• Title/Summary/Keyword: Solid State NMR

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NOISE Spectroscopy: Applications to Solid State NMR

  • Yang, Doo-Kyung;Zax, D.B.
    • Journal of the Korean Magnetic Resonance Society
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    • v.6 no.2
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    • pp.142-154
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    • 2002
  • One of the oldest, still unsolved, and often ignored problems in magnetic resonance remains the issue of how to observe undistorted, normal one-dimensional spectra where the frequencies and their relative intensities represent faithfully the distribution of spins and sites in the sample within the magnet. Often distortions in these parameters are accepted, as the price of sensitivity enhancement, or because it is unclear just how these distortions might be avoided. Surprisingly enough, the problem is exacerbated by the use of modern techniques of pulsed Fourier transform NMR. Noise spectroscopy is an approach to solving the problem of distorted NMR spectra, which is largely under appreciated; it promises virtually "unlimited" distortionless bandwidths without costly hardware investments. Nonetheless, its exploitation remains limited. We will discuss why noise spectroscopy belongs in the arsenal of tricks spectroscopists should be aware of, show examples where its use is essential if accurate, quantitative NMR is to be expected, and discuss some recent approaches which extend its applicability yet further, particularly in solid state NMR and in applications to quadrupolar nuclear spins.

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Solid-State $^1H$ and $^{29}Si$ NMR Studies of Silicate and Borosilicate Gel to Glass Conversion

  • 양경화;우애자
    • Bulletin of the Korean Chemical Society
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    • v.17 no.8
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    • pp.696-699
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    • 1996
  • Silicate and borosilicate gels were prepared by the sol-gel process and thermally treated in the 150-850 ℃ temperature range. Solid-state 1H MAS and 29Si CP/MAS NMR spectroscopy were used to investigate the effects of heat treatments on the silicate gel to glass conversion process. The 1H NMR isotropic chemical shifts and the relative intensities of hydrogen bonded and isolated silanol groups have been used to access the information concerning the dehydration process on the silicate gel surface. The 29Si NMR isotropic chemical shifts affected by the local silicon environment have been used to determine the degree of crosslinking, i.e. the number of siloxane bonds. These NMR results suggest that the silicate gel to glass conversion process is occurred by two stages which are dependent on the temperature; (1) the formation of particles up to 450 ℃ and (2) the formation of large particles by aggregation of each separated single particle above 450 ℃. In addition, the effects of B atom on the formation of borosiloxane bonds in borosilicates have been discussed.

A 2H solid-state NMR study on the lipid phase change in the presence of an antimicrobial peptide (항균성 펩타이드와 혼합된 인지질 분자의 상 변화에 대한 고체 중수소 핵자기 공명 연구)

  • Choi, Hyung Geun;Kim, Chul
    • Analytical Science and Technology
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    • v.26 no.1
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    • pp.61-66
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    • 2013
  • The activity of an antimicrobial peptide, protegrin-1, on the well-aligned lipid bilayer deposited on a thin coverglass plate was investigated by $^2H$ solid-state NMR spectroscopy. Orientational distribution and molecular motion in the lipid bilayer were determined from $^2H$ solid-state NMR spectrum. Reorientational motion of lipid molecules in the vacuum-dried state was found to be small but their orientational distribution was not able to be determined. As storage times were longer, the order of the alignment of lipid molecules in the lipid bilayer and percentages involved in the toroidal pore structures increased. We found that much longer time is required to get the equilibrium state of the peptide-lipid mixture under our experimental condition for investigating the action of the antimicrobial peptide like protegrin-1 on the lipid bilayers deposited on the thin coverglass plates.

Inclusion Complex of $Permethylated-{\bata}-Cyclodextrin$ with Benzaldehyde

  • Choi Hee-Sook
    • Bulletin of the Korean Chemical Society
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    • v.13 no.2
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    • pp.179-183
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    • 1992
  • A stable solid new inclusion complex with benzaldehyde and $permethyl-\beta-cyclodextrin$ was obtained by recrystallization method. The structure of the $benzaldehyde-permethyl-\beta-cyclodextrin$ inclusion complex in the solid and solution state have been studied by UV, IR, $^1H-NMR$, $^{13}C-NMR$ and FAB-mass spectroscopy.

Solid State Dynamic Nuclear Polarization of 1H Nuclear Spins at 0.3 T and 4.2 K

  • Shim, Jeong Hyun
    • Journal of the Korean Magnetic Resonance Society
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    • v.21 no.4
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    • pp.114-118
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    • 2017
  • Here, I report solid state Dynamic Nuclear Polarization (DNP) of $^1H$ nuclear spins at 0.3 T and 4.2 K. The DNP polarizer was developed based on a commercial X-band Electron Spin Resonance (ESR) modified for DNP, in combination with a NMR console and a liquid-Helium cryostat. By detuning magnetic field, DNP spectrum was measured to find the optimal condition. At +3 mT detuned from on-resonance field, $^1H$ NMR signal of 60:40 glycerol/water frozen solution doped with 20 mM perdeuterated-Tempone was amplified 43 times. The $^1H$ spin polarization obtained at 4.2 K is over 3100 times higher than that at 300 K. The width of the DNP spectrum, which is five times broader than ESR spectrum, is inconsistent with solid effect or thermal mixing, and presumably suggests a different DNP mechanism.

Organic Light-Emitting Diodes Fabricated from $Alq_3$ in Different Crystalline Polymorphs

  • Kaji, Hironori;Fukushima, Tatsuya
    • 한국정보디스플레이학회:학술대회논문집
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    • 2008.10a
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    • pp.185-188
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    • 2008
  • We have analyzed the structures of $Alq_3$ in different polymorphs by solid-state NMR. On the basis of the results, OLEDs were fabricated from different polymorphs of $Alq_3$. The current efficiency of the device fabricated from the mixture of $\alpha$-, $\gamma$-, and $\delta-Alq_3$ powders was higher than that from $\alpha-Alq_3$.

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Characterization of Vanadium Oxide Supported on $TiO_2-ZrO_2$ Catalysts by $^{51}V$ Solid-State NMR Spectroscopy

  • Park, Eun-Hee;Lee, Sung-Won;Lee, Man-Ho
    • Journal of the Korean Magnetic Resonance Society
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    • v.4 no.1
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    • pp.1-11
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    • 2000
  • Supported vanadium oxides are being used extensively as catalysts for a variety of reactions, including partial oxidations and ammoxidations. A series of vanadium oxide supported on TiO2-ZrO2 was obtained by impregnating ammonium metavanadate slowly into a mixed precipitateof Ti(OH)4-Zr(OH)4, followed by calcining in air at high temperatures. The prepared catalysts were characterized by 51V solid-state NMR. In the calcined catalysts 51V NMR studies indicated the peaks corresponding to distorted tetrahedral vanadia species at low V2O5 contents and octahedral vanadia species at high vanadia loadings. These results illustrate the suitability of 51V NMR as a unique quantitative spectroscopic tool in the structural analysis of vanadium(V) oxide catalytic materials.

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