• Title/Summary/Keyword: Differential Scanning Calorimetry)(DSC)

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Relationship between Palatability and Physicochemical Properties of Carbohydrate Components in Rice Endosperm (쌀 배유 조성 탄수화물 특성과 식미와의 연관성)

  • Kim, Chae-Eun;Sohn, Jae-Keun;Kang, Mi-Young
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.52 no.4
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    • pp.421-428
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    • 2007
  • Eight varieties of milled rice showing different palatabilities were studied in order to identify the relationship between physicochemical properties of carbohydrate components and their fine structure. Gopumbyeo showed the highest palatability value among the eight varieties tested. Both peak viscosity and breakdown were hightest in Hitomebore, and lowest in Mihyangbyeo. No relationship was indicated between the palatability and gelatinization properties. The amylose content of starch showed a significant difference among the varieties tested. However, no relationship was found between the structure of amylose and the palatability of milled rice. The degree of branching(B/A value) was highest in Saechucheongbyeo, and lowest in Palgongbyeo in fine structure of amylopectin. But no relationship was indicated between the B/A values and the palatability of milled rice. Difference was indicated in properties of gelatinization of starch by differential scanning calorimetry. The enthalphy for gelatinization showed a significant difference among the varieties. However, no relationship was found between the enthalphy for gelatinization and the palatability of milled rice. Monosaccharide in endosperm was composed of rice were compound of rhamnose, fucose, ribose, arabinose, and xylose. The total content of monosaccharides was highest in Saechucheongbyeo, and lowest in Palgongbyeo. However, 7 varieties of milled rice, expect Palgongbyeo, showed no relationship between the palatability and monosaccharides contents.

Study of a Supercritical Fluid Process for the Preparation of Hydroxypropyl-β-cyclodextrin Inclusion Complexes (Hydroxypropyl-β-cyclodextrin 포접복합체 제조를 위한 초임계유체 공정 연구)

  • Lee, Sang-Yun;Kim, Jeong-Kyu;Kim, Woo-Sik;Ryu, Jong-Hoon;Lim, Gio-Bin
    • Korean Chemical Engineering Research
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    • v.43 no.1
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    • pp.110-117
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    • 2005
  • In this work, solid-state inclusion complex powders of itraconazole and $2-hydroxypropyl-{\beta}-cyclodextrin(HP-{\beta}-CD)$ were produced by a supercritical anti-solvent (SAS) process. In order to evaluate the degree of complexation, the thermal behavior of the microparticulate complexes was investigated using differential scanning calorimetry. The experimental results obtained for the solubility and dissolution rate of the microparticulate inclusion complexes in a buffer solution of pH 1.2 showed that the complexation of itraconazole with $HP-{\beta}-CD$ results in a significant increase in the solubility and dissolution rate of itraconazole. The particle size of the SAS-produced inclusion complexes was dramatically reduced ($<0.1-0.5{\mu}m$) compared with untreated itraconazole ($30-50{\mu}m$) and $HP-{\beta}-CD$ ($50-100{\mu}m$). The solubility of itraconazole was increased with the increase of pressure at a constant temperature to ca. $758.6{\mu}g/mL$ in an aqueous medium of pH 1.2. The dissolution rate of itraconazole was observed to be significantly improved and about 90% of itraconazole was found to be dissolved within 5-10 min.

Thermal, Frictional and Wear Behavior of Carbon Nanofiber/Poly(methyl methacrylate) Composites (탄소나노섬유/폴리(메틸 메타크릴레이트) 복합재료의 열적 및 마찰 마모 거동 연구)

  • Park Soo-Jin;Im Se-Hyuk;Lee Jae-Rock;Rhee John-M.
    • Polymer(Korea)
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    • v.30 no.5
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    • pp.385-390
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    • 2006
  • In this work, the effect of carbon nanofiber (CNF) on thermal properties, and friction and wear behavior of CNF/PMMA composites were examined. While thermal properties of the composites were investigated with differential scanning calorimetry, thermograyimetric analyzer, and dynamic mechanical analyzer friction and wear behaviors were examined using a friction and wear tester. The glass transition temperature (Tg), integral procedural decomposition temperature (IPDT), storage modulus (E'), and tan ${\delta}$ appeared at higher temperatures with increasing CNF content, which were probably attributed to the presence of strong interactions between the carbonaceous fillers and the PMMA resins matrix. The wear loss in the composites decreased at 0.1 wt% CNF and then increased with 5-10 wt% CNF content. This was due to the existence of large aspect ratio CNF in PMMA which led to an alignment of PMMA chains and an increase of mechanical interlocking, resulting in the formation of crosslinked structures between CNF and PMMA in the composite.

Synthesis and Properties of Nonlinear Optical Polyquinonediimine Containing Di-Azobenzene Group in the Side Chain (곁사슬에 디아조벤젠기를 갖는 비선형 광학 폴리퀴논디이민의 합성과 특성에 관한 연구)

  • Lee, Sang-Bae;Yang, Jung-Sung;Park, Dong-Kyu
    • Polymer(Korea)
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    • v.25 no.4
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    • pp.496-502
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    • 2001
  • Thermally stable polyquinonediimines(PQDI) containing di-azobenzene in the side chain were synthesized by means of condensation polymerization under $TiCl_4$. The synthesized monomers and polymers were identified by FT-IR, $^1H-NMR$, and elemental analysis. Especially, the polymerization of PQDI was confirmed by the double-bonding peak of >C=N appearing near 1625cm$^{-1}$ in FT-IR spectrum. PQDI with di-azobenzene group in one side chain was insoluble in methanol, acetone and non-polar solvents having big dielectric constant, but had good solubility in polar solvents having small dielectric constant. Molecular weight distribution of PQDI measured by GPC was 1.38. It was confirmed to be amorphous polymer through X-ray diffraction by the appearance of the halo in case of PQDI containing di-azobenzene in the side chain. The glass transition temperature ($_g$) of synthesized polymer was measured to be 116$^{\circ}C$ by differential scanning calorimetry. The SHG value for ${\chi}^{(2)}$ was 1.2 pm/V (${\lambda}$ = 1.542 ${\mu}$m). The SHG value slightly decreased in an early stage but showed temporal stability after 20 hours.

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Effect of Solubilizing and Microemulsifying Excipients in Polyethylene Glycol 6000 Solid Dispersion on Enhanced Dissolution and Bioavailability of Ketoconazole

  • Heo, Min-Young;Piao, Zong-Zhu;Kim, Tae-Wan;Cao, Qing-Ri;Kim, Ae-Ra;Lee, Beom-Jin
    • Archives of Pharmacal Research
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    • v.28 no.5
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    • pp.604-611
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    • 2005
  • Polyethylene glycol (PEG) 6000-based solid dispersions (SDs), by incorporating various pharmaceutical excipients or microemulsion systems, were prepared using a fusion method, t o compare the dissolution rates and bioavailabilities in rats. The amorphous structure of the drug in SDs was also characterized by powder X-ray diffractometry (XRD) and differential scanning calorimetry (DSC). The ketoconazole (KT), as an antifungal agent, was selected as a model drug. The dissolution rate of KT increased when solubilizing excipients were incorporated into the PEG-based SDs. When hydrophilic and lipophilic excipients were combined and incorporated into PEG-based SDs, a remarkable enhancement of the dissolution rate was observed. The PEG-based SDs, incorporating a self microemulsifying drug delivery system (SMEDDS) or microemulsion (ME), were also useful at improving the dissolution rate by forming a microemulsion or dispersible particles within the aqueous medium. However, due to the limited solubilization capacity, these PEG-based SDs showed dissolution rates, below 50% in this study, under sink conditions. The PEG-based SD, with no pharmaceutical excipients incorporated, increased the maximum plasma concentration (C$_{max}$) and area under the plasma concentration curve (AUC$_{0-6h}$) two-fold compared to the drug only. The bioavailability was more pronounced in the cases of solubilizing and microemulsifying PEG-based SDs. The thermograms of the PEG-based SDs showed the characteristic peak of the carrier matrix around 60$^{\circ}C$, without a drug peak, indicating that the drug had changed into an amorphous structure. The diffraction pattern of the pure drug showed the drug to be highly crystalline in nature, as indicated by numerous distinctive peaks. The lack of the numerous distinctive peaks of the drug in the PEG-based SDs demonstrated that a high concentration of the drug molecules was dissolved in the solid-state carrier matrix of the amorphous structure. The utilization of oils, fatty acid and surfactant, or their mixtures, in PEG-based SD could be a useful tool to enhance the dissolution and bioavailability of poorly water-soluble drugs by forming solubilizing and microemulsifying systems when exposed to gastrointestinal fluid.

Thermal Stability of Grubbs' Catalyst and Its Reactivity with Self-healing Agents (Grubbs' Catalyst의 열안정성 및 자가치료제와의 반응성 평가)

  • Yoon, Sung Ho;Shi, Ya Long;Feng, Jun;Jang, Se Yong
    • Composites Research
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    • v.28 no.6
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    • pp.395-401
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    • 2015
  • This study investigated the thermal stability of Grubbs' catalyst and its reactivity with self-healing agents for self-healing damage repair. Four types of Grubbs' catalyst supplied by manufacturers were considered and each catalyst was tested in as-received and grinded conditions. Four types of self-healing agents were prepared by varying the mixing ratio of dicyclopentadiene (DCPD) and 5-ethylidene-2-norbonene (ENB). Heat flows as a function of temperature were measured through a differential scanning calorimetry (DSC) to determine the thermal stability of catalysts. Reaction heats of self-healing agents with the catalyst were measured to evaluate the reactivity of the catalyst. For this evaluation, Fluka Chemika Grubbs' catalyst was used based on the maximum temperature and the time to reach the maximum temperature. According to the results, catalysts had different shapes depending on the manufacturer and the results showed that the smaller the size of the catalyst the higher the reactivity with self-healing agents. As the ENB ratio in self-healing agents increased, the maximum temperature increased, and the time to reach the maximum temperature decreased. As the amount of the catalyst increased, the maximum temperature increased, and the time to reach the maximum temperature decreased. Considering the thermal stability of the catalyst and its reactivity with the self-healing agent, combination of 0.5 wt% catalyst and the D3E1 self-healing agent was optimal for self-healing damage repair. Finally, as the thermal decomposition may occur depending on the environmental temperature, the catalyst must not be exposed to temperature higher than that is necessary to maintain the thermal stability of the catalyst.

Production of Diacylglycerol-Oil from Lipase-Catalyzed Reaction Using Soybean Oil and Glyceryl Monooleate (대두유와 Glyceryl Monooleate의 효소적 반응을 이용한 Diacylglycerol 함유 유지의 생산)

  • Jeon, Mi-Sun;Lee, Cho-Rong;Lee, Ki-Teak
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.38 no.11
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    • pp.1559-1563
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    • 2009
  • Scaled-up production of oil containing diacylglycerol (DAG), so called diacylglycerol-oil, was produced by lipase-catalyzed reaction. Mixture of soybean oil and glyceryl monooleate with 1:2 molar ratio was esterified with Lipozyme RMIM in a batch-type reactor at 55$^{\circ}C$ and 300 rpm during 6 hr. After short-path distillation for removal of monoacylglycerol and free fatty acid as reaction by-products, diacylglycerol-oil mainly consisted of DAG (29 area%) and TAG (71 area%). The major compositional fatty acids in diacylglycerol-oil were oleic (44.36 wt%), and linoleic acids (37.36 wt%). Acid value and iodine value of diacylglycerol-oil were 0.13 and 112.6, respectively. Solid fat content (SFC) of diacylglycerol-oil was observed after differential scanning calorimetry (DSC) analysis in which three melting peaks at -25.0, 0.1, and 11.2$^{\circ}C$ were shown.

Synthesis and Properties of Arylacetylene Resins with Siloxane Units

  • Gao, Fei;Zhang, Lingling;Tang, Lemin;Zhang, Jian;Zhou, Yan;Huang, Farong;Du, Lei
    • Bulletin of the Korean Chemical Society
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    • v.31 no.4
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    • pp.976-980
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    • 2010
  • A series of arylacetylene resins with siloxane units were synthesized by the condensation reactions of m-diethynylbenzene magnesium reagents with various $\alpha,\omega$-bis(chloro)dimethylsiloxanes. These resins are liquids and are miscible with common organic solvents at room temperature. The structures of the resins were characterized by FT-IR, $^1H$ NMR, $^{13}C$ NMR, $^{29}Si$ NMR, and gel permeation chromatography (GPC). The thermal behaviors of the resins were examined with differential scanning calorimetry (DSC). These resins have good processability. They can be thermally cross-linked through the ethynyl groups to produce cured resins. The thermal and thermooxidative stabilities of the cured resins were studied by thermogravimetric analysis (TGA). The cured resins possess high thermal and thermooxidative stability. Their decomposition occurs at above $500^{\circ}C$ in both $N_2$ and air. With increasing the length of siloxane units in the resins, the thermal stability of the cured resins decreases in $N_2$. When the cured resins were sintered above $1450^{\circ}C$ under argon, hard and glassy SiOC ceramics were obtained. These SiOC ceramics have the decomposition temperatures at 5% weight loss above $800^{\circ}C$ in air.

Development of Chitosan Coated Solid Lipid Nano-particles Containing 7-Dehydrocholesterol (7-디하이드로콜레스테롤을 함유한 키토산 코팅 처리 Solid Lipid Nano-particle의 개발에 관한 연구)

  • Lee Geun-Soo;Kim Tae-Hoon;Lee Chun-Il;Pyo Hyeong-Bae;Choe Tae-Boo
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.31 no.2 s.51
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    • pp.141-146
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    • 2005
  • Unstable cosmetic active ingredients could rapidly break down in chemical and photochemical process. Therefore, it has become a very important issue to encapsulate active ingredient for the stabilization. 7-Dehydrocholesterol (7-DHC), a precursor of vitamin $D_3$, has been shown to increase levels of protein and mRNA for heat shock protein in normal human epidermal keratinocytes. However, topical dermal application of 7-DHC is restricted due to its poor solubility and chemical unstability. In this study, 7-DHC was incorporated into nano-emulsion (NE), solid lipid nano-particle (SLN), and chitosan coated solid lipid nano-particle (CASLN), respectively. In order to prepare NE and SLN dispersion, high-pressure homogenization at temperature above the melting point of lipid was used Hydrogenated lecithin and polysorbate 60 were used as stabilizer for NE and SLN. CASLN was prepared by high speed homogenizing after adding chitosan solution to the SLN dispersion and showed positively charged particle properties. Decomposition rate of 7-DHC in NE, SLN and CASLN was studied as a function of time at different temperature. Differential scanning calorimetry (DSC) and X-ray diffraction (XRD) studies were performed to characterize state of lipid modification. It appeared that CASLN is the most effective to stabilize 7-DHC and may be used for a useful topical dermal delivery system.

Preparation of Ion Exchange Membranes for Fuel Cell Based on Crosslinked Poly(vinyl alcohol) with Poly(acrylic acid-co-maleic acid)

  • Kim, Dae-Sik;Park, Ho-Bum;Lee, Chang-Hyun;Lee, Young-Moo;Moon, Go-Young;Nam, Sang-Yong;Hwang, Ho-Sang;Yun, Tae-II;Rhim, Ji-Won
    • Macromolecular Research
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    • v.13 no.4
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    • pp.314-320
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    • 2005
  • Crosslinked poly(vinyl alcohol) (PVA) membranes were prepared at various crosslinking temperatures using poly(acrylic acid-co-maleic acid) (PAM) containing different PAM contents. The thermal properties of these PVA/PAM membranes prepared at various reaction temperatures were characterized using differential scanning calorimetry (DSC). The proton conductivity and methanol permeability of PVA/PAM membranes were then investigated as PAM content was varied from 3 to 13 wt%. It was found that the proton and methanol transport were dependent on PAM content in their function both as crosslinking agent and as donor of hydrophilic -COOH groups. Both these properties decreased monotonously with increasing PAM concentration. The proton conductivities of these PVA/PAM membranes were in the range from $10^{-3}\;to\;10^{-2}S/cm$ and the methanol permeabilities from $10^{-7}\;to\;10^{-6}cm^{2}/sec$. In addition, the effect of operating temperature up to $80^{\circ}C$ on ion conductivity was examined for three selected membranes: 7, 9 and 11 wt% PAM membranes. Ion conductivity increased with increasing operating temperature and showed and S/cm at $80^{\circ}C$, respectively. The effects of crosslinking and ionomer group concentration were also examined in terms of water content, ion exchange capacity (IEC), and fixed ion concentration. In addition, the number of water molecules per ionomer site was calculated using both water contents and IEC values. With overall consideration for all the properties measured in this study, $7{\sim}9\;wt%$ PAM membrane prepared at $140^{\circ}C$ exhibited the best performance. These characteristics of PVA/PAM membranes are desirable in applications related to the direct methanol fuel cell (DMFC).