• 제목/요약/키워드: Solid state NMR

검색결과 225건 처리시간 0.022초

NOISE Spectroscopy: Applications to Solid State NMR

  • Yang, Doo-Kyung;Zax, D.B.
    • 한국자기공명학회논문지
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    • 제6권2호
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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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    • 제17권8호
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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.

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

  • 최형근;김철
    • 분석과학
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    • 제26권1호
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    • pp.61-66
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    • 2013
  • 얇은 유리판 위에 잘 정렬된 인지질 이중막에 작용하는 항균성 펩타이드 protegrin-1의 활성작용을 고체 $^2H$ 핵자기 공명 분광법을 이용하여 조사하였다. 수화 전후에 있어서 인지질 분자의 배향분포와 그 운동성을 고체 $^2H$ 핵자기 공명 스펙트럼을 통하여 확인하였다. 진공으로 건조된 상태에서는 인지질 분자의 운동성이 작다는 사실 외에는 인지질 분자들의 배향분포에 대한 정확한 상태를 알 수 없었다. 그러나 시료가 수화된 이후에는 시간이 지남에 따라 인지질 분자들이 잘 정렬되어 간다는 것과 원환체 기공이 형성되어 간다는 것을 확인할 수 있었다. Protegrin-1과 같은 항균성 펩타이드에 의한 인지질 이중막 변화를 본 연구논문에서 사용한 방법으로 확인하기 위해서는 상당히 긴 반응시간이 필요하다는 것을 확인하였다.

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

  • Choi Hee-Sook
    • Bulletin of the Korean Chemical Society
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    • 제13권2호
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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
    • 한국자기공명학회논문지
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    • 제21권4호
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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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    • 한국정보디스플레이학회 2008년도 International Meeting on Information Display
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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
    • 한국자기공명학회논문지
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    • 제4권1호
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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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