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

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Synthesis and characterization of soft magnetic composite in Fe2O3-Mg system by mechanical alloying (기계적합금화에 의한 Fe2O3-Mg계 연자성 콤포지트의 합성 및 평가)

  • Lee, Chung-Hyo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.25 no.6
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    • pp.245-251
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    • 2015
  • We have applied mechanical alloying (MA) to produce soft magnetic composite material using a mixture of elemental $Fe_2O_3$-Mg powders. An optimal milling and heat treatment conditions to obtain soft magnetic ${\alpha}$-Fe/MgO composite with fine microstructure were investigated by X-ray diffraction, differential scanning calorimetry (DSC) and vibrating sample magnetometer (VSM) measurement. It is found that ${\alpha}$-Fe/MgO composite powders in which MgO is dispersed in ${\alpha}$-Fe matrix are obtained by MA of $Fe_2O_3$ with Mg for 30 min. The saturation magnetization of ball-milled powders increases with increasing milling time and reaches to a maximum value of 69.5 emu/g after 5 h MA. The magnetic hardening due to the reduction of the ${\alpha}$-Fe grain size by MA was also observed. Densification of the MA powders was performed in a spark plasma sintering (SPS) machine at $800{\sim}1000^{\circ}C$ under 60 MPa. X-ray diffraction result shows that the average grain size of ${\alpha}$-Fe in ${\alpha}$-Fe/MgO nanocomposite sintered at $800^{\circ}C$ is in the range of 110 nm.

Storage Quality Characteristics of Bread Added with Dried Mulberry Pomace (저장 중 건오디박 첨가 빵의 품질 특성)

  • Kim, Hyun Jeong;Shin, Suk Kyung;Kim, Mee Ree
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.42 no.12
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    • pp.1972-1980
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    • 2013
  • The purpose of this study is to evaluate the storage quality characteristics of bread with added dried mulberry pomace (DMP, 0, 1, 3 or 5%) during storage at $4^{\circ}C$ for 7 days. During the entire storage period, the moisture content was higher in breads containing DMP compared with the control bread. Textural properties by TPA showed that the hardness of DMP bread maintained a lower hardness than that of the control during the entire storage period. Moreover, DSC (Differential Scanning Calorimetry) result showed that ${\Delta}H$ (crystal melting enthalpy) of the bread containing DMP was lower than that of the control bread, which indicate the retarding of retrogradation. The sensory preference test results demonstrated that the bread with 3% DMP had higher scores in over-all preference than the others. These results suggest that DMP delays the retrogradation of bread during storage.

Properties of Starch Isolated from Wet-milled Rice after Steeping at Elevated Temperatures for Annealing Effect (Annealing 수침처리에 따른 습식제분 쌀가루의 전분 특성)

  • Lee, Young-Tack;Yoo, Moon-Sik;Lee, Bo-Ram;Park, Jong-Hyun;Chang, Hak-Gil
    • Korean Journal of Food Science and Technology
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    • v.36 no.3
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    • pp.393-397
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    • 2004
  • Rice was steeped at elevated temperatures of $40,\;50,\;or\;60^{\circ}C$ for 2 hr, and physicochemical properties of starches isolated from wet-milled rice flour were investigated. Steeping at elevated temperatures slightly decreased lightness of rice starch, while increased yellowness and redness. Average granule size of rice starch was decreased by steeping treatment. Swelling power and solubility increased as temperature increased. Starch from rice steeped at $40^{\circ}C$ displayed highest swelling power and solubility. Differential scanning calorimetry data of starch obtained from steeped rice at $60^{\circ}C$ showed increased onset and peak temperatures, with narrower gelatinization temperature range, suggesting partial annealing effect. Pasting properties of starch measured by Rapid Visco-Analyzer indicated increased peak viscosity due to rice steeping at $40^{\circ}C$. Peak and breakdown viscosities decreased at $50\;and\;60^{\circ}C$, whereas setback and final viscosities increased.

Hydrophobic Cyclodextrin Derivatives as a Sustained Release Carrier of Azidothymidine (아지도싸이미딘의 지속성방출형담체로서의 소수성시클로덱스트린유도체)

  • Seo, Bo-Youn;Park, Gee-Bae;Lee, Kwang-Pyo
    • Journal of Pharmaceutical Investigation
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    • v.26 no.2
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    • pp.71-82
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    • 1996
  • This study has been undertaken to evaluate hydrophobic cyclodextrin(CD) derivatives as a sustained release carrier of azidothymidine(AZT), AZT, which has potent activity against AIDS and AIDS-related complex as thymidine analogue, has been reported that it has significant toxicity and short half life. Therefore, it is necessary to design sustained release oral dosage form to avoid undesirable side effects attributable to an excessive plasma concentration and to reduce the frequency of administration of AZT. Inclusion complexes of AZT with $acetyl-{\beta}-cyclodextrin\;(AC{\beta}CD)$ and $triacetyl-{\beta}-cyclodextrin(TA{\beta}CD)$ were prepared by solvent evaporation method. Interactions of AZT with CD were investigated by Differential Scanning Calorimetry(DSC) and Infrared Spectrophotometry(IR). The decreasing order of water solubilities of AZT and AZT-CD inclusion complexes were as follows; $AZT\;(27.873{\pm}0.015,mg/ml)\;>\;AZT-AC{\beta}CD\;(3.377{\pm}0.003)\;>\;AZT-TA{\beta}CD\;(2.528{\pm}0.001)$. Partition coefficients of $AZT-AC{\beta}CD\;and;\AZT-TA{\beta}CD$ inclusion complexes were increased by 1.27-fold, 1.54-fold in pH 1.2 and 1.32-fold, 1.47-fold in pH 6.8 in comparison with that of AZT. The mean dissolution time (MDT, min) which represents the rapidity of dissolution rate of AZT, $AZT-AC{\beta}CD,\;AZT-TA{\beta}CD$ were 5.12, 14.02 and 19.38 min in pH 1.2 and 2.52, 15.19 and 18.19 min in pH 6.8. AZT was very rapidly and completely dissolved in pH 1.2 and pH 6.8 within 5 minutes. But AZT-CD inclusion complexes showed the sustained release pattern in comparison with AZT alone. The simultaneous in situ nasal and jejunal recirculation study to compare the intrinsic absorptivity and the property of absorption sites revealed that the absorption of $AZT-TA{\beta}CD\;(N:35.35{\pm}1.08%,\;J:27.47{\pm}1.18%)$ was more than that of $AZT\;(N:16.89{\pm}2.25%,\;J:15.86{\pm}2.33%)$. The above results suggest that $TA{\beta}CD$ which is a hydrophobic cyclodextrin may serve as sustained release carrier with absorption enhancing effect.

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Slow Cook-Off Test and Evaluation for HTPE Insensitive Propellants (HTPE 둔감추진제 완속가열 시험평가)

  • Yoo, Ji-Chang;Kim, Chang-Kee;Kim, Jun-Hyung;Lee, Do-Hyung;Min, Byung-Sun
    • Journal of the Korean Society of Propulsion Engineers
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    • v.14 no.6
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    • pp.31-37
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    • 2010
  • This study was carried out to investigate the thermal decomposition and execute EIDS slow cook-off test for the propellant ingredients and 2 kinds of HTPE propellants. The thermal analysis of the propellant ingredients used in this study showed that the thermal stability of these materials decreases in the following order : AP > HTPE > AN > BuNENA. In addition, propellant HTPE 002 containing AN showed that an endothermic process at around $125^{\circ}C$ corresponding to the solid phase change(II$\rightarrow$I) of AN was followed by the exothermic process of BuNENA/AN mixture up to $200^{\circ}C$. In EIDS slow cook-off tests, HTPE 001 and HTPE 002 reacted at around $250^{\circ}C$ and $152^{\circ}C$ respectively, and both of them showed sudden temperature increase curves at $115^{\circ}C$. The critical temperatures, $T_c$, of thermal explosion for the propellants HTPE 001 and HTPE 002, were obtained from both the non-isothermal curves at various heating rates and Semenov's thermal explosion theory. Kissinger's method that was used to calculate $T_c$ was also employed to obtain the activation energies for thermal decompositions.

Characterization and consolidation of thermoelectric CrSi2 compound prepared by mechanical alloying (MA법으로 제조된 CrSi2 열전화합물의 평가 및 치밀화)

  • Lee, Chung-Hyo;Kim, Young
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.23 no.3
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    • pp.135-141
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    • 2013
  • Mechanical alloying was carried out to produce $CrSi_2$ thermoelectric compound using a mixture of elemental $Cr_{33}Si_{67}$ powders. An optimal milling and heat treatment conditions to obtain the single phase of $CrSi_2$ compound with fine microstructure were investigated by X-ray diffraction and differential scanning calorimetry measurement. $CrSi_2$ intermetallic compound with a grain size of 70 nm could be obtained by MA of $Cr_{33}Si_{67}$ powders for 70 hours and subsequently annealed at $650^{\circ}C$. Consolidation of the MA powders was performed in a spark plasma sintering (SPS) machine using graphite dies at $600{\sim}1000^{\circ}C$ under 60 MPa. The shrinkage of MA samples during SPS consolidation process increased gradually with increasing temperature up to $1000^{\circ}C$ and relatively significant at about $600^{\circ}C$. We tend to believe that these behaviors are deeply related to form a $CrSi_2$ compound during heating process, as can be realized from the DSC measurement. Electrical conductivity and Seebeck coefficient of sintered bodies were measured up to $900^{\circ}C$. Seebeck coefficient and power factor of $Cr_{33}Si_{67}$ compact prepared by MA and SPS at $1000^{\circ}C$ showed the maximum value of $125{\mu}V/K$ at $400^{\circ}C$ and $4.3{\times}10^{-4}W/mK^2$ at $350^{\circ}C$, respectively.

Fabrication and densification of Heusler Fe2VAl alloy powders by mechanical alloying (MA법에 의한 Heusler Fe2VAl 합금분말의 제조 및 치밀화)

  • Kim, Kwang-Duk;Lee, Chung-Hyo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.23 no.1
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    • pp.51-57
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    • 2013
  • We have applied mechanical alloying (MA) to produce Heusler $Fe_2VAl$ thermoelectric alloy using a mixture of elemental $Fe_{50}V_{25}Al_{25}$ powders. An optimal milling and heat treatment conditions to obtain the single phase of Fe2VAl compound with fine microstructure were investigated by X-ray diffraction and differential scanning calorimetry (DSC) measurement. The $Fe_{50}V_{25}Al_{25}$ MA sample ball-milled for 60 hours exhibits a bcc ${\alpha}$-(Fe,V,Al) solid solution. Single phase of Heusler $Fe_2VAl$ compound can be obtained by MA of $Fe_{50}V_{25}Al_{25}$ mixture for 60 hours and subsequently heated up to $700^{\circ}C$. Sintering of the MA powders was performed in a spark plasma sintering (SPS) machine using graphite dies at $900{\sim}1000^{\circ}C$ under 60 MPa. The Vickers hardness of bulk sample sintered at $1000^{\circ}C$ was high value of Hv 870. All compact bodies have a high relative density above 90 % with metallic glare on the surface.

The Synthesis and Properties of Nonlinear Optical Polyquinonediimine Containing Mono-Azobenzene Group in the Side Chain (곁사슬에 모노-아조벤젠기를 갖는 비선형 광학 폴리퀴논디이민의 합성과 성질에 관한 연구)

  • 이상배;양정성;박동규
    • Polymer(Korea)
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    • v.24 no.6
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    • pp.737-743
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    • 2000
  • Polyquinonediimines (PQDI) which have stable structure on heat and contains mono-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, $^1$H-NMR, and elementary analysis. Especially, PQDI was comfirmed by the double-bonding peak of >C=N appeared near 1625 $cm^{-1}$ / by means of FT-IR spectrum. PQDI containing mono-azobenzene group in both side chains wat not soluble in non-polar solvents at all but partially soluble in the polar solvents having small dielectric constant, and dissolved in the strong acid such as sulfuric acid and $CH_3$SO$_3$H. Molecular weight distribution of PQDI measured by GPC showed 1.74. It was confirmed through X-ray diffraction analysis that the polymer was partially crystalline at the low angle region, but amorphous after heat treatment at 1$25^{\circ}C$. The glass transition temperature (T$_{g}$ ) of synthesized polymer was measured as 1$25^{\circ}C$ by differential scanning calorimetry. The SHG value for $\chi$$^{(2)}$ after poling at 1$25^{\circ}C$ was 8.6 pm/V (λ=1.542 ${\mu}{\textrm}{m}$). The SHG value slowly decreased with time from the start but appeared temporal stability after 100 hours.

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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.