• Title/Summary/Keyword: F-19 NMR

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Characterization of $YBa_2Cu_3O_{7-x}F_y$ Superconducting Materials Made by a Sol-Gel Process (졸-겔법으로 제조한 $YBa_2Cu_3O_{7-x}F_y$ 초전도물질의 특성분석)

  • 김봉흡;강형부;김현택
    • The Transactions of the Korean Institute of Electrical Engineers
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    • v.41 no.5
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    • pp.525-532
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    • 1992
  • Fluorine-doped YBaS12TCuS13TOS17-xTFS1yT superconducting materials with y varing two orders of magnitude form 0.02 to 2.0 have been prepared by a sol-gel process by using metal nitrate salts, sodium hydroxide and sodium fluoride. Fluorine contents have been measured using an ion-selective electrode. All fluorine doped as reactant were found to be present in the resulted samples. From the observation of XRD it has been concluded that the samples with y 0.2 formed simply the single phase of perovskite structure, whereas those with y 0.5 yielded together some compounds such as BaFS12T, YFS13T and CuO in the resulted samples. The observation of solid state S019TF NMR has been carried out in order to check whether fluorine was actually incorporated into the lattice sites, and the experimental results revealed that the mole ratio of fluorine incorporated into the lattice sites of YBaS12TCuS13TOS17-xT was approximately 0.2 per mole of the compound. Also electrical resistivity measurement indicated that onset transition temperature has the tendency to increase slightly with increasing y in the dilute region as y 0.2.

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Synthesis and Surface Characteristics of Novel Oligomeric Silane with Perfluoropolyether (과불소 폴리에테르 포함 새로운 실란형 올리고머의 합성과 표면 특성)

  • Park, Eun-Young;Lee, Sang-Goo;Ha, Jong-Wook;Park, In-Jun;Lee, Soo-Bok;Lee, Yong-Taek
    • Polymer(Korea)
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    • v.32 no.4
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    • pp.397-402
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    • 2008
  • Perfluoropolyether(PFPE) has been widely applied in industry because of its very excellent properties of very high contact angle and low surface energy, good lubricant property and antifouling property. But the difficulty to synthesize PFPE has limited the research on this field. In this study, the novel silicon-containing oligomer with perfluoropolyether moiety was synthesized, and the structure was characterized by $^{19}F$-NMR and $^1H$-NMR. The surface properties of contact angle, sliding angle, and soil release property were investigated. The results show that PFPE in this study can be utilized as an anti-smudge coating material because it shows lower sliding angle and better soil release property than commercial products.

Synthesis, Cure Behavior, and Rheological Properties of Fluorine-Containing Epoxy Resins (불소함유 에폭시 수지의 합성, 경화 거동 및 유변학적 특성)

  • 박수진;김범용;이재락;신재섭
    • Polymer(Korea)
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    • v.27 no.3
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    • pp.176-182
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    • 2003
  • The fluorine-containing epoxy resin, 2-trifluorotoluene diglycidylether (FER) was prepared by reaction of 2-chloro-${\alpha}$,${\alpha}$,${\alpha}$-trifluorotoluene with glycerol diglycidylether in the presence of pyridine catalyst. Curing behavior of FER/DDM system was investigated using dynamic and isothermal DSC. Cure activation energy (Ea) was determined by Flynn-Wall-Ozawa's equation. The rheological properties of FER/DDM system were studied under isothermal condition using a rheometer. Cross-linking activation energy (Ec) was determined from the Arrhenius equation based on gel time and curing temperature. As a result, the chemical structure of FER was confirmed by FT-IR, $\^$13/C NMR, and $\^$19/F NMR spectroscopy. The cure activation energy of FER/DDM system was 55.4 kJ/mol and conversion and conversion rate were increased with the curing temperature. The cross-linking activation energy of FER/DDM system was 41.6 kJ/mol and gel time was decreased with the curing temperature.

Preparation and Characterization of Partially Fluorinated Poly (arylene ether sulfone)/PTFE Composite Membranes for Fuel Cell (연료전지용 부분불소계 Poly (arylene e ther sulfone)/PTFE 복합막의 제조 및 특성 분석)

  • Kim, Eun Hee;Chang, Bong-Jun;Kim, Jeong-Hoon
    • Membrane Journal
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    • v.22 no.3
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    • pp.191-200
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    • 2012
  • New composite membranes were manufactured by impregnating post-sulfonated poly(arylene ether sulfone)s containing perfluorocyclobutane (PFCB) groups into porous polytetrafluoroethylene (PTFE) films. Two kinds of post-sulfonated poly(arylene ether sulfone)s with two different monomer ratios (sulfonable biphenylene monomer : non-sulfonable sulfonyl monomer = 6 : 4, 4 : 6) were first prepared through three synthetic steps: synthesis of trifluorovinylether-terminated monomers, thermal cycloaddition polymerization and post-sulfonation using chlorosulfonic acid (CSA). The composite membranes were then prepared by adjusting the concentrations (5~20 wt%) of the resulting copolymers impregnated in the PTFE films. The water uptake, ion exchange capacity (IEC) and ion conductivity of the composite membranes were characterized and compared with their unreinforced dense membranes and Nafion. All the synthesized compounds, monomers and polymers were characterized by $^1H$-NMR, $^{19}F$-NMR and FT-IR and the composite membranes were observed with scanning electron micrographs (SEM).

Synthesis and Characterization of Two New Fluoroplumbate(II) Complexes: Tetrabutylammonium Fluorodihaloplumbate, (But)4N[PbX2F] (X = Cl, I)

  • Javanshir, Zahra;Mehrani, Kheyrollah;Ghammamy, Shahriare;Saghatforoush, LotfAli;Seyedsadjadi, Seyedabolfazl;Hassanijoshaghani, Ali;Tavakol, Hossein
    • Bulletin of the Korean Chemical Society
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    • v.29 no.8
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    • pp.1464-1466
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    • 2008
  • Tetrabutylammonium Fluorodichloroplumbate(II), N$(C_4H_9)_4$[$PbCl_2F$], TBAFDiCP and Tetrabutylammonium Fluorodiiodoplumbate(II), [$(C_4H_9)_4$N][$PbI_2F$], TBAFDiIP are the first examples of fluoroplumbate salts that have been prepared from the reaction of $(C_4H_9)_4$NF with $PbCl_2$ and $PbI_2$ respectively using either $CH_3CN$ solvent. These new compound characterized by elemental analysis, IR, UV/Visible, $^1H$ NMR, and $^{19}F$ NMR techniques.

$^{13}$C NMR Study of the Application of the 'Tool of Increasing Electron Demand' to the 9-Aryl-tricyclo[3.3.1.0$^{2,8}$]non-9-yl, and 8-Aryl-Tetracyclo[3.2.1.0$^{2,7}$.0$^{4,6}$]oct-8-yl cations

  • Wie-Chang Jin;Gweon-Young Ryu;Chun Yoon;Shin Jung Hyu
    • Bulletin of the Korean Chemical Society
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    • v.10 no.6
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    • pp.591-595
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    • 1989
  • The$^{13}C$ NMR shifts of a series of para-substituted 9-aryl-tricyclo$[3.3.1.0^{2,8}]$non-9-yl and 8-aryl-tetracyclo$[3.2.1.0^{2,7}.0^{4,6}]$-oct-8-yl cations were measured in $FSO_3H/SO_2ClF \;at\; -90^{\circ}C\; or\; -70^{\circ}C$ in order to examine whether the ${\rho}^{c+}$ values can be used to explain the mechanism for the stabilization of the geometrically rigid cyclopropylcarbinyl cations. Plots of the ${\Delta}{\delta}^{c+}$ shifts against ${\sigma}^{c+}$ reveal excellent linear correlation. The tricyclononyl systems yield a ${\rho}^{c+}$ value of -4.95 with a correlation coefficient r = 0.9948. The tetracyclo-octanyl systems give a ${\rho}^{c+}$ value of -6.39 with r = 0.9943. A fair parallelism exists between the results of $^{19}F$ nmr studies and the change of ${\rho}^{c+}$ values in these cations. Accordingly, the present study established that the ${\rho}^{c+}$ value can be used as a mearsure of the geometric influence for the charge delocalization in cyclopropylcarbinyl cations.

$^{13}C-NMR$ Study of the Applicaton of the “ Tools of Increasing Electron Demand ” to the 8-Aryl-tricyclo $[3.2.1.0^{2,7}]$oct-8-yl Cations

  • Gweon-Young Ryu;Jung-Hyu Shin
    • Bulletin of the Korean Chemical Society
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    • v.12 no.2
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    • pp.193-196
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    • 1991
  • The $^{13}C-NMR$ shifts of a series of para-substituted $8-aryl-tricyclo[3.2.1.0^{2,7}]oct-8-yl$ and $9-aryl-tricyclo[3.3.1.0^{2,8}]-non-9-yl$ cations were measured in $FSO_3H/SO_2ClF\ at\-90^{\circ}$ in order to examine whether the ${\rho}^{C^+}$ values can be used as a measure of the geometric influence on the charge delocalization resulting from ${\rho}$ conjugation in rigid tricyclopropylcarbinyl cations. Plot of the ${\Delta}{\delta}^{C+} shifts against the ${\sigma}^{C+}$ constants revealed excellent linear correlation. The 8-aryl tricyclooctyl systems yielded a ${\rho}^{C+}$ value of -5.00 with r = 0.9962. Previous investigation of the 9-aryl-tricyclononyl systems gave a correlation coefficient of r = 0.9948 with a slope of ${\rho}^{C+}$ = -4.95. A fair parallelism exists between the results of $^{19}F-NMR $ studies and the change of ${\rho}^{C+}$ value in these cations. Consequently, it is established that the ${\rho}^{C+}$ value can be used to explain the mechanism of charge stabilization of the rigid cyclopropylcarbinyl cation such as tricyclo $[3.2.1.0^{2,7}]oct-8-yl$ cation.

$^{15}$N NMR Relaxation Study of the Catalytic Residues in Y14F Mutant Ketosteroid Isomerase

  • Yoon, Ye-Jeong;Lee, Hyeong-Ju;Kim, Chul;Lee, Hee-Cheon
    • Journal of the Korean Magnetic Resonance Society
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    • v.8 no.2
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    • pp.77-85
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    • 2004
  • $^1$H-detected $^{15}$N NMR was employed to investigated the effect of mutation (Y14F) on the dynamic properties of catalytic residues in ${\Delta}^5$-3- ketosteroid isomerase (KSI) from Conamonas testosteroni. In particular, the backbone dynamics of the catalytic residues have been studied in free enzyme and its complex with a steroid ligand, 19-nortestosterone hemisuccinate, by $^{15}$N relaxation measurements. The relaxation data were analyzed using the model-free formalism to extract the model-free parameters (S$^2$, ${\tau}_e$, and R$_{ex}$). The results show that the mutation causes a significant decrease in the order parameter (S$^2$) for the catalytic residues of free Y14F KSI, presumably due to breakdown of the hydrogen bond network by mutation. In addition, the order parameters of Phe-14 and Asp-99 increased slightly upon ligand binding, indicating a slight restriction of the high-frequency (pico- to nanosecond) internal motions of the residues in the complexed Y14F KSI, while the order parameter of Tyr-55 decreased significantly upon ligand binding.

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Structure Determination of Antifungal KRF-001 Produced by Bacillus subtilis subsp. krictiensis (Bacillus subtilis subsp. krictiensis가 생산하는 항진균 물질 KRF-001의 구조 결정)

  • 김성기;이남경;정태숙;김영국;최진자;복성해
    • Microbiology and Biotechnology Letters
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    • v.19 no.6
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    • pp.598-603
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    • 1991
  • An antifungal mixture of six members (component A to F), KRF-001 produced by Bacillzts subtilis subsp. krictiensis was isolated from the fermentation broth. Molecular weight of component A to F was determined by FAB-MS to be 1042, 1056, 1056, 1070, 1070 and 1084 respectively. Various instrumental analyses (amino acid analysis, GC-MS, $^1H-NMR, ^1HH$ COSY NMR) revealed that the mixture was a homologous cyclic peptide composed of each one mole of glutamine, proline, tyrosine, serine, unusual $\beta$-amino acid and three moles of asparagine. The structural differences of component A to F were found in carbon number and terminal structure of the unusual $\beta$-amino acid. After determination of the sequence and stereochemistry of those amino acids, the tentative structure of KRF-001 was determined.

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