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

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안정성 개선을 위한 무기화합물과 사이클로세린 복합 입자 (Inorganic Compound and Cycloserine Composite Particles for Improved Stability)

  • 김동원;김희서;윤홍준;조혁준;진성규
    • 한국분말재료학회지
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    • 제31권2호
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    • pp.126-131
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    • 2024
  • The aim of this study was to improve the chemical stability of cycloserine containing organic and inorganic compounds. Composite particles were manufactured with a 1:1 weight ratio of organic/inorganic compounds and cycloserine. The influence of organic/inorganic compounds on the stability of cycloserine was investigated under accelerated stress conditions at 60℃/75% RH for 24 hours. In addition, the properties of the composite particles were evaluated using differential scanning calorimetry (DSC), scanning electron microscopy (SEM), and the dissolution of the drug was assessed by preparing it as a hard capsule. Among the organic and inorganic compounds investigated, calcium hydroxide most improved the stability of cycloserine under accelerated stress conditions (53.3 ± 2.2% vs 1.7 ± 0.2%). DSC results confirmed the compatibility between calcium hydroxide and the cycloserine, and SEM results confirmed that it was evenly distributed around the cycloserine. Calcium hydroxide also showed more than 90% cycloserine dissolution within 15 minutes. Therefore, the calcium hydroxide and cycloserine composite particles may be candidates for cycloserine oral pharmaceuticals with enhanced drug stability.

니켈-타이타늄 호선의 상전이 온도 범위와 상전이 행동 비교 (Comparison of transition temperature range and phase transformation behavior of nickel-titanium wires)

  • 이유현;임범순;이용근;김철위;백승학
    • 대한치과교정학회지
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    • 제40권1호
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    • pp.40-49
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    • 2010
  • 본 연구의 목적은 martensitic (M-NiTi), austenitic (A-NiTi) 및 thermodynamic nickel-titanium wire (T-NiTi)의 물리적 특징과 상전이 정도를 평가하는 것이다. 재료는 $0.016\;{\times}\;0.022$ inch의 M-NiTi (Nitinol Classic, NC), A-NiTi (Optimalloy, OPTI)와 T-NiTi (Neo-Sentalloy, NEO)이었으며, differential scanning calorimetry (DSC), 3점굽힘실험, X-ray diffraction (XRD), 미세구조 분석을 시행하였으며, ANOVA test로 통계처리하였다. DSC분석 결과 OPTI와 NEO는 heating curve에서 2개의 peak, cooling curve에서 1개의 peak를 보였고, NC는 heating과 cooling curve에서 1개의 넓고 약한 peak를 보였다. Austenite finishing ($A_f$) 온도는 OPTI $19.7^{\circ}C$, NEO $24.6^{\circ}C$, NC $52.4^{\circ}C$였다. 3점굽힘실험 결과 NC, OPTI, NEO 모두 residual deflection을 보였으며, NC와 OPTI의 load range가 NEO보다 컸다. XRD와 미세구조 분석결과 OPTI와 NEO는 Martensite finishing ($M_f$)에서 martensite와 austenite가 섞여 있음이 관찰되었다. NEO와 OPTI는 NC보다 개선된 물리적 특징과 상전이 행태를 보였다. NiTi 호선의 물리적, 온도에 따른 행태는 예상되었던 상전이 정도에 의해 완벽하게 설명되지 않았으며, 그 이유는 복잡한 martensite variants의 존재와 열과 stress에 의해 유도된 독립적인 상전이에 기인한다고 생각된다.

Sodium Stearoyl Lactylate가 아밀로펙틴과의 결합물 형성 및 밀전분의 호화와 노화에 미치는 영향 (Effect of Sodium Stearoyl Lactylate on Complex Formation with Amylopectin and on Gelatinization and Retrogradation of Wheat Starch)

  • 장재권;이윤형;이석훈;변유량
    • 한국식품과학회지
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    • 제32권3호
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    • pp.500-506
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    • 2000
  • 시차주사열량계(differential scanning calorimetry, DSC)를 사용하여 분석한 결과 밀전분으로 부터 분리한 아밀로펙틴은 밀전분의 노화특성과 일치된 특성을 나타내었다. 수분함량 8%의 아밀로펙틴과 SSL을 10 : 1의 중량 비율(w/w)로 혼합하여 DSC로 1차 가열과 냉각 후 2차 가열한 결과 $55{\sim}70^{\circ}C$의 온도범위에서 용융 peak를 나타낸 반면 SSL은 $40{\sim}55^{\circ}C$의 온도범위에서 용융 peak를 나타내어 서로 다른 융점을 나타내었다. 또한 아밀로펙틴과 SSL의 혼합물은 가열과 냉각을 반복함에 따라 결정질의 아밀로펙틴 g당 용융 peak의 엔탈피값이 증가되는 결과를 보였다. 전체 수분함량 50%에서 밀전분과 밀전분으로 부터 분리한 아밀로오스와 아밀로펙틴 각각에 대해 SSL을 5 : 1의 중량비율로 혼합하여 DSC로 1차와 2차 가열한 결과 SSL의 용융 peak 이외에 SSL과 아밀로펙틴의 결합물로 판단되는 $60-70^{\circ}C$ 범위의 가역적인 용융 peak가 관찰되었다. SSL과 아밀로펙틴 결합물은 V 도형의 아밀로오스와 지방 결합물과 차이가 있는 결정질을 나타내는 X-ray diffraction angle$(2{\theta})$ 값을 나타내었다. 전체수분함량 60%에서 SSL은 밀전분의 호화 엔탈피값을 감소시켰으며 아밀로오스와 지방결합물의 용융 엔탈피값을 증가시켰다. 동일한 전체수분함량에서 밀전분과 아밀로펙틴에 대해 SSL을 20 : 1과 10 : 1의 비율로 혼합한 겔의 저장실험은 SSL을 포함한 시료가 SSL을 포함하지 않은 시료보다 노화에 대해 억제효과를 나타내었다.

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DSC에 의한 전분의 Endothermic peak와 효소분석법에 의한 호화도 비교 (Comparison of Differential Scanning Calorimetry with Enzymatic Method for the Determination of Gelatinization Degree of Corn Starch)

  • 이부용;목철균;이철호
    • 한국식품과학회지
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    • 제25권4호
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    • pp.400-403
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    • 1993
  • Corn starch와 waxy corn starch를 시료전분으로 사용하여 수분함량 $20{\sim}80%$ 범위에서 DSC를 사용하여 얻은 흡열곡선의 엔탈피와 효소분석법으로 전분의 호화도를 측정하여, 측정방법들 사이의 차이를 비교하여 보았다. DSC로 시료전분의 엔탈피 측정시 수분함량 70%까지는 수분함량 증가에 따라 엔탈피가 비례적으로 증가하였으나 70% 이상의 수분함량에서는 엔탈피가 평형에 도달하였으며 waxy corn starch가 4.2 cal/g, corn starch가 3.23cal/g의 엔탈피를 나타내었다. 효소분석법으로 호화도를 측정하였을 때는 수분함량의 증가에 따라 80% 수분함량까지도 시료전분의 호화도가 비례적으로 증가하였다. DSC에 의한 엔탈피 변화와 효소분석법에 의한 호화도 결과를 비교하여 보면 수분함량 70% 이하에서는 서로 직선적인 비례관계를 나타내었으나, 수분함량 70% 이상의 고 수분계 전분은 DSC로 측정시 엔탈피 차이가 나지 않았으나 효소분석법으로 측정했을 때는 수분함량 80%까지도 호화도 차이가 잘 나타났다.

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Effect of enzyme treatment on the DSC and TGA behavior of silkworm powder

  • Jo, You-Young;Bae, Sung Min;Kim, HyunBok;Lee, Kwang Gill;Kweon, HaeYong
    • International Journal of Industrial Entomology and Biomaterials
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    • 제37권1호
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    • pp.29-32
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    • 2018
  • Silkworm powder's thermal property is an important factor for its storage and marketing. This study examined the effect of edible enzyme on the thermal property of silkworm powder using Thermogravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC). Results of the TGA showed that regardless of the enzyme treatment, the weight loss patterns of silkworm powders exhibited 3 step thermal property deterioration at approximately $80^{\circ}C$, $280^{\circ}C$, and $480^{\circ}C$ due to water evaporation and thermal degradation. This is similar with the DSC which also resulted in all samples two endothermic peaks attributed also to water evaporation and thermal degradation. These results indicated that the use of enzyme such as protease and cellulase might not affect significantly the thermal properties of silkworm powder.

Solid State of Tulobuterol : Characterization, Dissolution, Transformation

  • Do, Eui-Seon;Sohn, Young-Taek
    • Journal of Pharmaceutical Investigation
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    • 제41권6호
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    • pp.371-376
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    • 2011
  • The objective of this work was to investigate the existence of new crystal forms of tulobuterol which is used to prevent morning asthma attacks by ${\beta}_2$ agonist and the transformation of crystal forms. Three crystal forms of tulobuterol have been isolated by recrystallization and Form 2 was transformed to Form 4 at 52% RH and 95% RH and these four crystal forms are characterized by differential scanning calorimetry (DSC), powder X-ray diffractometry (PXRD) and thermogravimetric analysis (TG). The DSC and PXRD patterns of four crystal forms of tulobuterol were different respectively. The dissolution patterns of these three crystal forms of tulobuterol were studied and they showed significant differences in the dissolution rate. After storage of 2 months at 0% RH (silica gel, $20^{\circ}C$), 52% RH (saturated solution of $Na_2Cr_2O_7{\cdot}2H_2O/20^{\circ}C$) and 95% RH (saturated solution of $Na_2HPO_4/20^{\circ}C$), Form 1 and Form 3 were not transformed. But Form 2 was transformed to Form 4 at 52% RH and 95% RH.

PCM 소재 특성 측정 (PCM Property Measurement)

  • 이영우;조예림;박병흥
    • 융복합기술연구소 논문집
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    • 제4권2호
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    • pp.51-54
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    • 2014
  • Energy storage not only reduces the mismatch between supply and demand but also improves the performance and reliability of energy systems. The different forms of energy that can be stored, including mechanical, electrical and thermal energy. Phase change materials (PCM) are latent heat storage materials. A large number of phase change materials (organic, inorganic and eutectic) are available in any required temperature range. We concentrated on eutectic materials and made a eutectic by mixing urea and choline chloride. Heat capacity ($C_p$) is one of the most important properties to be considered when a process is developed using the eutectic and currently DSC (Differential Scanning Calorimetry) has been proved as an effective technique to measure the heat capacity. This study focused on measuring heat capacity ($C_p$) of the mixing urea and choline chloride by DSC.

Cellulase 처리가 쌀의 이화학적 특성 및 밥의 텍스쳐 특성에 미치는 영향 (The Effect of Cellulase Treatment on the Physicochemical Properties of Rice and the Texture of Cooked Rice)

  • 김영경;안승요
    • 한국식품과학회지
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    • 제28권4호
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    • pp.720-729
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    • 1996
  • 추청벼, 조생통일벼, IR 36등 세 품종의 쌀에 셀룰라제(cellulase) 처리가 팽윤력, 용해도, 아밀로그래프, differential scanning calorimetry (DSC), 가용성 탄수화물 용출 및 밥의 경도 등에 미치는 효과에 대하여 시험하였다. 효소처리에 의하여 세 품종의 쌀에서 모두 팽윤력과 용해도가 증가하였으며 아밀로그램 점도는 모두 감소하였다. 시차 주사 열량계(DSC)를 이용한 밥의 노화 시험에서는 효소 처리의 뚜렷한 효과가 없었다. 효소처리한 쌀의 가용성 탄수화물의 겔 크로마토그래피에서 분자량 10,000미만의 세포벽 분해산물이 확인되었다. Rheometer로 측정한 밥의 경도는 효소처리한 모든 품종의 쌀에서 감소하였다.

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A Study on Reaction Kinetics of PTMG/TDI Prepolymer with MOCA by Non-Isothermal DSC

  • Ahn, WonSool;Eom, Seong-Ho
    • Elastomers and Composites
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    • 제50권2호
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    • pp.92-97
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    • 2015
  • A study on reaction kinetics for a PTMG/TDI prepolymer with 2,2'-dichloro-4,4'-methylenedianiline (MOCA), of which formulations may be generally used for fabricating high performance polyurethane elastomers, was peformed using non-isothermal differential scanning calorimetry (DSC). A number of thermograms were obtained at several constant heating rates, and analysed using Flynn-Wall-Ozawa (FWO) isoconversional method for activation energy, $E_a$ and extended-Avrami equation for reaction order, n. Urea formation reaction of the present system was observed to occur through the simple exothermic reaction process in the temperature range of $100{\sim}130^{\circ}C$ for the heating rate of $3{\sim}7^{\circ}C/min$. and could be well-fitted with generalized sigmoid function. Though activation energy was nearly constant as $53.0{\pm}0.5kJ/mol$, it tended to increase a little at initial stage, but it decreases at later stage by the transformation into diffusion-controlled reaction due to the increased viscosity. Reaction order was evaluated as about 2.8, which was somewhat higher than the generally well-known $2^{nd}$ order values for the various urea reactions. Both the reaction order and reaction rate explicitly increased with temperature, which was considered as the indication of occurring the side reactions such as allophanate or biuret formation.

Cocrystallization of Poly(1,4-cyclohexylenedimethylene terephthalate-co-hexamethylene terephthalate) Copolymers

  • Jeong, Young-Gyu;Jo, Won-Ho;Lee, Sang-Cheol
    • Macromolecular Research
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    • 제12권5호
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    • pp.459-465
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    • 2004
  • We have synthesized poly(l,4-cyclohexylenedimethylene terephthalate-co-hexamethylene terephthalate) [P(CT-co-HT)] random copolymers having various comonomer contents, from 0 to 100 mol% HT, by melt-condensation and have investigated their crystallization behavior by using differential scanning calorimetry (DSC) and wide-angle X-ray diffraction (WAXD). We observed that P(CT-co-HT)s exhibit clear melting and crystallization peaks in their DSC thermograms and sharp diffraction peaks in their WAXD patterns for all of their copolymer compositions as a result of cocrystallization of the CT and HT units, even though the copolymers are statistically random copolymers. When we plotted the melting and crystallization temperatures of P(CT-co-HT)s and the d-spacings of all the reflections against the copolymer composition, we observed a eutectic point at ca. 80 mol% HT, which suggests that a crystal transition occured from a PCT-type crystal to a PHT-type crystal. Both the DSC and WAXD results support the notion that P(CT-co-HT) copolymers undergo an isodimorphic cocrystallization.