• Title/Summary/Keyword: 핵자기 공명분광분석

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Stability Constants for Transition Metal ions of Hexadentate $N_6$ Ligands Containing Two Pyridyl Groups (피리딘을 포함하는 여섯자리 $N_6$ 리간드와 전이금속 이온 착물의 안정도상수)

  • Kim, Sun-Deuk;Kim, Jun-Kwang;Park, Yoon-Yul
    • Analytical Science and Technology
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    • v.12 no.5
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    • pp.397-402
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    • 1999
  • The open-chain hexadentate $N_6$, ligand containing two pyridyl groups, 1,15-bis(2-pyridyl)-2,6,10,14-tetraazapentadecane (bpyped) has been synthesized as its tetrahydroehloride salt and characterized by EA, IR, NMR, and Mass. Its proton dissociation constants($logK{^n}_H$) and stability constants ($log\;K_{ML}$) for Co(II), Ni(II), Cu(II) and Zn(II) ions were determined at $25^{\circ}C$ and ionic strength 0.10 M($KNO_3$) in aqueous solution by potentiometry and compared with those or analogous $N_6$ ligands contain one or two propylenic spacers, which make six-membered chelate rings, between the aliphatic nitrogen atoms.

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Preparation of Polypropylene/Clay Nanocomposites Using Aminosilane Treated Clay (아미노실란 개질 클레이를 사용한 폴리프로필렌 클레이 나노복합재료)

  • Hong Chae-Hwan;Bae Jin-Woo;Lee Yong-Bum;Lee Choon-Soo;Jho Jae-Young;Nam Byeong-Uk
    • Polymer(Korea)
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    • v.30 no.4
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    • pp.318-325
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    • 2006
  • Polypropylene-clay nanocomposites were studied by the modification of clay with amino silanes to introduce covalent bonds in nanocomposites, and prepared by melt-compounding with polypropylene, clay modified with amino silanes and maleic anhydride grafted polypropylene. The . .structure and surface properties of modified clay were determined by x-ray diffraction, infrared spectrum, and solid-state $^{29}Si$ nuclear magnetic resonance spectrum. The modification of clay with aminosilanes led to the increase of the silicate interlayers to about $19.8{\AA}$, the weakening effects of hydroxy group at $3650cm^{-1}$ and the signal of amine groups at -69 ppm proved that the modification had taken place.

Sequence Structure and Thermal Property of Poly(butylene terephthalate) (PBT)/p-Acetoxybenzoic Acid (ABA) Copolymers Obtained Through Melt Trans-esterification Reaction (용융 에스테르 교환반응에 의해 제조된 폴리부틸렌테레프탈레이트/파라아세톡시벤조산 공중합체의 서열구조와 열적 성질)

  • 김도경;박수영;박종래
    • Polymer(Korea)
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    • v.24 no.1
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    • pp.58-64
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    • 2000
  • Poly(butylene terephthalate-co-oxybenzoate) (PBOT ) was synthesized by melt trans-esterification of poly(butylene terephthalate)(PBT) and p-acetoxybensoic acid (ABA) at 250, 260, and 27$0^{\circ}C$ with the compositions of PBT/ABA of 4/6, 5/5, 6/4. The sequence analysis of PBOT with a $^1$H FT-NMR indicated that the number of consecutive oxybenzoate units ranges from 1.2 to 1.5, which is larger than that of the corresponding poly(ethylene terephthalate)(PET)/ABA (PEOT) obtained at the same reaction conditions as the PBOT. The difference in the block length influenced the thermal degradation behavior: Polyoxybezoate (POB), PBT and PEOT showed one-step degradation whereas PBOT exhibited two-step degradation. The results suggested that PBOT consisted of three phases of PBT-rich phase, random phase of PBT and ABA, and ABA-rich phase.

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Cobalt(III) Complex of Ethylenediamine-N,N'-di-${\alpha}$-Isobutyric Acid (Ethylenediamine-N,N'-di-${\alpha}$-Isobutyric Acid의 코발트(III) 착물)

  • Moo-Jin Jun;Chang-Yoon Han;Chang-Woo Park;Sung Rack Choi;Kwang-Ha Park
    • Journal of the Korean Chemical Society
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    • v.30 no.1
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    • pp.84-89
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    • 1986
  • A newflexible $N_2O_2$-type tetradentate ligand. Ethylenediamine-N,N'-di-${\alpha}$-isobutyric acid(eddib), has been synthesized, and dichloro cobalt(III) complex of eddib has been prepared via the air-oxidation technique. Only S-cis isomer has been yielded during the preparation of complex. Ring strain and steric hinderance are cited as the cause for the preference for the S-cis geometric configuration. On series of cobalt(III) complexes of eddib, $[Co(eddib)L]^{n+}$ $(L = Cl{\cdot}(H_2O),\;CO_3^{2-},\;(H_2O)_2)$have been prepared in situ. In their electronic absorption spectra, the absorption maxima and their intensities of the above series of complexes are on the ordinary line of the spectrochemical and hyperchromic series. Elemental analysis, IR, NMR and electronic absorption spectra have been used to characterize the complex and geometries of the complex.

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A Study on the Charge Transfer Complex Formed between 2,4-Dihalogen or 2,4,6-trihalogenanisole Derivatives and Iodine or Iodine Monochloride (2,4-디할로겐 또는 2,4,6-트리할로겐아니솔 유도체들과 요오드 또는 염화요오드 사이에 생성된 전하이동 착물에 관한 연구)

  • Kim, You Sun;Park, Kyung Bae
    • Journal of the Korean Chemical Society
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    • v.20 no.5
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    • pp.380-390
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    • 1976
  • The trends of forming a charge transfer complex have been studied for electron donors such as anisole, 4-chloroanisole, 2,4-dichloroanisole, 2-fluoro-4-chloroanisole, 2-bromo-4-chloroanisole, 2-iodo-4-chloroanisole, 2-fluoro-4,6-dichloroanisole, 2,4,6-trichloroanisole, 2-bromo-4,6-dichloroanisole, 2-iodo-4,6-dichloroanisole, and 2-iodo-4,5,6-trichloroanisole, and electron acceptors such as iodine and iodine monochloride in the carbon tetrachloride or the hexane solvent system. It was found that the formation of a charge transfer complex was influenced by the Van der Waals Radii of the 2-halogen atoms on the benzene ring and further the overall steric moiety of the molecule of the electron donor. These trends were also experienced in a system of chloroform and one of the prementioned electron donor by means of a nuclear magnetic resonance spectrometry. The spectrophotometrical data on the formation of the charge transfer complex were presented and the results were discussed with views of the steric structure of the 2-halogen atom on the benzene ring.

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Characterization of Hyaluronic Acid Membrane Cross-linked with Lactide (락타이드로 가교시킨 히아루론산 막의 특성)

  • Kwon, Ji-Young;Cheong, Seong-Ihl
    • Polymer(Korea)
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    • v.29 no.6
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    • pp.599-604
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    • 2005
  • The hyaluronic acid (HA) with excellent biocompatibility has been combined with lactide, the ester dimer of polylactide, with good biodegradability to produce biocompatible materials which can control the period of degradation in a human body. By freeze frying method, HA and lactide were crosslinked with crosslinking agent, 1-ethyl-3-(3-dimethyl aminopropyl) carbodiimide (EDC). Degree of lactide and EDC reaction was determined by the analysis of nuclear magnetic resonance spectroscopy. Both lactyl group and EDC conversion increased as the mole ratio of lactide to HA increased from 5 to 13. The membrane swelled less and became more brittle with the more addition of lactyl group resulting from the higher mole ratio of lactide to HA. Swelling ratio decreased and tensile modulus increased due to the more addition of lactyl group as the EDC concentration increased or reaction temperature decreased. Drug release experiment from various membranes with different degree of crosslinking showed that permeability decreased with increasing degree of crosslinking. The degradation became slower with the more addition of lactyl group. Mechanical property and degradation rate of the synthesized membrane were shown to be controlled through adjusting operation parameters such as mole ratio, temperature, and crosslinking agent concentration.

Metal-Nitrosyl Complexes(II) : Synthesis and Characterization of Dinitrosyltungsten(O) Complexes (금속-니트로실 착물 (제 2 보) : 디니트로실 텅스텐(O) 착물의 합성과 특성)

  • Sang-Oh Oh;Seong-Jong Mo
    • Journal of the Korean Chemical Society
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    • v.36 no.6
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    • pp.906-913
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    • 1992
  • The polymeric compound [{$W(NO)_2Cl_2$}$_n$] were prepared by reductive nitrosylation of $WNaNO_2$ and acidified $WFeSO_4$ with $WWCl_6$ at room temperature. The reactions of [{$W(NO)_2Cl_2$}$_n$] with unidentate and bidentate ligands afforded neutral monomeric [$W(NO)_2Cl_2L_2$(or L-L)] in a relative high yields (70$\sim$90%). 3,5-lutidine, ${\gamma}$-cyanopyridine, 1,2-phenylenediamine, 1,10-phenanthroline, sym-diphenylethylenediamine, 9,10-phenanthrenequinone, 1,3-bis(diphenylphosphino)propane, 1,1'-bis(diphenylphosphino)ferrocene and 8-hydroxyquinoline were used as coordinating ligands. These dinitrosyltungsten complexes were characterized by elemental analysis, $^1H$-NMR, infrared, and UV-visible spectroscopy are reported. The spectral data indicated that geometric structures of the products were cis-dinitrosyl-trans-dichloro-cis-$L_2$ of $C_{2v}$ symmetry.

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Synthesis of Lactide/Hyaluronic Acid Polymer Membrane for the Application of Drug Delivery System (약물방출시스템 적용을 위한 락타이드/히아루론산 고분자 막의 제조)

  • Kim, Min-Su;Kwon, Ji-Young;Cheong, Seong-Ihl
    • Membrane Journal
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    • v.15 no.4
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    • pp.281-288
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    • 2005
  • The hyaluronic acid (HA) with excellent biocompatibility can be combined with lactide, the ester dimer of polylactide, with good biodegradability to produce biocompatible materials applicable to drug delivery system. By freeze drying method, HA and lactide were crosslinked with crosslinking agent, 1-ethyl-3-(3-dimethyl aminopropyl) carbodiimide. Degree of lactide and EDC reaction was determined by the analysis of nuclear magnetic resonance (NMR) spectroscopy. The degree of lactide and EDC reaction increased and swelling ratio decreased as the mole ratio of lactide to HA or crosslinking agent concentration increased or reaction temperature decreased. The drug release experiment result from membranes having different degree of lactide reaction showed that drug release rate reduced in proportion to the degree of lactide reaction. The drug release experiment result from drugs having different hyrodphobicity showed that the more hydrophobic drug was released more slowly.

Formation of New Thorium (IV) Complexes with Crown Ethers (새로운 Thorium (IV)-Crown Ether 착물형성)

  • Jung, Hak-Jin;Jung, Oh-Jin;Suh, Hyouck-Choon
    • Journal of the Korean Chemical Society
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    • v.31 no.3
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    • pp.258-270
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    • 1987
  • A series of new thorium nitrate complexes with crown ethers have been synthesized from the reaction of the hydrated thorium nitrate, with the appropriate crown ethers of different cavity sizes in various solvents such as methanol, ethanol, butanol, methylacetate, acetone, tetrahydrofuran and acetylacetone. CHN elemental analysis, ICPAS, thermal analysis and Karl-Fischer method have been used to characterize their compositions, and the spectroscopic methods of IR, UV, $^1H-NMR$, and X-ray diffraction have been employed to determine the structures and solvolysis phenomena of these complexes. and the electrical conductances were measured in DMSO, and water solvent. The solvolysis have been observed only in the complexes synthesized in acetylacetone solvent. In the solvated complexes of 15-crown-5 and 18-crown-6, the mole ratio of $Th^{4+}$: ligand : acetylacetone is found to be 1:1:1, but in the non-solvated complexes of 12-crown-4 and 15-crown-5, the mole ratios of Th:L are 1:2 and 2:3, respectively, and that in the complexes of both 18-crown-6 and dicyclohexano-18-crown-6 is 1:1. All complexes which were not solvated have shown $n{\to}{\sigma}^{\ast}$ electronic transitions of crown ether whereas complexes solvated have exhibited both $n{\to}{\sigma}^{\ast}$ of crown ether and $n{\to}{\pi}^{\ast}$ transitions of acac. The dissociation mole ratio of $Th^{4+}$ and nitrate ion is found to be 1:1 in aprotic solvent, and 1:4 in protic solvent like water.

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Phase Behavior and Structural Analyses of the THF + H2 Binary Clathrate Hydrate (THF + H2 이성분계 크러스레이트 하이드레이트의 상거동 및 구조 분석)

  • Cha, Jong-Ho;Park, Youngjune;Cha, Min-Jun;Yeon, Sun-Hwa;Lee, Huen
    • Korean Chemical Engineering Research
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    • v.46 no.6
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    • pp.1095-1099
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    • 2008
  • In this study, we investigated that hydrate formation and phase behavior of the $THF+H_2$ binary clathrate hydrates. In order to confirm the binary clathrate hydrate formation we employed the Raman and NMR spectroscopies that are known to be quite powerful tools, particularly for examining the cage occupancy pattern of guest molecules. In addition, we traced the P-T profiles from clathrate hydrate formation and dissociation process, which made it possible for the resulting phase equilibrium boundary to be clearly established. In the binary clathrate hydrate matrix we further identified that the relatively large THF molecules can only occupy the large $5^{12}6^4$ cavities, while the small $H_2$ molecules are entrapped in the empty $5^{12}$ cavities in structure-II, making the hydrate to be stable above 273 K even at relatively low pressure condition. Considering that pure $H_2$ hydrate can be produced at the extreme pressures higher that 1,000 bar, we can conclude that the water-soluble second guest inclusion induces $H_2$ storage and transportation to be readily achievable under much milder conditions.