• Title/Summary/Keyword: F-19 NMR

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Textile Surface Modification by Environmentally Friendly Waterborne Fluorinated Acrylate Copolymer (환경친화형 수분산성 불소 아크릴레이트 공중합체에 의한 섬유 표면개질)

  • Yoo Su-Yong;Kim Jung-Du;Moon Myung-Jun;Suh Cha-Su;Ju Chang-Sik;Lee Min-Gyu
    • Journal of Environmental Science International
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    • v.13 no.10
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    • pp.947-953
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    • 2004
  • Waterborne fluorinated acrylate copolymer (WFAC) for surface modification of textile was synthesized from perfluoroalkyl ethyl acrylate, octadecyl acrylate, glycidyl methacrylate, surfactant and 3,3 methyl-methoxy butanol. The structures of the synthesized WFAC were determinated by FT-IR and $^{19}F-NMR$ analysis. The thermal stability investigated with DSC and TGA was decreased with increasing the content of fluorinated acrylate in the copolymer. However, the particle sizes of WFAC were increased with increasing the content of fluorinated acrylate in the copolymer. The surface energies calculated by contact angles of WFAC were in the range of 29.80$\~$13.41 dyne/cm. On the observing SEM of the textile surface treated with WFAC, the textile was swollen and compacted with increasing the concentration of water repellency agent. WFAC synthesized in this study showed a good water repellency.

Preparation and Characterization of Random Copolymer Electrolyte Membranes Containing PFCB (Perfluorocyclobutane) Group (PFCB (Perfluorocyclobutane) Group을 포함한 랜덤 공중합체 고분자 전해질 막 제조 및 특성연구)

  • Kim Jeong-Hoon;Kim Dong-Jin;Chang Bong-Jun;Lee Soo-Bok;Joo Hyeok-Jong
    • Membrane Journal
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    • v.16 no.3
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    • pp.221-229
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    • 2006
  • This study is about the preparation and characterization of sulfonated random copolymer membranes containing perfluorocyclobutane (PFCB), fluorenyl, and sulfonyl units. The polymers were prepared through three synthetic steps, that is, the synthesis of a trofluorovinylether-terminated monomer, its thermal polymerization, and post-sulfonation using chlorosulfonic acid. A series of sulfonated random copolymers with different ion exchange capacity (IEC) were prepared by changing contents of fluorenyl uints in polymers with fixed molar ratio of chlorosulfonic acid during the post-sulfonation reaction. All the synthesized compounds were characterized by FT-lR, $^1H-NMR$, $^{19}F-NMR$, and Mass spectroscopy. As the content of sulfonated fluorenyl units increased, the IEC, water uptake, and ion conductivity of the sulfonated random copolymer membranes increased. The sulfonated random copolymer S-1 and S-2 showed higher values of ion conductivity than the Nafion-115 in a wide range of temperatures ($25{\sim}80^{\circ}C$).

Preparation and Characterization of Fluorenyl Polymer Electrolyte Membranes Containing PFCB Groups (PFCB Group을 포함한 Fluorene계 고분자 전해질막 제조 및 특성연구)

  • Kim Jeong-Hoon;Kim Dong-Jin;Chang Bong-Jun;Shin Chong-Kyu;Lee Soo-Bok;Joo Hyeok-Jong
    • Membrane Journal
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    • v.16 no.1
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    • pp.16-24
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    • 2006
  • We report on the preparation and characterization of sulfonated polymer membranes containing perfluorocyclobutane (PFCB) units and fluorene units. The polymers were prepared through three synthetic steps, that is, the synthesis of a trifluorovinylether-terminated monomer, its thermal polymerization, and post-sulfonation using chlorosulfonic acid. A series of sulfonated polymers with different ion exchange capacity (IEC) were prepared by changing the content of chlorosulfonic acid during the post-sulfonation reaction. All the synthesized compounds were characterized by FT-IR, $^{1}H-NMR,\;^{19}F-NMR$, and Mass spectroscopy. As the content of chlorosulfonic acid increased, the SD, IEC, water uptake, and ion conductivity of the sulfonated polymer membranes increased. The sulfonated polymer 4 showed higher values of ion conductivity than the Nafion-$115^{\circledR}$ in a wide range of temperatures ($25{\sim}80^{\circ}C$).

Are Bound Residues a Solution for Soil Decontamination\ulcorner

  • Bollag, Jean-Marc
    • Proceedings of the Korean Society of Soil and Groundwater Environment Conference
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    • 2003.10a
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    • pp.111-124
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    • 2003
  • Processes that cause immobilization of contaminants in soil are of great environmental importance because they may lead to a considerable reduction in the bioavailability of contaminants and they may restrict their leaching into groundwater. Previous investigations demonstrated that pollutants can be bound to soil constituents by either chemical or physical interactions. From an environmental point of view, chemical interactions are preferred, because they frequently lead to the formation of strong covalent bonds that are difficult to disrupt by microbial activity or chemical treatments. Humic substances resulting from lignin decomposition appear to be the major binding ligands involved in the incorporation of contaminants into the soil matrix through stable chemical linkages. Chemical bonds may be formed through oxidative coupling reactions catalyzed either biologically by polyphenol oxidases and peroxidases, or abiotically by certain clays and metal oxides. These naturally occurring processes are believed to result in the detoxification of contaminants. While indigenous enzymes are usually not likely to provide satisfactory decontamination of polluted sites, amending soil with enzymes derived from specific microbial cultures or plant materials may enhance incorporation processes. The catalytic effect of enzymes was evaluated by determining the extent of contaminants binding to humic material, and - whenever possible - by structural analyses of the resulting complexes. Previous research on xenobiotic immobilization was mostly based on the application of $^{14}$ C-labeled contaminants and radiocounting. Several recent studies demonstrated, however, that the evaluation of binding can be better achieved by applying $^{13}$ C-, $^{15}$ N- or $^{19}$ F-labeled xenobiotics in combination with $^{13}$ C-, $^{15}$ N- or $^{19}$ F-NMR spectroscopy. The rationale behind the NMR approach was that any binding-related modification in the initial arrangement of the labeled atoms automatically induced changes in the position of the corresponding signals in the NMR spectra. The delocalization of the signals exhibited a high degree of specificity, indicating whether or not covalent binding had occurred and, if so, what type of covalent bond had been formed. The results obtained confirmed the view that binding of contaminants to soil organic matter has important environmental consequences. In particular, now it is more evident than ever that as a result of binding, (a) the amount of contaminants available to interact with the biota is reduced; (b) the complexed products are less toxic than their parent compounds; and (c) groundwater pollution is reduced because of restricted contaminant mobility.

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Amine and Olefin Complexes of Pt(II) Having a PCP-Pincer Ligand

  • Park, Soon-Heum
    • Bulletin of the Korean Chemical Society
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    • v.23 no.1
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    • pp.132-136
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    • 2002
  • $Pt(2,6-(Cy_2PCH_2)_2C_6H_3)(OTf)\;(OTf=CF_3SO_3^-)$ readily reacts with various amines to afford cationic amine complexes $[Pt(2,6-(Cy_2PCH_2)_2C_6H_3)(amine)](OTf)\;(amine=NH_3,\;NHMe_2,\;NHC_4H_8,\;NH_2Ph,\;NH_2(Tol-p))$ in high yields. These complexes have been fully characterized by IR, $^1H-,\;^{19}F{^1H}-,\;and\;^{31}P{^1H}-NMR$ spectroscopy, and elemental analyses. Reaction of $Pt(2,6-(Cy_2PCH_2)_2C_6H_3)(OTf)$ with acrylonitrile quantitatively produced the ${\pi}$-olefinic complex $Pt(2,6-(Cy_2PCH_2)_2C_6H_3)(CH_2=CHCN)](OTf)$ which is only stable in solution in the presence of acrylonitrile. Attempt at isolating this complex in the pure solid state was failed due to partial decomposition into $Pt(2,6-(Cy_2PCH_2)_2C_6H_3)(OTf)$ The equilibrium constants $(K_{eq}=[Pt(PCP)-(NH_2R)^+][CH_2=CHCN]/[Pt(PCP)(CH_2=CHCN)^+][NH_2R]:\;[Pt(2,6-(Cy_2PCH_2)_2C_6H_3)(CH_2=CHCN)]^++NH_2R{\rightleftarrows}[Pt(2,6-(Cy_2PCH_2)_2C_6H_3)(NH_2R)]^++CH_2=CHCN=Ph,\;p-tolyl)$ were calculated to be 0.28 (for R = Ph) and 3.1 (R = p-tolyl) at $21^{\circ}C$. The relative stability of the ${\sigma}$-donor amine versus the ${\pi}$-olefinic acrylonitrile complex has been found largely dependent upon the amine-basicity $(pK_b)$, implicating that acrylonitrile practically competes with amine in the platinum coordination sphere. On the contrary to the formation of the acrylonitrile complex, no reaction of $Pt(2,6-(Cy_2PCH_2)_2C_6H_3)(OTf)$ with other olefins such as ethylene, styrene and methyl acrylate was observed.

Ligand Binding Properties of the N-Terminal Domain of Riboflavin Synthase from Escherichia coli

  • Lee, Chan-Yong;Illarionov, Boris;Woo, Young-Eun;Kemter, Kristina;Kim, Ryu-Ryun;Eberhardt, Sabine;Cushman, Mark;Eisenreich, Wolfgang;Fischer, Markus;Bacher, Adelbert
    • BMB Reports
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    • v.40 no.2
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    • pp.239-246
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    • 2007
  • Riboflavin synthase from Escherichia coli is a homotrimer of 23.4 kDa subunits and catalyzes the formation of one molecule each of riboflavin and 5-amino-6-ribitylamino- 2,4(1H,3H)-pyrimidinedione by the transfer of a 4-carbon moiety between two molecules of the substrate, 6,7- dimethyl-8-ribityllumazine. Each subunit comprises two closely similar folding domains. Recombinant expression of the N-terminal domain is known to provide a $C_2$-symmetric homodimer. In this study, the binding properties of wild type as well as two mutated proteins of N-terminal domain of riboflavin synthase with various ligands were tested. The replacement of the amino acid residue A43, located in the second shell of riboflavin synthase active center, in the recombinant N-terminal domain dimer reduces the affinity for 6,7-dimethyl-8-ribityllumazine. The mutation of the amino acid residue C48 forming part of activity cavity of the enzyme causes significant $^{19}F$ NMR chemical shift modulation of trifluoromethyl derivatives of 6,7-dimethyl-8-ribityllumazine in complex with the protein, while substitution of A43 results in smaller chemical shift changes.

Characterization and performance of post treated PVDF hollow fiber membrane

  • Eman S. Sayed;Hayam F. Shaalan;Magda I. Marzouk;Heba A. Hani
    • Membrane and Water Treatment
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    • v.15 no.2
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    • pp.79-88
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    • 2024
  • Modification of Polyvinylidene fluoride (PVDF) hollow fiber membranes (HFMs) characteristics and performance were investigated via post treatment using different oxidants. sodium hypochlorite (NaOCl), hydrogen peroxide (H2O2) and potassium persulfate (KPS). Fourier transform infrared (FTIR) and Proton nuclear magnetic resonance (1H-NMR) results revealed no structural differences after post treatment. Cross-sectional micrographs show finger-like structures at the outer and inner walls of the HFMs and sponge-like structures in middle, where NaOCl and KPS post treated fibers exhibited a decrease in finger-like structures in addition to aggregates appearing on the surface, consequently leading to an increase in the surface roughness (Ra) from 48 nm to 52.8nm and 56 nm, respectively. Hydrogen peroxide post treatment only was observed to decrease the water contact angle from 98° to 81.4°. It was also observed that the elongation at break and the modulus deceased after NaOCl post treatment from 34.5 to 28.5% and from 19.3 Mpa to 16.6 Mpa, respectively. Moreover, pure water flux after H2O2 post treatment increased from 87.8 LMH/bar to 113 LMH/bar at 0.45 bar, while no changes were detected for the methylene blue dye rejection (74%) between raw and hydrogen peroxide post treated fibers at the same pressure. According to the findings hydrogen peroxide post treated PVDF HFMs have the most uniform surfaces, with almost no alterations in structural and mechanical properties or porosities with enhanced hydrophilicity and pure water flux maintaining appropriate rejection. Therefore, it is considered an efficient surface modifying agent for UF/NF membranes or low-pressure separators.

The Effect of Nuclear Overhauser Enhancement in Liver and Heart $^{31}P$ NMR Spectra Localized by 2D Chemical Shift Technique (이차원 화학변위 기법을 이용한 간 및 심장 $^{31}P$ 자기공명분광에서의 Nuclear Overhauser 효과에 대한 연구)

  • Ryeom Hun-Kyu;Lee Jongmin;Kim Yong-Sun;Lee Sang-Kwon;Suh Kyung-Jin;Bae Sung-Jin;Chang Yongmin
    • Investigative Magnetic Resonance Imaging
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    • v.8 no.2
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    • pp.94-99
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    • 2004
  • Purpose : To investigate the signal enhancement ratio by NOE effect on in vivo $^{31}P$ MRS in human heart muscle and liver. we also evaluated the enhancement ratios of different phosphorus metabolites, which are important in 31P MRS for each organ. Materials and Methods : Ten normal subjects (M:F = 8:2, age range = 24-32 yrs) were included for in vivo $^{31}P$ MRS measurements on a 1.5 T whole-body MRI/MRS system using $^1H-^{31}P$ dual tuned surface coil. Two-dimensional Chemical Shift Imaging (2D CSI) pulse sequence for $^{31}P$ MRS was employed in all $^{31}P$ MRS measurements. First, $^{31}P$ MRS performed without NOE effect and then the same 2D CSI data acquisitions were repeated with NOE effect. After postprocessing the MRS raw data in the time domain, the signal enhancements in percent were estimated from the major metabolites. Results : The calculated NOE enhancement for liver $^{31}P$ MRS were $\alpha-ATP\;(7\%),\;\beta-ATP\;(9\%),\;\gamma-ATP\;(17\%),\;Pi\;(1\%),\;PDE\;(19\%)$ and $PME\;(31\%)$. Because there is no creatine kinase activity in liver, PCr signal is absent. For cardiac $^{31}P$ MRS, whole body coil gave better scout images and thus better localization than surface coil. In $^{31}P$cardiac multi-voxel spectra, DPG signal increased from left to right according to the amount of blood included. The calculated enhancement for cardiac $^{31}P$ MRS were : $\alpha-ATP\;(12\%),\;\beta-ATP\;(19\%),\;\gamma-ATP\;(30\%),\;PCr\;(34\%),\;Pi\;(20\%),\;(PDE)\;(51\%),\;and\;DPG\;(72\%)$. Conclusion : Our results revealed that the NOE effect was more pronounced in heart muscle than in liver with different coupling to 1H spin system and thus different heteronuclear cross-relaxation.

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Bioactivities and Isolation of Functional Compounds from Decay-Resistant Hardwood Species (고내후성 활엽수종의 추출성분을 이용한 신기능성 물질의 분리 및 생리활성)

  • 배영수;이상용;오덕환;최돈하;김영균
    • Journal of Korea Foresty Energy
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    • v.19 no.2
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    • pp.93-101
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    • 2000
  • Wood of Robinia pseudoacacia and bark of Populus alba$\times$P. glandulosa, Fraxinus rhynchophylla and Ulmus davidiana var. japonica were collected and extracted with acetone-water(7:3, v/v) in glass jar to examine whether its bioactive compounds exist. The concentrated extracts were fractionated with hexane, chloroform, ethylacetate and water, and then freeze-dried for column chromatography and bioactive tests. The isolated compounds were sakuranetin-5-O-$\beta$-D-glucopyranoside from Populus alba $\times$Pl glandulosa, 4--ethyoxy-(+)-leucorobinetinidin frm R. pseudoacacia and fraxetion from F. rhynchophylla and were characterized by $^1H$ and$^{13}C $ NMR and positive FAB-MS. Decay-resistant activity was expressed by weight loss ratio and hyphae growth inhibition in the wood dust agar medium inoculated wood rot fungi. R. pseudoacacia showed best anti-decaying property in both test and its methanol untreated samples, indicating higher activity than methanol treated samples in hyphae grwoth test. In antioxidative test, $\alpha$-tocopherol, one of natural antioxidants, and BHT, one of synthetic antioxidants, were used as references to cmpare with the antioxidant activities of the extacted fractions. Ethylacetate fraction of F. rhynchophylla bark indicated the hightest activity in this test and all fractions of R. pseudiacacia extractives also indicated higher activities compared with the other fractions. In the isolated compounds, aesculetin isolated from F. rhynchophylla bark showed best activity and followed by robonetinidin from R. pseudoacaica.

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