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Structural Characterization of Branched Polyesters Using TOF-SIMS Combined with Transesterification

  • Lee, Yeonhee;Seunghee Han;Yoon, Jung-Hyeon;Hyuneui Lim;Moojin Suh
    • Proceedings of the Korean Vacuum Society Conference
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    • 1999.07a
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    • pp.203-203
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    • 1999
  • Mass spectrometry technique provides the molecular weight distribution, data on the sequence of repeat units, polymer additives, and impurities, and structural information. time-of-Flight secondary Ion Mass Spectrometry (TOF-SIMS) has been used for structural characterization of various polymers1-2. the masses of repeat units and terminal groups and molecular weight distributions of polymers have been determined from their TOF-SIMS spectra. TOF-SMIS provides good sensitivity and structural specificity for high mass ions so that intact oligomers and large polymer fragments are observed. In this study, we investigated the detailed structural information on the oligomers and fragment ions of branched poly(1,3-butylene adipate) and branched poly[di(ethylene glycol) adipate] and the transesterification products of branched polyesters with trifluoroacetic acid or chloro difluoroacetic acid. Branched polyesters were chosen because they are important polymers but difficult to characterize; thus branched polyesters provide challanging test for TOF-SIMS. TOF-SIMS spectra of polyesters are obtained from thin polymer films cast from solution on a silver substrate. A good solvent for a polumer solution disrupts intermolecular forces between polymer chains but leaves the polumer intact. Transesterification reactions are potentially useful for characterization of high molecular weight and intractable polyesters. Transesterification products of polyesters and trifluoroacetic acid or an integral number of polyester repeat units and an additional diol. The progress of such reactions was monitored using peak intensities of reactants and products in TOF-SIMS spectra. The increasing abundance of tagged ions indicates that the reaction has progressed with time.

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Preparation and Properties of Eu3+ Doped Y2O3 Nanoparticles with a Solvothermal Synthesis Using the Ethylene Glycol (에틸렌 글리콜을 이용하여 용매열 합성으로 Eu3+가 도핑된 Y2O3 나노 입자의 제조 및 특성)

  • 신수철;조태환
    • Journal of the Korean Ceramic Society
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    • v.40 no.7
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    • pp.709-714
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    • 2003
  • Eu doped $Y_2$ $O_3$ nanoparticles were prepared with the solvothermal synthesis using the ethyleneglycol solvent at 20$0^{\circ}C$ for 3-5 h and then annealed in air at 1000-140$0^{\circ}C$ for 2-4 h. The X-ray diffraction pattern of annealed crystals at 100$0^{\circ}C$ for 2 h could be indexed as pure cubic cell of $Y_2$ $O_3$ phase with lattice parameters a=10.5856 $\AA$ which is very close to the reported data (JCPDS Card File, 41-1105 a=10.6041 $\AA$). Average size of prepared phosphor particles have about 100 nm, which were spherical morphology. The phosphor particle sizes decreased and the emission intensity increased at the annealing temperature. Though PL spectrum analysis, the 3% Eu doped $Y_{2-x}$ $O_3$:E $u_{x}$ $^{3+}$(x=0.06) phosphor showed the excitation spectrum at 250 nm wavelength and the maximum emission spectrum at 611 nm wavelength.

Effect of TiO2 Nanotube Length on Photocatalytic Activity with Different Light Intensities: Cr(VI) Reduction and Hydrogen Production (광량 및 TiO2 나노튜브 길이별 광활성 연구: Cr(VI)환원 및 수소제조)

  • Joo, Hyun-Ku;Shim, Eun-Jung;Lee, Jae-Min;Yoon, Jae-Kyung
    • Journal of Hydrogen and New Energy
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    • v.22 no.4
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    • pp.432-442
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    • 2011
  • Anodized tubular $TiO_2$ electrodes (ATTEs) with three noticeably different lengths are prepared to determine their optimum length for the photo-driven activity in the reaction of Cr(VI) reduction and hydrogen evolution. The ATTEs with ethylene glycol have longer $TiO_2$ tubes (7-15.6 ${\mu}m$) than those with hydrfluoric acid (0.6-0.8 ${\mu}m$). These samples, which differ only in the length of the tubes, with a wall thickness of ca. 20 nm, consist mainly of an anatase crystalline phase after heat treatment at $650^{\circ}C$, since the anatase crystallites at the tube walls do not undergo transformation into rutile phase, due to the constraints imposed by the wall thickness. Among them, the medium size (ca. 8 ${\mu}m$) tubes provide the optimum conditions, irrespective of the light intensity, which is explained in terms of the correlation between the amount of photons and the adsorbed electron acceptors and their location. Photocatalytic Cr(VI) reduction leads to ca. 60% reduction of Cr(VI) even under 1 sun irradiation with the medium-sized anodized $TiO_2$ tubes, but only ca. 20% with the short- and long-sized tubes. For hydrogen evolution, tubes longer than 8 ${\mu}m$ do not exhibit better performance with any light intensity.

Effect of ultrasonic waves on anti-freezing for plate-type heat exchanger (평판형 열교환기에서의 제빙억제를 위한 초음파의 영향)

  • Cho, Ki-Ryang;Choi, Kwang-Il;Kim, On;Park, Ki-won
    • Journal of Advanced Marine Engineering and Technology
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    • v.41 no.3
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    • pp.176-181
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    • 2017
  • This study attempted to examine a method of anti-freezing on a plate-type heat exchanger in a low-temperature environment. Freezing condition was observed after ultrasonic waves were generated. Data were recorded to determine the optimal conditions for freezing. Ethylene glycol, which is commonly used in antifreeze formulations, was used as the brine, and the temperature was varied between -8 and $-16^{\circ}C$. The water for freezing provided by the thickness of 1-3 mm. In addition, experiments were conducted by adjusting the output to identify the changes that occurred due to the incidence of ultrasonic energy. The results of the anti-freezing effect were brine temperature, freezing thickness, and frequency band of ultrasonic waves.

Fabrication and NOx Gas Sensing Properties of LaMeO3 (Me = Cr, Co) by Polymeric Precursor Method (Polymeric Precursor법에 의한 LaMeO3 (Me = Cr, Co)의 제조 및 NOx 가스 검지 특성)

  • Lee, Young-Sung;Shimizu, Y.;Song, Jeong-Hwan
    • Korean Journal of Materials Research
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    • v.21 no.8
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    • pp.468-475
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    • 2011
  • [ $LaMeO_3$ ](Me = Cr, Co) powders were prepared using the polymeric precursor method. The effects of the chelating agent and the polymeric additive on the synthesis of the $LaMeO_3$ perovskite were studied. The samples were synthesized using ethylene glycol (EG) as the solvent, acetyl acetone (AcAc) as the chelating agent, and polyvinylpyrrolidone (PVP) as the polymer additive. The thermal decomposition behavior of the precursor powder was characterized using a thermal analysis (TG-DTA). The crystallization and particle sizes of the $LaMeO_3$ powders were investigated via powder X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and particle size analyzer, respectively. The as-prepared precursor primarily has $LaMeO_3$ at the optimum condition, i.e. for a molar ratio of both metal-source (a : a) : EG (80a : 80a) : AcAc (8a) inclusive of 1 wt% PVP. When the as-prepared precursor was calcined at $700^{\circ}C$, only a single phase was observed to correspond with the orthorhombic structure of $LaCrO_3$ and the rhombohedral structure of $LaCoO_3$. A solid-electrolyte impedance-metric sensor device composed of $Li_{1.5}Al_{0.5}Ti_{1.5}(PO_4)_3$ as a transducer and $LaMeO_3$ as a receptor has been systematically investigated for the detection of NOx in the range of 20 to 250 ppm at $400^{\circ}C$. The sensor responses were able to divide the component between resistance and capacitance. The impedance-metric sensor for the NO showed higher sensitivity compared with $NO_2$. The responses of the impedance-metric sensor device showed dependence on each value of the NOx concentration.

Hydrothermal Synthesis of Smectite from Zeolite (제올라이트로부터 스멕타이트 수열 합성에 대한 연구)

  • Chae, Soo-Chun;Kim, You-Dong;Jang, Young-Nam;Bae, In-Kook;Ryu, Kyung-Won;Lee, Sung-Ki
    • Journal of the Mineralogical Society of Korea
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    • v.19 no.4 s.50
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    • pp.301-310
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    • 2006
  • Smectites were synthesized from Na-P type and Na-A type zeolites by the hydrothermal synthetic method, and their physicochemical properties were studied. The optimal synthetic conditions for producing smectite were $290^{\circ}C$, 72 hr and $75{\sim}100kgf/cm^2$ in autogenous pressure. pHs of initial reaction solutions for the synthesis of smectites from Na-P type and Na-A type zeolite s were pH 6 and pH 10, respectively. The synthetic smectite was confirmed as $12{\AA}$-beidellite by a series of analysis such as X-ray diffraction analysis with random and oriented mounts, ethylene glycol treatment, and Greene-Kelly test, and their several physicochemical properties were studied.

Electrochemical Deposition of Copper on Polymer Fibers

  • Lim, Seung-Lin;Kim, Jaecheon;Park, Jongdeok;Kim, Sohee;Lee, Jae-Joon
    • Journal of Electrochemical Science and Technology
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    • v.7 no.2
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    • pp.132-138
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    • 2016
  • In this study, we report the fabrication of functional complex fibers, which have been studied widely globally for numerous applications. Here, we fabricated conductive complex fibers with antibacterial properties by coating metal ions on the surface of plastic (polypropylene) fibers using the electroless and electrochemical deposition. First, we polished the polypropylene melt-blown fiber surface and obtained an absorbing Pd seed layer on its surface. Subsequently, we substituted the Pd with Cu. Bis-3-sulfopropyl-disulfide disodium salt (SPS), polyethylene glycol (PEG), and ethylene thiourea (ETU) were used as the brightener, carrier, and leveler, respectively for the electroplating. We focused on most achieving the stable plating condition to remove dendrites, which are normally during electroplating metals so that smooth layer is formed on the fiber surface. The higher the amount of SPS, the higher was the extent of irregular plate-like growth. Many irregularities in the form of round spheres were observed with increase in the amount of PEG and ETU. Hence, when the additives were used separately, a uniform coating could not be obtained. A stable coating was obtained when the three additives were combined and a uniform 5-9 μm thick copper layer with a stable morphology could be obtained around the fiber. We believe that our results can be applied widely to obtain conductive fibers with antibacterial properties and are useful in aiding research on conductive lightweight composite fibers for application in information technology and robotics.

Expression and Localization of Heat Shock Protein 70 in Frozen-thawed IVF and Nuclear Transferred Bovine Embryos

  • Chung, K.S.;Choi, Y.J.;Song, S.J.;Do, J.T.;Yoon, B.S.;Kim, Y.J.;Lee, H.T.
    • Korean Journal of Animal Reproduction
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    • v.26 no.4
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    • pp.311-320
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    • 2002
  • The objective of this study was to assess the developmental potential in vitro produced embryos frozen-thawed with the various containers, and also examined expression and localization of heat shock protein 70 at these embryos. For the vitrification, 2-cell, 8-cell and blastocyst stage embryos produced by in vitro fertilization (IVF) and nuclear transfer (NT) were exposed the ethylene glycol 5.5 M freezing solution (EC 5.5) for 30 sec, loaded on each containers such EM grid, straw and cryo-loop, and then immediately plunged into liquid nitrogen. Thawed embryos were serially diluted in sucrose solution, each for 1 min. and cultured in CRI-aa medium. Survival rates of the vitrification production were assessed by re-expanded, hatched blastocysts. There were no differences in the survival rates of IVF using EM grid and cryo-loop. However, survival rates by straw were relatively lower than other containers. The use of cryo-loop resulted in only survival of nuclear transferred embryos (43.7%). Also, there embryos after IVF or NT were analysed by semi-quantitive reverse transcription-polymerase chain reaction (RT- PCR) methods for hsp 70 mRNA expression. Results revealed the expression of hsp 70 mRNh were higher thawed embryos than control embryos. Immunocytochemistry used to localize the hsp 70 protein in embryos. Two and 8-cell embryos derived under control condition was evenly distributed in the cytoplasm but appeared as aggregates in some frozen-thawed embryos. However, in the control, blastocysts displayed aggregate signal while Hsp70 in frozen-thawed blastocysts appeared to be more uniform In distribution. Therefore, this result suggests that the exploiting Hsp 70 in the early embryos may be role for protection of stress condition for increase viability of embryos within IVF, NT and there frozen-thawed embryos.

Experimental Study on Heat Transfer Characteristics of Ice Slurry at Direct Transportation Loop (직접 수송 루프에서 아이스슬러리의 열전달 특성에 관한 실험적 연구)

  • Lee, Dong-Won;Kim, Jeong-Bae
    • Journal of Energy Engineering
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    • v.19 no.4
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    • pp.234-239
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    • 2010
  • Heat transfer characteristics were experimentally investigated for ice slurry which was made from 6.5% ethylene glycol-water solution flowing in the circular pipe. The test section was made of a copper tube of 13.84 mm inner diameter and 1,500 mm length. The ice slurry was heated by passing hot water through an annulus surrounding the test section. The ice packing factor(IPF) and the mass flux of the experiments were varied from 0 to 25% and from 1,000 to 3,000 kg/$m^2s$ respectively at a fixed hot water temperature and flow rate. The measured heat transfer rates increase with the mass flow rate and IPF; however the effect of IPF appears to be minor at high mass flow rate. At the low mass flow rate condition, a sharp increases in the heat transfer coefficient was observed when the IPF was above 15 ~ 20%. And finally the measured heat transfer coefficients were compared with those calculated from the correlations.

The Comparison of Survival Rates of Vitrified Mouse Blastocysts in Various Vitrification Solutions and Apparatuses (다양한 유리화 용액과 동결기구에서 유리 동결 생쥐 포배기 배아의 생존율 비교)

  • Cho, Dong-Hyu;Lee, Ky-Sook;Rheu, Chul-Hee;Kwon, Jung-Kee;Lee, Jeong-Heon
    • Journal of Veterinary Clinics
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    • v.29 no.1
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    • pp.27-32
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    • 2012
  • The purpose of this study was to evaluate survival rates of vitrified mouse blastocysts in various vitrification solutions (cryoprotectants) and apparatuses. The mouse blastocysts were harvested from culture of mouse 2 cell embryo and were divided into three group (i) untreated (control); (ii) exposed to cryoprotectant agents; or (iii) cryopreserved by various vitrification apparatuses. Vitrification solutions are 40% ethylene glycol (EG) + 5.8 mg/mL ficoll + 0.5M sucrose (EFS solution), 3M glycerol + 3M EG (ES solution), 20% EG + 20% dimethyl sulfoxide (ED solution), 3M EG + 1.0 m sucrose (ES solution). Vitrification apparatuses consisted of 5 groups ; closed plastic straw (CPS), electron microscope (EM) grid, cryoloop, open pulled straw (OPS), and glass micropippete in plastic straw (GPS). The survival rates of control were 88.0%. The survival rates of exposed blastocysts in EFS, GE, ED, and ES solutions were 70.8%, 43.5% (P<0.01), 83.3% and 65.2%, respectively. The survival rates of vitrified blastocysts in CPS, EM grid, cryoloop, OPS and GPS were 56.5% (P< 0.01), 72.7%, 83.3%, 60.9% (P<0.05) and 54.2% (P<0.01), respectively. Among the vitrification solutions, the highest survival rate was seen in blastocysts vitrified in EG + DMSO (83.3%). The survival rate was not significantly different from that of the control (88%). Blastocysts cryopreserved with glycerol in all groups had an overall low survival rate of 43.5%. Survival rate of mouse blastocysts between vitrification apparatuses showed higher in cryoloop.