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

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Understanding the Mechanism of Indomethacin-Saccharin Co-crystal Formation Using In-line Monitoring System based on PVM and FBRM (PVM 및 FBRM 기반 인라인 모니터링을 통한 indomethacin-saccharin 공결정의 생성 메커니즘이해)

  • Kim, Paul;Cho, Min-Yong;Choi, Guang J.
    • Korean Chemical Engineering Research
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    • v.55 no.2
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    • pp.180-189
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    • 2017
  • Pharmaceutical co-crystals primarily to improve the solubility as well as stability of insoluble drug are to be investigated more intensively for IMDs as US FDA has reclassified co-crystal as a special case of solvates in August this year. In this study, we proposed a mechanism of indomethacin-saccharin co-crystal formation and the creation of transient indomethacin meta-stable form using in-line monitoring tools with the addition rate of anti-solvent as a critical process parameter. Among various instruments, we combined PVM (particle vision measurement) and FBRM (focused beam reflectance measurement) for the in-line monitoring of anti-solvent co-crystallization process. The off-line characterization of resulting powders was carried out employing the PXRD (powder x-ray diffraction) and DSC (differential scanning calorimeter). It was observed that the pathway to the final IMC-SAC co-crystal was significantly dependent upon the anti-solvent addition rate. The process conditions to obtain high quality co-crystal powder effectively were established. Consequently, we concluded that in-line monitoring combing the PVM and FBRM should be useful for the in-line monitoring of pharmaceutical co-crystallization processes.

Thermal and Mechanical Properties of Epoxy Composition Containing Modified Halosite Nanotubes with Silane Coupling Agent (실란 커플링제를 이용하여 개질한 할로이사이트 나노튜브가 함유된 에폭시 조성물의 열적·기계적 물성)

  • Kim, TaeHee;Lim, Choong-Sun;Kim, Jin Chul;Seo, Bongkuk
    • Journal of Adhesion and Interface
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    • v.18 no.2
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    • pp.68-74
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    • 2017
  • Epoxy resins are widely used in various fields due to their excellent thermal, mechanical and chemical properties. In order to improve the mechanical properties of the epoxy composition after curing, various materials are mixed in the epoxy resin. Among the nano materials, CNT is the most widely used. However, CNT has limitations in terms of manufacturing process and manufacturing cost. Therefore, there is a growing interest in naturally occurring HNTs having similar structure to that of CNT. In this study, the thermal and mechanical properties of epoxy compositions containing HNTs treated with two types of silane compounds were investigated. The mechanical properties of silane-treated HNT were measured by using a universal testing machine. The differential scanning calorimeter (DSC), thermogravimetric analysis (TGA), and thermomechanical analysis (TMA) were used to measure thermal properties. As a result of the above tests, when the HNT was surface-treated with aminosilane, the tensile strength of the epoxy composition containing the HNT was higher than that of the epoxy composition containing epoxy silane treated HNT. The linear thermal expansion coefficients (CTE) obtained from the thermomechanical analysis of the two epoxy compositions for the comparison of dimensional stability showed that the HNT composition treated with aminosilane showed a lower value of CTE than that of epoxy composition including the pristine HNT.

Study on the Thermal Decomposition Characteristics of the Tert-butylperoxymaleate using the DSC (DSC를 이용한 터셔리부틸퍼옥시말레이트의 열분해특성에 관한 연구)

  • Lee, Jung-Suk;Choi, Yi-Rac;Han, Ou-Sup
    • Journal of the Korean Institute of Gas
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    • v.24 no.3
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    • pp.40-46
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    • 2020
  • Tertbutylperoxymaleate is the one of the organic peroxides used as a raw material of initiator formulations of artificial marble manufacturing. In this study, the thermal decomposition characteristic of TBPM was evaluated using the differential scanning calorimeter in the air and nitrogen circumstance. Regardless of the reaction atmosphere, TBPM showed the exothermic peak due to the drastic decomposition reaction below 130 ℃. The activation energy estimated by dynamic methods had a range of 203~217 kJ/mol and that estimated by model-free analysis method had a range of 118~232 kJ/mol with a thermal conversion. And the ADT24, the temperature that lead to the maximum heating rate within 24 hours, was evaluated as (80~95) ℃ using the estimated activation energy.

Improved Dissolution of Solid Dispersed Atorvastatin Using Spray-Dryer (분무건조기를 이용한 아토르바스타틴 고체분산체의 용출율 개선)

  • Lee, Jun-Hee;Kim, Dae-Sung;Kim, Won;Park, Jong-Hak;Ahn, Sik-Il;Kim, Yun-Tae;Rhee, John-M.;Khang, Gil-Son
    • Journal of Pharmaceutical Investigation
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    • v.38 no.4
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    • pp.249-254
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    • 2008
  • Solid dispersions of poorly water-soluble drug, atorvastatin, were prepared with Eudragit L100 to improve the solubility by spray dryer. To investigate the correlation between physicochemical properties and dissolution rate of solid dispersions, the samples were characterized by scanning electron microscopy (SEM), differential scanning calorimeter (DSC) and fourier transform infrared spectroscopy (FT-IR). SEM and DSC were found that atorvastatin is amorphous in the Eudragit L100 solid dispersion. FT-IR was used to analyze the salt formation by interaction between atorvastatin and Eudragit L100. The dissolution rate of solid dispersed atorvastatin was markedly increased compared to drug powder in stimulated intestinal juice (pH 6.8). Thus, the solid dispersed atorvastatin using the spray drying method with Eudragit L100 may be effective for the bioavailability.

On the In situ Composites Containing TLCP Polymerized in PMMA Solution (PMMA 용액에서 중합된 TLCP in situ 복합재료에 관한 연구)

  • Kim, Sung-Kug;Yun, Doo-Soo;Choi, Soo-Kyung;Bang, Moon-Soo;Choi, Jae-Kon;Jo, Byung-Wook
    • Applied Chemistry for Engineering
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    • v.10 no.1
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    • pp.148-153
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    • 1999
  • In situ composites containing a thermotropic liquid crystalline polymer were prepared by polycondensation of 1,4-bis(p-hydroxy-benzoyloxy)butane with 2-bromoterephthaloyl chloride in a poly(methyl methacrylate) solution. Morphology and mechanical, thermal properties of the composites were examined by differential scanning calorimeter(DSC), dynamic mechanical thermal analyser(DMTA), optical microscope and scanning electron microscope(SEM). The TLCP domains showed nematic phase. The glass transition temperature($T_g$) and mechanical properties of the PMMA in the composites increased with increasing the content of TLCP. The TLCP domains were finely dispersed in the PMMA matrix. The 20 wt % TLCP/PMMA composite prepared by in situ polymerization showed more improved mechanical property with finely well dispersed morphology compared with that prepared by solution blending of the same composition.

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Effect of Particle Size of HPMC on Dissolution Rate of Venlafaxine HCl and Carbamazepine Sustained Release Tablet (HPMC의 입도에 따른 염산벤라팍신 및 카바마제핀 서방성 정제의 용출 특성)

  • Cha, Jae-Uk;Cha, Ja-Hyun;Hong, Jun-Kee;Lee, Sung-Wan;Ko, Won-Hwa;Beak, Hyun-Ho
    • Polymer(Korea)
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    • v.36 no.3
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    • pp.332-337
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    • 2012
  • The primary objective of this work is to find the properties of sustained release dissolution pattern depending on solubility of drugs, so venlafaxine HCl and carbamazepine tablets were made by using polymer wich various particle size. Hydroxy propyl methyl cellulose (HPMC) has been utilized in this study as an excipient that is one of the most widely used polymers for an oral sustained release formulation, and drug release pattern was strongly influenced by swelling rate depending on particle size of HPMC. Scanning electron microscope (SEM) was employed to investigate the surface of tablets with various HPMC particle size, and differential scanning calorimeter (DSC) was employed to investigate the crystallization of drugs in tablets. The release model equation was applied to analyze the main mechanism of drug release pattern. The results demonstrate that drug release pattern is controlled by the drug solubility and HPMC particle size.

Preparation and Characterization of Calcium Alginate Microcapsules by Emulsification-Internal Gelation (에멀션-내부 젤화에 의한 알긴산 칼슘 마이크로캡슐의 제조 및 특성)

  • Park Soo-jin;Kang Jin-Young
    • Polymer(Korea)
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    • v.29 no.4
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    • pp.369-374
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    • 2005
  • In this work, the calcium alginate microcapsules containing lemon oil were prepared by emulsification-internal gelation and their potential use as aromatherapy was examined by the controlled release system. The lemon oil encapsulated in the alginate was successfully observed by Fourier transform (FT-IR) spectroscopy and differential scanning calorimeter (DSC) measurements. Analysis of the diameters and shapes of microcapsules was conducted by scanning electron microscopy (SEM). The mean diameters ranging from 4 to 7 um and encapsulation yield ranging from 50 to $85\%$ were obtained. The controlled release of the lemon oil at $37^{circ}$ was demonstrated by the infrared moisture determination (IMDB). It was found that the amount of released lemon oil decreased with increasing concentrations of alginate and $CaCl_2$ due to the higher the cross-linking density of the capsules prepared. The oil release from the capsule was measured as a function of physical force. We confirmed that the external factor could control the collapse of capsule wall and the release rate.

Synthesis and Characterization of Transparent Copolyimide Films (I) (투명한 폴리이미드 공중합체 필름의 합성과 특성 연구 (I))

  • Park, Jong-Su;Chang, Jin-Hae
    • Polymer(Korea)
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    • v.32 no.6
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    • pp.580-586
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    • 2008
  • Copolyimides were synthesized from 4,4'-(hexafluoroisopropylidene)diphthalic anhydride (6FDA) and 1,3-bis(3-aminophenoxy)benzene (BAPB) with different mole ratios of 2,2-bis[4-(4-aminophenoxy)pheny1]hexafluoropropane (BAPP). The solution cast film of poly(amic acid) (PAA) was heat treated at different temperatures to create copolyimide films. The PI copolymer films were found to exhibit good optical transparencies. The thermomechanical properties, morphology, and optical transparency of PI films were examined using fourier transform infrared spectroscopy (FT-IR), wide-angle X-ray diffraction (XRD), scanning electron microscopes (SEM), differential scanning calorimeter(DSC), thermo-gravimetric analyzer (TGA), universal tensile machine (UTM), and IN - Vis. spectrometer. The glass transition temperature ($T_g$), ultimate strength, and initial modulus linearly increased with increasing BAPP mole fraction. However, thermal stability($T_D{^i}$) of the copolyimide remains constant regardless of BAPP loadings. It was found, however, that the optical transparency decreases slightly upon increasing the BAPP content because of the formation of the charge transfer complexes.

Morphology, Thermal and Mechanical Properties of Poly(lactic acid)/Poly(butylene adipate-co-terephthalate)/CMPS Blends (Poly(lactic acid)/Poly(butylene adipate-co-terephthalate)/CMPS 블렌드의 형태학, 열적 및 기계적 특성)

  • Kang, Kyoung-Soo;Kim, Bong-Shik;Jang, Woo-Yeul;Shin, Boo-Young
    • Polymer(Korea)
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    • v.33 no.2
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    • pp.164-168
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    • 2009
  • The effects of chemically modified thermoplastic starch (CMPS) on the morphology, thermal and mechanical properties of the blends of poly (lactic acid)(PLA) and poly(butylene adipate-co-terephthalate)(PBAT) were studied. Blends of PLA/PBAT with the CMPS contents of 10, 20 and 30 wt% on the basis of PLA/PBAT weight were prepared by a twin screw extruder. The morphology, thermal and mechanical properties of the blends were examined by using scanning electron microscope (SEM), differential scanning calorimeter (DSC) and a tensile tester. The DSC study revealed that PLA/PBAT blends are thermodynamically immiscible, while the compatibility was much improved by addition of the CMPS.

Fatty Acids, Amino Acids and Thermal Properties of Specialty Rice Cultivars (특수미 품종의 지방산과 아미노산 조성 및 열적 특성)

  • Choi, In-Duck
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.39 no.9
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    • pp.1405-1409
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    • 2010
  • The compositions of fatty acid and amino acid of specialty rice which includes colored rice (Heugjinju, Jeugjinju, Josangheugchalbyeo), flavored rice (Heughyangmi, Hyangmi1), and giant embryo rice (Keunnun) were determined and compared to those of regular rice (Ilpumbyeo, Whaseonchalbyeo). Major fatty acids were linoleic acid (C18:2) and oleic acid (C18:1), which were composed of 75~80% of total fatty acids. Major amino acids were glutamic acid and aspartic acid in most cultivars but Jeugjinju in which cysteine (169.61 nmol) and GABA (129.32 nmol) were the most abundant amino acids. Thermal properties measured by differential scanning calorimeter (DSC) revealed that the enthalpy (${\Delta}H$) for starch gelatinization was the highest in Josangheugchalbyeo and Whaseonchalbyeo. It suggests that the starch structure of waxy rice could be more crystallized compared to non-waxy rice, and also that amylopectin could have more impact on starch gelatinization than amylose. The on-set and complete temperature for starch gelatinization were higher in colored rice of Heugjinju and Jeugjinju, and regular rice of Whateonchalbyeo.