• 제목/요약/키워드: Solution NMR

검색결과 565건 처리시간 0.025초

Polycyclotriphosphazene Derivative Grafted and NanometerY2O3 Doped SPEEK Composite Membrane for DMFC

  • Li, Xia;Guo, Qiang;Zhang, Tianjiao;Qian, Junzhi;Tan, Xiaolin
    • 대한화학회지
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    • 제57권5호
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    • pp.625-633
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    • 2013
  • A type of polycyclotriphosphazene derivative (PCTPD), hexasulfanilic acid polycyclotriphosphazene (HSACP) and HSACP grafting SPEEK, sulfonated poly[2-(petachloropolycyclotriphosphazene-oxy)] etheretherketone (SPPSACPEEK) were synthesized, which were characterized by FTIR and $^{31}P$ NMR. Then three types of composite membranes such as HSACP grafting SPEEK, HSACP blending SPEEK, and nano $Y_2O_3$ doping and HSACP grafting SPEEK, respectively, were continuously prepared by solution-casting method. Comparing to SPEEK membranes with different amount of HSACP grafted or blended, grafting 15 wt% HSACP and doping 10 wt% nano $Y_2O_3$ SPEEK membrane conducted outstanding overall behavior of proton conductivity reaching $3.18 {\times}10^{-2}$ S/cm at $90^{\circ}C$ which was merely junior to SPEEK with 15 wt% HSACP grafted, methanol permeability coefficient getting $9.46{\times}10^{-8}cm^2{\cdot}s^{-1}$, swelling degree of 20.9% and solid residue of 98.98% which was superior to all specimen.

Positive-Type Photosensitive Polyimide Based on a Photobase Generator Containing Oxime-Urethane Groups as a Photosensitive Compound

  • Jang Young-Min;Seo Ji-Young;Chae Kyu-Ho;Yi Mi-Hye
    • Macromolecular Research
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    • 제14권3호
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    • pp.300-305
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    • 2006
  • The chemical structure of a semi-aromatic polyimide-I, which was prepared by the chemical imidization of cyclopentanetetracarboxylic dianhydride and 2,2-bis(4-aminophenyl)hexafluoropropane, was characterized by $^{13}C-NMR$ spectroscopy. The chemically imidized polyimide-I was used for the preparation of a photosensitive polyimide (PSPI) through the addition of benzophenone and benzophenone oxime hexamethylene diurethane (BOHD), a photobase generator containing oxime-urethane groups. The polyimide-I film containing benzophenone and BOHD was not soluble in 2.38 wt% tetrabutylammonium hydroxide solution in $H_2O$. However, it became soluble following irradiation with 310 nm UV light. A positive tone image with a resolution of $5{\mu}m$ was obtained with this PSPI, having sensitivity($D_c$) of $1.2J/cm^2$ and contrast(${\gamma}_p$) of 1.08. Thus, a polyimide, which is not intrinsically photosensitive, can become photosensitive through the addition of a photobase generator containing oxime-urethane groups as a photosensitive compound.

히알루론산에 결합된 리포산 자기조립체의 제조 및 특성 (Self-Aggregated Nanoparticles of Lipoic Acid Conjugated Hyaluronic Acid)

  • 홍인림;김영진
    • 폴리머
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    • 제32권6호
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    • pp.561-565
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    • 2008
  • 본 연구에서는 천연고분자인 히알루론산(hyaluronic acid, HA)에 항산화제인 리포산(lipoic acid, LA)을 그래프트시켜 양친성 공중합체를 결합하였다. 이 공중합체는 수용액상에서 자기조립에 의해서 친수성인 히알루론산이 소수성인 리포산을 감싸는 형태의 고분자 입자를 형성한다. 히알루론간과 리포산을 결합하기 전에 adipic acid dihydrazide(ADH)을 이용하여 히알루론산의 카복실 부분을 개질시켰다. 히알루론산의 개질 분석과 HA-g-LA의 결합을 확인하기 위해 분광학적 분석방법을 이용하여 분석하였다. 형성된 입자는 DLS와 TEM을 사용하여 크기를 측정하였고 나노크기의 구조를 이룬다는 것을 확인하였다. 나노크기의 고분자 입자는 소수성 물질을 포함하는 전달체로 사용될 수 있다.

키토산-리포산 자기 조립체의 제조 및 특성 (Preparation and Characterization of Self-aggregated Nanoparticles of Chitosan-Lipoic Acid Conjugate)

  • 박은주;김영진
    • 폴리머
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    • 제32권6호
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    • pp.544-548
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    • 2008
  • 본 연구에서는 키틴의 알칼리 가수분해를 통해 탈아세틸화도가 조절된 세 가지 조건의 키토산을 제조하였고, 이 키토산이 수용성을 지니게 화학적 분해법을 이용해 분자량을 조절하였다. 이렇게 제조된 분자량이 조절된 세 가지 조건의 탈아세틸화도를 가지는 키토산 각각에 항산화제인 리포산을 합성하여 항산화 능력을 가지는 생체 적합성 나노 구조체를 형성하였다. 키토산-리포산의 합성을 확인하기 위하여 분광학적 분석 방법을 사용하여 분석하였다. 키토산-리포산 합성체는 수용액 상태에서 자기조립체를 형성하며 이렇게 형성된 자기조립체 나노 입자는 약 135 nm 정도의 크기를 가지고 있음을 알 수 있었다.

Backbone 1H, 15N and 13C Resonance Assignment and Secondary Structure Prediction of HP0062 (O24902_HELPY) from Helicobacter pylori

  • Jang, Sun-Bok;Ma, Chao;Park, Sung-Jean;Kwon, Ae-Ran;Lee, Bong-Jin
    • 한국자기공명학회논문지
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    • 제13권2호
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    • pp.117-125
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    • 2009
  • HP0062 is an 86 residue hypothetical protein from Helicobacter pylori strain 26695. HP0062 was identified ESAT-6/WXG100 superfamily protein based on structure and sequence alignment and also contains leucine zipper domain sequence. Here, we report the sequence-specific backbone resonance assignment of HP0062. About 97.7% of all $^1H_N,\;^{15}N,\;^{13}C_{\alpha},\;^{13}C_{\beta}\;and\;^{13}C=O$ resonances were assigned unambiguously. We could predict the secondary structure of HP0062 by analyzing the deviation of the $^{13}C_{alpha}\;and\;^{13}C_{\beta}$ chemical shifts from their respective random coil values. Secondary structure prediction shows that HP0062 consist of two ${\alpha}$-helices. This study is a prerequisite for determining the solution structure of HP0062 and can be used for the study on interaction between HP0062 and DNA and other Helicobacter pylori proteins.

제미니형 디에틸렌글리콜 디카르복실레이트 류의 합성 및 특성 (Synthesis and Properties of Gemini Type's Diethylene Glycol Dicarboxylates)

  • 최은지;전영수;이재덕;정노희
    • 한국응용과학기술학회지
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    • 제27권3호
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    • pp.257-265
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    • 2010
  • This study concerned about "Gemini type co-surfactant" which has very interesting properties with new components. They were synthesized by reaction of diethylene glycol monoethyl ether and dicarboxylic acid. The structure could be comfirmed with FT-IR and $^1H$-NMR. Surface active properties such as surface tension, evaluated cmc, cloud point, emulsing power were measured respectively at given conditions. Their surface tensions in the aqueous solution were decreased to 33~35 dyne/cm, which was lower than 39 dyne/cm of SDS, and their cmc values evaluated by surface tension method were $5.0{\times}10^{-1}\sim7.5{\times}10^{-1}$ mol/L. And the emulsifying power was excellent in jojoba oil. All of the synthesized Gemini surfactants possessed good water solubility and their cloud point were $48\sim58^{\circ}C$. As results, Gemini surfactants which were synthesized are expected to be applied as O/W emulsifiers.

Synthesis and X-Ray Structure of 25-Acetoxy-26,27,28-trimethoxycalix[4]arene

  • ;;;임수경
    • Bulletin of the Korean Chemical Society
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    • 제15권12호
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    • pp.1108-1112
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    • 1994
  • 25-Acetoxy-26,27,28-trimethoxycalix[4]arene was synthesized by the treatment of calix[4]arene trimethyl ether with acetyl chloride in the presence of NaH. The solution conformation was inferred as a partial cone conformation based on the $^1H$-and $^{13}C$ NMR spectra. The crystal structure has been determined by X-ray diffraction method. The crystals are monoclinic, space group $P2_1$/n, a=8.186 (1), b=17.137 (2), c=19.878 (3) ${\AA}$, ${\beta}$=95.67 (1)$^{\circ}$, Z=4, V=2774.90 ${\AA}^3$, $D_c$= 1.22 g $cm^{-3}$, $D_m$=1.23 g $cm^{-3}$. The intensity data were collected on an Enraf-Noninus CAD-4 Diffractometer with a graphite monochromated $Cu-K{\alpha}$ radiation. The structure was solved by direct method and refined by full-matrix least-squares methods to a final R value of 0.054 for 3675 observed reflections. The molecule possesses a partial cone conformation with one flattened phenyl unit, in which one anisol ring, distal to the ester ring, is inverted. The acetoxyphenyl ring is flattened.

Highly Porous Pillared Clay with Multistacked $SiO_2/TiO_2$ Nanosols

  • 조진호;박주형;윤주병
    • Bulletin of the Korean Chemical Society
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    • 제19권11호
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    • pp.1185-1188
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    • 1998
  • Layered nanocomposite, SiO2/TiO2 sol pillared clay, has been prepared by the ion exchange reaction of Na' ion in montmorillonite with positively charged mixed SiO2/TiO2 sol. The nanosized sol particles were synthesized by mixing SiO2 sol solution with TiO2 one, which is obtained by acidic hydrolysis of TEOS and TiCl4, respectively. From powder XRD, the basal spacing (d001) of the sample calcined at 400 ℃ was found to be ca. 60 Å, due to the multistacking of nanosized SiO2 and TiO2 sol particles, which was confirmed by the pore size analysis from 129Xe NMR and micropore analysis calculated from nitrogen adsorption. The BET specific surface area shows the value of 684 m2g-1 (Langmuir 1115 m2g-1), which is the highest among various pillared clays ever reported previously, and the total porosity is found to be 0.51 mlg-1, and the pores are mainly composed of micropore with a size of ca. 11.8 Å. This result agrees with the adsorption capacity obtained from water adsorption. According to diffuse reflectance ultraviolet-visible spectroscopy, it is found that the TiO2 particles stabilized in the interlayer space of montmorillonite are quantum-sized of ca. 20 Å.

Synthesis, Structure, and Antitumor Activity of Novel Platinum(II) Complexes Involving Asymmetric Chiral Diamines as Carrier Ligands

  • 이은주;전무진;손윤수
    • Bulletin of the Korean Chemical Society
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    • 제20권12호
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    • pp.1469-1474
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    • 1999
  • New platinum(II) complexes with asymmetrically substituted chiral diamine ligands A₂PtX₂, (A₂ = NH₂CH(CH₃)CH₂NH($c-C_5H_9)$ (apcpa), NH₂CH(CH₃)CH₂NH($c-C_6H_11)$ (apcha); X₂ = 2Cl, isopropylidenmalonate (IPM), 1,1'-cyclobutandicarboxylate (CBDCA)) have been synthesized and characterized by means of elemental analyses, infrared and NMR spectroscopies, and X-ray crystallography. The crystal structures of (S-apcha)Pt[CBDCA] ·3H₂O (orthorhombic, P2₁2₁2(No. 18), a = 6.926(3), b = 15.243(3), c = 19.319(4)Å, V = 2039.5(10) ų, Z = 4, R = 0.072) and (S-apcha)Pt[IPM] ·2.5 H₂O (monoclinic, P2/C(No. 13), a = 9.882(1), b =18.502(1), c = 22.056(1)Å, V = 4032.8(5)ų, Z = 8, R=0.093) exhibit that the platinum atoms achieve a typical square planar arrangement with two nitrogen atoms in cis position and with the chiral center retained. The spectroscopic data disclose that these platinum complexes are stable and their molecular structures are retained in aqueous solution. Among these platinum complexes, the asymmetric diamine-Pt(II) complexes with chloride leaving group exhibit high in vivo activity comparable to cisplatin against leukemia L1210 cell line.

An NMR Study on Molecular Motions of $\alpha$,2,6-Trichlorotoluene in Solution State

  • Ahn, Sang-Doo;Lee, Jo-Woong
    • Bulletin of the Korean Chemical Society
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    • 제15권7호
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    • pp.553-559
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    • 1994
  • Dynamics of $CH_2CI$ group in ${\alpha},2,6$-trichlorotoluene dissolved in $CDCl_3$ was studied by observing various relaxation modes for $^{13}C$ under proton undecoupled condition. Partially relaxed $^{13}C$ spectra were obtained at $34^{\circ}C$ as a function of evolution time after applying various designed pulse sequences to this $AX_2$ spin system. It was found that nonlinear regression analysis of the relaxation data for these magnetization modes could provide the information about dipolar and spin-rotational auto-correlation and cross-correlation spectral densities for fluctuation of the $^{13}C-^1H$ internuclear vector in $CH_2Cl$ group. The results show that the effect of cross-correlation is comparable in magnitude to that of auto-correlation and the relaxation in this spin system is dominated by dipolar mechanism rather than spin-rotational one. From the resulting spectral density data we could calculate the bond angle ${\angle}HCH\;(105.1$^{\circ}$) and elements of the rotational diffusion tensor for $CH_2Cl$ group.