The relative intensities of excimer and monomer fluorescence of pyrene are a simple linear function of the viscosity of a homologous series of solvents. The microviscosity(${\eta}$)of the hydrocarbon region of SPMV was measured by this method and the value was $57.3{\pm}5.3\;cP$ at $37^{\circ}C$. In the presence of lidocaine-HCl and procaine-HCl, the values decreased to $46.5{\pm}5.1\;cP$ and $54.7{\pm}4.8\;cP$, respectvely. The differential scanning thermograms of DMPC multilamellar liposomes showed that local anesthetics significantly lowered the phase transition temperature, broadened the thermogram peaks, and reduced the size of the cooperative unit. These results indicate that local anesthetics have significant fluidizing effects on biomembranes and perturbation of membrane lipids may produce some, but not all, of their pharmacological actions.

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Synthesis and Characterization of Polypropylene-grafted Graphene Oxide via "Grafting-to" Method (폴리프로필렌으로 그래프트된 그래핀 옥사이드 제조 및 특성 분석)

  • Lee, Jong-Hee;Oh, Chang-Ho;Lim, Jung-Hyurk;Kim, Kyung-Min
    • Polymer(Korea)
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    • v.39 no.1
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    • pp.180-184
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    • 2015
  • PP-grafted GO was prepared by the reaction of graphene oxide (GO) containing 2-bromoisobuyryl groups and polypropylene (PP) having hydroxyl groups (PP-OH) via a "grafting-to" method. GO-Br was synthesized by the reaction of GO and 2-bromoisobutyryl bromide under a basic condition. PP-MAH was reacted with ethanolamine to produce PP-OH. The melting temperature of PP-grafted GO was shifted to the higher temperature than that of PP-OH. Also, the thermal stability of PP-grafted GO was increased as compared to PP-OH and GO. These results demonstrated that the grafted coating polymer PP was effective for enhancing the thermal stability of GO. The higher surface roughness of PP-grafted GO was resulted from the chemical attachment of PP on the surface of GO. The characterization of PP-grafted GO was conducted from Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and scanning electron microscope (SEM).

Evaluation of Porcine Myofibrillar Protein Gel Functionality as Affected by Microbial Transglutaminase and Red Bean [Vignia angularis] Protein Isolate at Various pH Values

  • Jang, Ho Sik;Lee, Hong Chul;Chin, Koo Bok
    • Food Science of Animal Resources
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    • v.35 no.6
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    • pp.841-846
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    • 2015
  • This study was investigated to determine the effect of microbial transglutaminase (MTG) with or without red bean protein isolate (RBPI) on the porcine myofibrillar protein (MP) gel functionality at different pH values (pH 5.75-6.5). Cooking yield (CY, %), gel strength (GS, gf), differential scanning calorimetry (DSC), and scanning electron microscopy (SEM) were determined to measure gel characteristics. Since no differences were observed the interaction between 1% RBPI and pH, data were pooled. CY increased with the addition of 1% RBPI, while it was not affected by pH values. GS increased with increased pH and increased when 1% RBPI was added, regardless of pH. There were distinctive endothermic protein peaks, at 56.55 and 75.02℃ at pH 5.75, and 56.47 and 72.43℃ at pH 6.5 in DSC results, which revealed decreased temperature of the first peak with the addition of 1% RBPI and increased pH. In SEM, a more compact structure with fewer voids was shown with the addition of 1% RBPI and increased pH from 5.75 to 6.5. In addition, the three-dimensional structure was highly dense and hard at pH 6.5 when RBPI was added. These results indicated that the addition of 1% RBPI at pH 6.5 in MTG-mediated MP represent the optimum condition to attain maximum gel-formation and protein gel functionality.

Formation and Thermal Properties of Amorphous Ti40Cu40Ni10Al10 Alloy by Mechanical Alloying (Mechanical Alloying에 의한 비정질 Ti40Cu40Ni10Al10 합금의 형성 및 열적특성)

  • Kim, Hyun-Goo
    • Journal of Powder Materials
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    • v.16 no.5
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    • pp.363-369
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    • 2009
  • The amorphization process and the thermal properties of amorphous Ti$_{40}$Cu$_{40}$Ni$_{10}$Al$_{10}$ powder during milling by mechanical alloying were examined by X-ray diffractometry (XRD), differential scanning calorimetry (DSC), and transmission electron microscopy (TEM). The chemical composition of the samples was examined by an energy dispersive X-ray spectrometry (EDX) facility attached to the scanning electron microscope (SEM). The as-milled powders showed a broad peak (2$\theta$ = 42.4$^{\circ}$) with crystalline size of about 5.0 nm in the XRD patterns. The entire milling process could be divided into three different stages: agglomeration (0 < t$_m$ $\leq$ 3 h), disintegration (3 h < t$_m$ $\leq$ 20 h), and homogenization (20 h < t$_m$ $\leq$ 40 h) (t$_m$: milling time). In the DSC experiment, the peak temperature T$_p$ and crystallization temperature T$_x$ were 466.9$^{\circ}C$ and 444.3$^{\circ}C$, respectively, and the values of T$_p$, and T$_x$ increased with a heating rate (HR). The activation energies of crystallization for the as-milled powder was 291.5 kJ/mol for T$_p$.

Gelatinization Properties of Waxy Black Rice Starch (찰흑미 전분의 호화 특성)

  • Choi, Gyeong-Cheol;Na, Hwan-Sik;Oh, Geum-Soon;Kim, Sung-Kon;Kim, Kwan
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.34 no.1
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    • pp.87-92
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    • 2005
  • This study was investigated to examine gelatinization properties of waxy black rice starches. X-ray diffraction patterns in raw starches showed traditional A type of cereals. The crystalline regions of both black rice and Shinsunchalbyeo starches disappeared when temperature increased to $65^{\circ}C$ where the crystalline regions of two starches changed to amorphous ones. Scanning Electron Microscope showed that granule type of Shinsunchalbyeo starch was more collapsed compared to that of black rice starch heated at 6$0^{\circ}C$. Gelatinization in both samples completed when samples were heated at 63$^{\circ}C$. The results by Differential Scanning Calorimetry (DSC) revealed that gelatinization patterns were similar in both samples. In Rapid Visco Analyzer examination, there was no difference in peak viscosity, breakdown, final viscosity and setback between Shinsunchalbyeo and waxy black rice starches.

The Effect of Grain Size and Cooling Rate on Phase Transformation for Mechanically Alloyed Ni-36at.%Al Alloy (기계적 합금화된 Ni-36at.%Al 합금의 상변태에 미치는 결정립 크기 및 냉각속도의 영향)

  • Kim, Seong-Uk;Kim, Dae-Geon;Kim, Ji-Sun;An, In-Seop;Kim, Yeong-Do
    • Korean Journal of Materials Research
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    • v.10 no.9
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    • pp.642-647
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    • 2000
  • Nanocrystalline NiAl alloy containing 36at.%Al was synthesized by mechanical alloying (MA). Synthesized powder was sintered by a pulse electric current sintering (PECS) facility. Effecting parameters on the phase transformation were discussed in terms of cooling rate and time spent on heat treatment. The behavior of phase transformation for sintered parts was examined by differential scanning calorimetry (DSC) and X-ray diffraction (XRD) method. Microstructure was observed by scanning electron microscopy (SEM). Martensitic lattice parameter and volume fraction was calculated by direct comparison method in X-ray diffraction analysis.

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Preparation and Characterization of Simvastatin Solid Dispersion using Aqueous Solvent

  • Kim, Kwang-Hyeon;Park, Jun-Bom;Choi, Won-Jae;Lee, Han-Seung;Kang, Chin-Yang
    • Journal of Pharmaceutical Investigation
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    • v.41 no.4
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    • pp.239-247
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    • 2011
  • Simvastatin is an inhibitor of 3-hydroxy-3-methylglutaryl-coenzyme A (HMG-CoA) reductase, which catalyzes the conversion of HMG-CoA to mevalonate, an early and rate-limiting step in the biosynthesis of cholesterol. Simvastatin has good permeability, but it also has low solubility (BCS class II), which reduces its bioavailability. To overcome this problem, a solid dispersion is formed using a spray-dryer with polymeric material carrier to potentially enhance the dissolution rate and extend drug absorption. As carriers for solid dispersion, Gelucire$^{(R)}$44/14 and Gelucire$^{(R)}$ 50/13 are semisolid excipients that greatly improve the bioavailability of poorly-soluble drugs. To avoid any toxic effects of an organic solvent, we used aqueous medium to melt Tween$^{(R)}$ 80 and distilled water. The structural behaviors of the raw materials and the solid dispersion were analyzed by differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD) and scanning electron microscopy (SEM). The DSC and PXRD data indicated that the crystalline structure of simvastatin was transformed to an amorphous structure through solid dispersion. Then, solid dispersion-based tablets containing 20 mg simvastatin were prepared with excipients. Dissolution tests were performed in distilled water and artificial intestinal fluid using the USP paddle II method. Compared with that of the commercial tablet (Zocor$^{(R)}$ 20 mg), the release of simvastatin from solid dispersion based-tablet was more efficient. Although the stability study is not complete, this solid dispersion system is expected to deliver poorly water-soluble drugs with enhanced bioavailability and less toxicity.