• Title/Summary/Keyword: DSC measurement

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Polyesters Biosynthesis of Alcaligenes eutrophus H16(ATCC 17699) from Various Mono- and Dicarboxylic Acids and Diols

  • Song, Jae-Jun;Shin, Yong-Chul
    • Journal of Microbiology and Biotechnology
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    • v.3 no.2
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    • pp.123-128
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    • 1993
  • The polyesters (polyhydroxyalkanoates; PHAs) production capability in a two-step cultivation of Alcaligenes eutrophus H16(ATCC 17699) was investigated by using various organic carbon sources. The carbon sources used included linear $C_2~C_10$ monocarboxylic acids, $C_3~C_10$ dicarboxylic acids, crotonic acid, and several linear vicinal and $\omega$-diols. The polyesters synthesized were characterized by 500 MHz $^1 H-NMR$ spectroscopy, intrinsic viscosity$[\eta]$ measurement in chloroform and differential scanning calorimetry (DSC). The PHAs synthesis data showed that the use of C-odd ($C_3, C_5, and C_7$) monocarboxylic acids resulted in poly(3-hydroxybutyrate-co-3-hydroxyvalerate)(P(3HB-co-3HV) (3HV content ranging 40 to 70 mol%) while the use of $C_9$ substrate gave the copolyester containing only 4 mol% of 3HV. All culture products obtained on $C_3$~C$_{10}$ dicarboxylic acids gave exclusively P(3HB). 500 MHz $^1 H-NMR$ analysis showed that all polyesters synthesized generally contained 1~2 mol% 3HV even for the unrelated substrates such as the carboxylic acids with even number of carbon. When $\alpha, \omega$-diols with even number of carbon were used as substrates, 4-hydroxybutyrate(4HB) was inserted into the polyester chain composed of P(3HB-co-4HB). Vicinal diols were generally not utilized by the bacterium for polyester production.n.

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Mechanical alloying effect and structural observation of (V, Fe)-N amorphous alloy powders (기계적 합금화에 의한 (V, Fe)-N계 비정질 합금의 제조 및 구조변화)

  • 이충효;전성용;김지순
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.14 no.4
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    • pp.129-134
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    • 2004
  • In this study, we investigated the effect of a nitrogen atom on the amorphization of V-Fe alloy through solid-gas reaction during mechanical alloying (MA). MA by planetary ball mill of $V_{70}Fe_{30}$ elemental powders was carried out under the nitrogen gas atmosphere. Amorphization has been observed after 160 hours of ball milling in this case. The DSC spectrum for the mechanically alloyed ($V_{70}Fe$_{30}$)_{0.89}N_{0.11}$ powders exhibits a sharp exothermic peak due to crystallization at about $600^{\circ}C$. Structural transformation from the bcc crystalline to amorphous states was also observed through X-ray and neutron diffractions. We take a full advantage of a negligibly small scattering length of the V atom in the neutron diffraction measurement. During amorphization process the octahedral unit, which is typical of a polyhedron formed in any crystal structures, was preferentially destroyed and transformed into the tetrahedral unit. Futhermore, neutron diffraction measurements revealed that a nitrogen atom is selectively situated at a center of the polyhedron formed by V atoms.

Highly Sulfonated Poly(Arylene Biphenylsulfone Ketone) Block Copolymers Prepared via Post-Sulfonation for Proton Conducting Electrolyte Membranes

  • Lee, Kyu Ha;Chu, Ji Young;Kim, Ae Rhan;Nahm, Kee Suk;Yoo, Dong Jin
    • Bulletin of the Korean Chemical Society
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    • v.34 no.6
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    • pp.1763-1770
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    • 2013
  • A series of the block copolymers were successfully synthesized from post-sulfonated hydrophilic and hydrophobic macromers via three-step copolymerization. The degrees of sulfonation (DS) of the copolymers (10%, 30%, or 50%) were controlled by changing the molar ratio of the hydrophilic and hydrophobic parts. The resulting block copolymers were characterized by $^1H$ NMR and other technologies. The membranes were successfully cast using dimethyl sulfoxide (DMSO) solution at $100^{\circ}C$. The copolymers were characterized to confirm chemical structure by $^1H$ NMR and FT-IR. Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) demonstrated that all sulfonated block copolymers exhibited good thermal stability with an initial weight loss at temperatures above $240^{\circ}C$. The membranes showed acceptable ion exchange capacity (IEC) and water uptake values in accordance with DS. The maximum proton conductivity was 184 mS $cm^{-1}$ in block copolymer-50 at $60^{\circ}C$ and 100% relative humidity, while the conductivity of Nifion-115 was 160 mS $cm^{-1}$ under the same measurement conditions. AFM images of the block copolymer membranes showed well separated the hydrophilic and hydrophobic domains. From the observed results it is that the prepared block membranes can be considered as suitable polymer electrolyte membranes for the application of polymer electrolyte membrane fuel cells (PEMFC).

Studies on Synthesis of N,N’-Bis(diphenyl phosphoro)diaminohexane and Flame Retardancy Effects of BDPDH on PET Fabrics. (N,N’-Bis(diphenyl phosphoro)diaminohexane의 합성과 PET 직물에 대한 방염성에 관한 연구)

  • Lee, Kwang-Woo;Heo, Man-Woo;Yoon, Jong-Ho;Lee, Chang-Sub;Cho, Yong-Seok;Kim, Sam-Soo;Cho, Hwan
    • Textile Coloration and Finishing
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    • v.6 no.2
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    • pp.55-62
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    • 1994
  • The mend for fabric products has been increased remarkably with increasing population, housings, mutistory buildings,...and etc. during the last two decades. However, since fabrics are highly combustible and can produce toxic gases during the combution, fabric products can result in serious human injury as well as financial damage. Acknowledged by this, a new phosphorus based flame retardant suitable for PET fabric has been synthesized by making use of the reaction of diphenyl chloro phosphate and hexamethylenediamine. Since the starting meterials are relatively cheap and the yield of this reaction is high (more than 90%), this reaction seems to be very effective as wall as very economic. By analyzing various spectrophotometric analysis data such as NMR, FT-IR, and Mass, this new flame retardant is identified to be N,N’-Bis(diphenyl chlorophosphoro)diamino hexane. In the mean time, DSC measurement has shown that the melting point and the boiling point of this material are around 115$^{\circ}C$ and around 40$0^{\circ}C$, respectively. The flame retardancy test done on the PET fabric processed by this flame retardant have shown excellent in times of flame contact, times of flame contact for washable. The most economical finishing condition estimated 10% in concentration of BDPDH, Moreover, it has been also found that the drape stiffness of the PET fiber processed by the flame retartant is changed very litter compared to the unprocessed original PET fabrics. Judging from this, the potential of this new phosphrdus based compond as a flame retardant for PET fabric seems to be high.

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The study of thermal properties of graphene/Cu foam hybrid structures (그래핀/구리폼과 그래파이트 하이브리드 구조체의 열전도 특성 연구)

  • Kim, Hee Jin;Kim, Hyeungkeun;Kim, Yena;Lee, Woo Sung;Yoon, Dae Ho;Yang, Woo Seok
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.23 no.5
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    • pp.235-240
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    • 2013
  • Pure-carbon materials such as graphite, graphene, carbon nanotubes, and diamond have very high thermal conductivities. The reported thermal conductivity of graphene is in the range 3000~5000W/m-K at room temperature. Here, we developed graphene/cu foam hybrid type heat spreader to obtain higher thermal conductivity than Cu foam. Hybrid materials were characterized using optical microscopy (OM), scanning electron microscopy (SEM) and thermal conductivity measurement system; LFA (Laser Flash Analysis @ LFA 447, NETZSCH). We suggest that excellent thermal properties of graphene/cu foam hybrid structures are beneficial for all proposed electrical applications and can lead to a thermal management application.

Electrical conduction phenomena of $C_{22}$--quinolium(TCNQ) langmuir-blodgett films under the high-electric field ($C_{22}$-quinolium(TCNQ) LB막의 고전게 전기전도 현상)

  • 신동명;김태완;홍언식;송일식;유덕선;강도열
    • Electrical & Electronic Materials
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    • v.7 no.2
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    • pp.138-144
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    • 1994
  • Electrical conduction phenomena of $C_{22}$-quinolium(TCNQ) Langmuir- Blodgett(LB) films are reported through a study of current-voltage(I-V) characteristics along a perpendicular direction. The I-V characteristics were investigated by applying a step or a pulse voltage to the specimen as well as changing temperatures in the range of 20-250[.deg. C] It show an ohmic behavior in low-electric field, and a nonohmic behavior in high-electric field. This nonohmic behavior has been interpreted in terms of a conduction mechanism of space-charge limited current and Schottky effect. When the electric field is near the strength of 10$_{6}$ V/cm, there occur anomalous phenomena similar to breakdown. When step or pulse voltage is applied, the breakdown voltage shifts to the higher one as the step or pulse time width becomes shorter. To see the influence of temperature, current was measured as a function of temperature under the several bias voltages, which are lower than that of breakdown. It shows that the current increases to about 103 times near 60-70[.deg. C], and remains constant for a while up to around 150[.deg. C] and then suddenly drops. We have also performed a DSC(differential scanning calorimetry) measurement with $C_{22}$-quinolium(TCNQ) powder in the range of 30-300[.deg. C]. These results imply that the anomalous phenomena occuring in the high electric field are caused by the electrical and internal thermal effect such as a joule heating.ating.

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Study of Physico-Chemical Properties of N,N-Diacyl, O-Acyl Chitosan Oligomer (N,N-디아실, O-아실 키토산 올리고머의 물리화학적 특성에 관한 연구)

  • Lee, Ok-Sub;Ha, Byung-Jo;Kim, Jun-Oh;Park, Soeng-Kyu;Lee, Yoon-Sik
    • Applied Chemistry for Engineering
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    • v.8 no.3
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    • pp.365-373
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    • 1997
  • Chitosan oligomer having aldehyde group at reducing end was prepared by oxidative-deamination reaction of chitosan by using sodium nitrite, and the resulting aldehyde group was redeced to 2,5-anhydro-D-mannitol group. The obtained chitosan oligomer showed an average degree of polymerization(DP) 2 by GPC analysis. It was highly soluble in lipophilic solvents. N,N-diacyl, O-acyl chitosan oligomer was obtained trom the reaction between chitosan oligomer and acyl chloride under 4-dimethoxyaminopyridine catalyst. From DSC measurement, N,N-dilauroyl, O-lauroyl chitosan oligomer showed mesophase region, which was confirmed by polarizing microscope as thermotropic liquid crystalline state. X-ray diffraction pattern revealed that N,N-dilauroyl, O-lauroyl chitosan oligomer was highly crystalline, whereas chitosan oligomer was not.

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Crystal Structure of $KD_2PO_4$: Neutron and X-ray Diffraction Studies ($KD_2PO_4$의 결정구조: 중성자와 X-선 회절에 의한 연구)

  • 김신애;심해섭;이창희
    • Korean Journal of Crystallography
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    • v.11 no.3
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    • pp.162-166
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    • 2000
  • KD₂PO₄ single crystals were grown from D₂O with reagent KH₂PO₄ and the crystal structure was determined by X-ray and neutron diffraction methods. The crystals are tetragonal at room temperature, I42d, with lattice parameters of a=7.4633(7), c=6.9785(5) Å and Z=4. Intensity data were collected on an Enraf-nonius CAD4 diffractometer with a graphite monochromated MoK/sub α/ radiation (λ=0.7107Å) and on the neutron four circle single crystal diffractometer with Ge(331) monochromated neutron beam (λ=0.997Å). The structure was refined by full-matrix least-square to final R and wR values of 0.030 and 0.072, respectively, for 204 observed reflections with I>2σ(I) by X-ray diffraction and to final R=0.041 and wR=0.096 for 144 observed relfecdtions by neutron diffraction. The O…O distance of 2.516(4)Å obtained by X-ray diffraction is the same as that of 2.515(4)Å by neutron diffraction. On the other hand, the O-D/H distance of 0.84(4)Å by X-ray diffraction is considerably shorter than 1.029(7) Åby neutron diffraction. Hydrogen and deuterium can be readily distinguished by neutrons. In this crystal 66% of H-positions were substituted by D and the rest 34% occupied by H. The phase transition temperature of DKDP obtained with deuteration levels is f193K. This value agrees fairly well with the result of DSC measurement. The nuclear density distribution by neutron diffraction provides an observation of the disordered state of D/H in KD₂PO₄ at room temperature.

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Effects of proanthocyanidin, a crosslinking agent, on physical and biological properties of collagen hydrogel scaffold

  • Choi, Yoorina;Kim, Hee-Jin;Min, Kyung-San
    • Restorative Dentistry and Endodontics
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    • v.41 no.4
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    • pp.296-303
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    • 2016
  • Objectives: The purpose of the present study was to evaluate the effects of proanthocyanidin (PAC), a crosslinking agent, on the physical properties of a collagen hydrogel and the behavior of human periodontal ligament cells (hPDLCs) cultured in the scaffold. Materials and Methods: Viability of hPDLCs treated with PAC was measured using the 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay. The physical properties of PAC treated collagen hydrogel scaffold were evaluated by the measurement of setting time, surface roughness, and differential scanning calorimetry (DSC). The behavior of the hPDLCs in the collagen scaffold was evaluated by cell morphology observation and cell numbers counting. Results: The setting time of the collagen scaffold was shortened in the presence of PAC (p < 0.05). The surface roughness of the PAC-treated collagen was higher compared to the untreated control group (p < 0.05). The thermogram of the crosslinked collagen exhibited a higher endothermic peak compared to the uncrosslinked one. Cells in the PAC-treated collagen were observed to attach in closer proximity to one another with more cytoplasmic extensions compared to cells in the untreated control group. The number of cells cultured in the PAC-treated collagen scaffolds was significantly increased compared to the untreated control (p < 0.05). Conclusions: Our results showed that PAC enhanced the physical properties of the collagen scaffold. Furthermore, the proliferation of hPDLCs cultured in the collagen scaffold crosslinked with PAC was facilitated. Conclusively, the application of PAC to the collagen scaffold may be beneficial for engineering-based periodontal ligament regeneration in delayed replantation.

Mechanical Properties of PVC Composite Containing Iron Dust (제철 분진을 함유한 PVC 복합체 수지의 기계적 성질)

  • Nah, Jae-Woon;Kim, Myung-Yul
    • Elastomers and Composites
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    • v.33 no.5
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    • pp.370-376
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    • 1998
  • Mechanical properties of PVC[poly(vinylchloride)] composites containing the dust from blast and converter (Kwangyang Iron Co.) were investigated as a function of dust content. Tensile strength is increased, when the blast dust is mixed with PVC to the extent of 8.83wt % and impact strength is not significantly changed. From these results, it is suggested that blast dust containing CaO, SiO, MgO, $A1_2O_3$ and metallugical particle is compatible with PVC. Thermogravimetric analysis(TGA) showed that residual weight(%) at temperature $600^{\circ}C$ increased with the amount of blast dust and differential scanning calorimetry(DCS) showed that the thermal stability of PVC composite was increased when the weight ratio of blast dust was 8.83wt % X-ray diffractometry measurement also showed their blends and structures.

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