• 제목/요약/키워드: Temperature variation H NMR

검색결과 12건 처리시간 0.023초

($^{11}$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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    • 한국초전도학회 2000년도 High Temperature Superconductivity Vol.X
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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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$^1H-NMR$을 이용한 계피의 t-cinnamaldehyde 정량분석 (Quantitative Analysis of t-Cinnamaldehyde of Cinnamomum cassia by $^1H-NMR$ Spectrometry)

  • 송명종;유종수;백남인
    • Applied Biological Chemistry
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    • 제48권3호
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    • pp.267-272
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    • 2005
  • 계피(계지, Cinnanmomum cassia)의 주요성분인, trans-cinnamaldehyde를 $^1H-NMR$ 분광법을 이용하여 정량분석하였다. 핵자기 공명법을 이용한 정량분석의 응용가능성을 확인하기 위하여, t-cinnamaldehyde의 $^1H-NMR$ 스펙트럼에서 시료의 농도와 측정온도를 변화시킴에 따라 chemical shift의 변화와 적분값의 변화를 관찰하였다. t-Cinnamaldehyde(7.1429 mg/ml)를 19, 25, 30, 40 및 $50^{\circ}C$ 하에서 $^1H-NMR$ 측정한 결과, aldehyde methine signal(doublet)의 chemical shift가 9.7202, 9.7184, 9.7169, 9.7142 및 9.7124 ppm에서 관측되었다. 이는 측정온도는 signal의 chemical shift의 변화에 중요한 변수가 되지 않는다는 것을 의미하였다. 또한, aldehyde signal의 적분값이 $1.37(19^{\circ}C),\;1.37(25^{\circ}C),\;1.37(30^{\circ}C),\;1.37(40^{\circ}C)$$1.37(50^{\circ}C)$로써, 측정온도가 signal의 적분값에는 전혀 영향을 미치지 않는 것으로 나타났다. 동일한 온도 $25^{\circ}C$에서 0.4464, 0.8929, 1.7857, 3.5714, 7.1429 및 14.286 mg/ml의 농도의 시료에 대한 $^1H-NMR$ 측정 결과, aldehyde기의 chemical shifts는 각각 9.7206, 9.7201, 9.7196, 9.7192, 9.7185 및 9.7174 ppm에서 나타났다. 이는 각 시료의 농도가 증가함에 따라서 aldehyde의 signal이 고자장으로 약간 이동하는 것으로 나타났다. Aldehyde기의 doublet methine signal의 적분값과 각 시료의 농도에 따른 calibration curve는 직선으로 나타났으며, 매우 높은 회귀율($r^2=1.0000$)을 보였다. t-Cinnamaldehyde와 aldehyde기를 갖는 물질로써, C. cassia의 또 다른 구성성분인 t-2-methoxycinnamaldehyde($7.1429\;mg/ml\;CDCl_3,\;25^{\circ}C$)에 대해서, $^1H-NMR$ 스펙트럼을 측정한 결과, t-cinnamaldehyde는 ${\delta}_H$ 9.7174(9.7078, 9.7270)서 관측되었다. t-2-Methoxycinnamaldehyde는 ${\delta}_H$ 9.6936(9.6839, 9.7032)에서 관측되었다. 따라서, 두 화합물의 chemical shift의 차이는 resolution 값이 0.45 Hz인 NMR 스펙트럼 상에서 충분히 구분할 수 있을 정도로 나타났다. 위의 방법을 이용하여, 추출용매에 따른 C. cassia 내의 t-cinnamaldehyde의 함량을 분석한 결과, n-hexane, $CHCl_3$ 및 EtOAc로 추출하였을 때에, 각각 94.2 mg/g(0.94%), 137.6 mg/g(1.38%), 140.1 mg/g(1.40%)으로 결정되었다.

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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    • 제33권2호
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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.

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

  • 이인성;신현택;이종필;이수원;홍진웅
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 2001년도 추계학술대회 논문집
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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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유입변압기용 절연유의 절연파괴특성 (Electrical Breakdown Properties of Insulating Oils for oil-immersed transformer)

  • 이인성;신현택;이종필;이수원;홍진웅
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 2001년도 추계학술대회 논문집 Vol.14 No.1
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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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    • 제51권2호
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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.

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

  • 옥치완;신태용
    • 약학회지
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    • 제31권5호
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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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    • 제15권5호
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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.

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

  • 정우식
    • 공업화학
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    • 제3권2호
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    • pp.312-317
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    • 1992
  • 디옥소우라늄(VI) (우라닐) 이온과 질산 이온과의 상호작용을 산소-17 핵자기공명분광법으로 연구하였다. $UO_2NO_3{^+}$의 우라닐 산소 원자(이후 우라닐 산소)의 산소-17 공명신호는 우라닐 이온의 그것보다 낮은 자기장에서 나타났다. $UO_2NO_3{^+}$의 안정도상수를 5, 15, 25, $35^{\circ}C$에서 질산 이온 농도에 따른 산소-17 화학적 이동의 변화로부터 구했으며, 그 값은 이온강도에 따라 달랐다. 안정도상수의 온도 의존성으로부터 계산한 열역학적 파라미터는 다음과 같다: ${\Delta}H=-(27.2{\pm}1.7)kJ\;mol^{-1}$${\Delta}S=-(110{\pm}7)JK^{-1}mol^{-1}$. 우라닐 이온과 여러가지 음이온의 배위자와의 1:1 착물형성 반응에 대한 엔탈퍼와 엔트로피 사이에는 직선관계가 있었다.

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