• Title/Summary/Keyword: Temperature variation H NMR

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($^{11}$B NMR study of vortex dynamics in LuNi$_2$B$_2$C

  • Lee, K.H.;Seo, S.W.;Kim, D.H.;Khang, K.H.;Seo, H.S.;Hwang, C.S.;Cho, B.K.;Lee, Moo-Hee
    • 한국초전도학회:학술대회논문집
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    • v.10
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    • pp.107-110
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    • 2000
  • ($^{11}$B NMR measurements have been performed on single crystals of LuNi$_2$B$_2$C superconductor to investigate vortex lattice structures and dynamical behavior. The spectrum in the superconducting state is significantly broadened by local field inhomogeneity due to the vortex lattice and the peak point of the spectrum shifts toward low magnetic field due to the imperfect field penetration. The linewidth of the spectrum reflecting local field variation is much smaller than expected for conventional vortex lattices and shows peculiar increase at low temperature. Furthermore, the transverse relaxation rate, 1/T$_2$, probing the slow motion of vortices, exhibits a single peak as temperature decreases. These prominent results highlight significant fluctuation of vortices even for this low T$_c$, and nearly isotropic 3D superconductor.

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Quantitative Analysis of t-Cinnamaldehyde of Cinnamomum cassia by $^1H-NMR$ Spectrometry ($^1H-NMR$을 이용한 계피의 t-cinnamaldehyde 정량분석)

  • Song, Myoung-Chong;Yoo, Jong-Su;Baek, Nam-In
    • Applied Biological Chemistry
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    • v.48 no.3
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    • pp.267-272
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    • 2005
  • trans-Cinnamaldehyde, a major component of Cinnamomum cassia, was quantitatively analyzed using the $^1H-NMR$ spectrometry. Applicability of this method was confirmed through observing the variation of chemical shift in the $^1H-NMR$ spectrum of t-cinnamaldehyde and the integration value according to various sample concentrations or running temperatures. When the $^1H-NMR$ spectrometry was run for t-cinnamaldehyde (7.1429 mg/ml) at 19, 25, 30, 40 and $50^{\circ}C$, the chemical shifts of the doublet methine signal due to an aldehyde group were observed at 9.7202, 9.7184, 9.7169, 9.7142 and 9.7124 ppm, respectively, to imply that the running temperature had no significant variation in the chemical shift of the signal. The integration values of the signal were $1.37\;(19^{\circ}C),\;1.37\;(25^{\circ}C),\;1.37\;(30^{\circ}C),\;1.37(40^{\circ}C)$ and $1.37(50^{\circ}C)$, respectively, to also indicate running temperature gave no effect on the integration value. When the sample solutions with various concentrations such as 0.4464, 0.8929, 1.7857, 3.5714, 7.1429 and 14.286 mg/ml were respectively measured for the $^1H-NMR$ at $25^{\circ}C$, the chemical shifts of the aldehyde group were observed at 9.7206, 9.7201, 9.7196, 9.7192, 9.7185 and 9.7174 ppm. Even though the signal was slightly shifted to the high field in proportion to the increase of sample concentration, the alteration was not significant enough to applicate this method. The calibration curve for integration values of the doublet methine signal due to the aldehyde group vs the sample concentration was linear and showed very high regression rate ($r^2=1.0000$). Meantime, the $^1H-NMR$ spectra (7.1429 mg/ml $CDCl_3,\;25^{\circ}C$) of t-cinnamaldehyde and t-2-methoxycinnamaldehyde, another constituent of Cinnamomum cassia, showed the chemical shifts of the aldehyde group as ${\delta}_H$ 9.7174 (9.7078, 9.7270) for the former compound and ${\delta}_H$ 9.6936 (9.6839, 9.7032) for the latter one. The difference of the chemical shift between two compounds was big enough to be distinguished using the NMR spectrometer with 0.45 Hz of resolution. The contents of cinnamaldehyde in Cinnamomum cassia, which were respectively extracted with n-hexane, $CHCl_3$, and EtOAc, were determiend as 94.2 \;mg/g (0.94%), 137.6 mg/g (1.38%) and 140.1 mg/g(1.40%) t-cinnamaldehyde in each extract, respectively, by using the above method.

Hyperpolarized 129 NMR Study of TiO2 Nanotubes

  • Lee, Sang-Man;Lee, Soon-Chang;Mehrotra, Vandana;Kim, Hae-Jin;Lee, Hee-Cheon
    • Bulletin of the Korean Chemical Society
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    • v.33 no.2
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    • pp.511-514
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    • 2012
  • A continuous flow hyperpolarized (HP) $^{129}Xe$ NMR spectroscopy was employed for the first time to investigate $TiO_2$ nanotubes (Ti-NTs) synthesized from commercial nanoparticles with different reaction times. A single peak attributing to channels for Ti-NTs was observed for variable temperature HP $^{129}Xe$ NMR spectra. It was also noted that there is alteration in value for heat of adsorption, ${\Delta}H$ from $12.6{\pm}1.3$ to $16.4{\pm}0.4kJ/mol$ and variation in chemical shift of the xenon adsorbed in channels, ${\delta}_s$ from $120{\pm}2\sim135{\pm}9ppm$ which were closely correlated to channel length and it was shown that P25-24 Ti-NTs with longest channel is most favorite Ti-NTs for Xe adsorption.

Electrical Breakdown Properties of Insulating Oils for oil-immersed transformer (유입변압기용 절연유의 절연파괴특성)

  • 이인성;신현택;이종필;이수원;홍진웅
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2001.11a
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    • pp.605-608
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    • 2001
  • With the intention of investigating the breakdown properties of oil-immersed transformer oils in temperature range of 20∼100[$^{\circ}C$], we are made researches AC breakdown in the gap of 500∼2,500[$\mu\textrm{m}$]. The classification for the physical properties of oil for oil-immersed transformer by FTH and $^1$H-NMR experiments was confirmed to type of mineral oils. As the dependance of breakdown properties due to electrode gap length variation, breakdown voltage was found increasing according to the increase of gap, while dielectric strength was decreasing. As a result the characteristics for AC breakdown, It goes to prove that the breakdown voltage was increased to 90[$^{\circ}C$] but decreased over 90[$^{\circ}C$] in the temperature range. Also, breakdown voltage was found increasing in the increase of gap and the rising of temperature according to Weibull distribution.

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Electrical Breakdown Properties of Insulating Oils for oil-immersed transformer (유입변압기용 절연유의 절연파괴특성)

  • Lee, I.S.;Shin, H.T.;Lee, J.P.;Lee, S.W.;Hong, J.W.
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2001.11b
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    • pp.605-608
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    • 2001
  • With the intention of investigating the breakdown properties of oil-immersed transformer oils in temperature range of $20\sim100[^{\circ}C]$, we are made researches AC breakdown in the gap of $500\sim2500[{\mu}m]$. The classification for the physical properties of oil for oil-immersed transformer by FTIR and H-NMR experiments was confirmed to type of mineral oils. As the dependance of breakdown properties due to electrode gap length variation, breakdown voltage was found increasing according to the increase of gap, while dielectric strength was decreasing. As a result the characteristics for AC breakdown, It goes to prove that the breakdown voltage was increased to $90[^{\circ}C]$ but decreased over $90[^{\circ}C]$ in the temperature range. Also, breakdown voltage was found increasing in the increase of gap and the rising of temperature according to Weibull distribution.

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Synthesis of Alkoxy Modified Silicone Using Alkali Catalyst

  • Lee, Kangseok;Shim, Sang Eun
    • Elastomers and Composites
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    • v.51 no.2
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    • pp.99-105
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    • 2016
  • Alkoxy modified silicone (PAMS) was synthesized from hydroxyl-terminated polydimethylsiloxane (OH-PDMS) and vinyltrimethoxysilane (VTMO) under alkali catalyst (NaOH and KOH) at room temperature ($25^{\circ}C$) via condensation polymerization. Then, the structural verification of the synthesized PAMS was confirmed using $^1H$-NMR and FT-IR spectroscopy. The reaction rate of PAMSs was studied in terms of the concentration variation of alkali catalyst. The reaction rate increased with the concentration of alkali catalyst, but no correlation between conversion and concentration of alkali catalyst was observed.

Spectrophotometric Determination of Phenothiazine Derivatives by using Picric acid as Electron Acceptor (Picric acid를 전자수용체로 한 Phenothiazine계 화합물의 정량법)

  • 옥치완;신태용
    • YAKHAK HOEJI
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    • v.31 no.5
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    • pp.322-329
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    • 1987
  • A rapid and sensitive spectrophotometric method has been developed for quantitation of some phenothiazine derivatives (PTZDS). The method depends on the formation of insoluble yellow complexes between PTZDS and picric acid (PCA) in aqueous layer. These complexes are quantitatively extracted from aqueous phase into chloroform. The binding ratio of PTZDS-PCA complexes were presumed as PTZDS-1 to PCA-1 by means of mole ratio and continuous variation methods. The complexes are stable for more than 24hours in chloroform layer at room temperature. Most of compounds associated with pharmaceutical preparation of PTZDS do not interfere with this method. However, chlorpheniramine and diphenhydramine interfere with the riaethod. The binding state of PTZDS-PCA complexes were presumed by IR and $^1$H-NMR spectra as intermolecular hydrogen bonding.

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Suspension Polymerization and Characterization of Transparent Poly(methyl methacrylate-co-isobornyl methacrylate)

  • Park, Sung-Il;Lee, Sang-In;Hong, Soon-Jik;Cho, Kuk-Young
    • Macromolecular Research
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    • v.15 no.5
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    • pp.418-423
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    • 2007
  • A methacrylate copolymer based on isobornyl methacrylate (IBMA) and methyl methacrylate (MMA) was synthesized in an aqueous suspension via free-radical polymerization. The potential of this copolymer as a heat-resistant optical polymer is also discussed. 1,1,3,3-tetramethylbutyl peroxy-2-ethyl hexanoate and n-octyl mercaptan were used as the initiator and chain transfer agents, respectively. The effect of IBMA on the properties of the copolymer was investigated. The composition of the copolymer was analyzed using $^1H-NMR$, and the heat resistance by measuring the glass transition temperature, which exhibited a linear dependency on the IBMA content in the copolymer. Variation of the chain transfer content used in the synthesis step was effective for the optimization of the copolymer for practical use.

Study of Complex Formation of Dioxouranium(VI) Ion with Nitrate Ion by 17O NMR Spectroscopy (산소-17 핵자기공명분광법을 이용한 디옥소우라늄(VI) 이온의 질산 이온과의 착물형성에 관한 연구)

  • Jung, Woo-Sik
    • Applied Chemistry for Engineering
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    • v.3 no.2
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    • pp.312-317
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    • 1992
  • The interaction of dioxouranium(VI) (uranyl) ion with nitrate ion has been studied by $^{17}O$ NMR spectroscopy. The $^{17}O$ resonance of uranyl oxygen atoms(uranyl oxygens hereafter) of $UO_2NO_3{^+}$ was at lower field than that of uranyl ion. The stability constants of $UO_2NO_3{^+}$ were obtained from the variation of $^{17}O$ chemical shifts with nitrate-ion concentration at 5, 15, 25, $35^{\circ}C$ and depend on the ionic strength. Thermodynamic parameters calculated from temperature dependence of the stability constants were as follows : ${\Delta}H=-(27.2{\pm}1.7)kJ\;mol^{-1}$ and ${\Delta}S=-(110{\pm}7)JK^{-1}mol^{-1}$. There was a linear relationship between the enthalpy and entropy for 1:1 complex formation of the uranyl ion with a variety of anionic ligands.

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