• 제목/요약/키워드: Static NMR

검색결과 18건 처리시간 0.021초

Ferroelectric-Paraelectric Phase Transition of CsH2PO4 studied by Static NMR and MAS NMR

  • Lim, Ae Ran;Lee, Kwang-Sei
    • 한국자기공명학회논문지
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    • 제19권1호
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    • pp.29-35
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    • 2015
  • The microscopic dynamics of $CsH_2PO_4$, with two distinct hydrogen bond lengths, are studied by static nuclear magnetic resonance (NMR) and magic angle spinning (MAS) NMR. The proton dynamics of the two crystallographically inequivalent hydrogen sites were discussed in terms of the $^1H$ NMR and $^1H$ MAS NMR spectra. Although the hydrogen bonds have two inequivalent sites, H(1) and H(2), distinct proton dynamics for the two sites were not found. Further, the $^{133}Cs$ spectrum is more or less continuous near $T_{C1}$ (=153 K). Finally, the phase transition mechanism of $T_{C1}$ in $CsH_2PO_4$ is related to the ordering of protons.

Structural characteristics of [N(CH3)4]2CdCl4 determined by 1H MAS NMR, 13C CP/ MAS NMR, and 14N NMR

  • Lee, Seung Jin;Lim, Ae Ran
    • 한국자기공명학회논문지
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    • 제19권1호
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    • pp.18-22
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    • 2015
  • The structural geometry of $[N(CH_3)_4]_2CdCl_4$ in a hexagonal phase is studied by $^1H$ MAS NMR, $^{13}C$ CP/MAS NMR, and $^{14}N$ NMR. The changes in the chemical shifts for $^{13}C$ and $^{14}N$ in the hexagonal phase are explained by the structural geometry. In addition, the temperature dependencies of the spin-lattice relaxation time in the rotating frame $T_{1{\rho}}$ for $^1H$ MAS NMR and $^{13}C$ CP/MAS NMR are measured.

Low-ε Static Probe Development for 15N-1H Solid-state NMR Study of Membrane Proteins for an 800 MHz NB Magnet

  • Park, Tae-Joon;Choi, Sung-Sub;Jung, Ji-Ho;Park, Yu-Geun;Kim, Yongae
    • Bulletin of the Korean Chemical Society
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    • 제34권3호
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    • pp.823-826
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    • 2013
  • A low-${\varepsilon}$ solid-state NMR(Nuclear Magnetic Resonance) probe was developed for the spectroscopic analysis of two-dimensional $^{15}N-^1H$ heteronuclear dipolar coupling in dilute membrane proteins oriented in hydrated and dielectrically lossy lipid environments. The system employed a 800 MHz narrow-bore magnet. A solenoid coil strip shield was used to reduce deleterious RF sample heating by minimizing the conservative electric fields generated by the double-tuned resonator at high magnetic fields. The probe's design, construction, and performance in solid-state NMR experiments at high magnetic fields are described here. Such high-resolution solid-state NMR spectroscopic analysis of static oriented samples in hydrated phospholipid bilayers or bicelles could aid the structural analysis of dilute biological membrane proteins.

Design and Implementation of Portable NMR Probe Magnet

  • Junxia, Gao;Yiming, Zhang;Jiashen, Tian
    • Journal of Magnetics
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    • 제22권1호
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    • pp.14-22
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    • 2017
  • The NMR's probe consists of the static magnetic field generator (magnetic source) and the RF coil. It is very strict for the homogeneity of the static magnetic field intensity of the magnetic source, so the cost of the magnetic source is more expensive in the entire nuclear magnetic resonance instrument. The magnetic source generally consists of electromagnet, permanent magnet and superconducting magnet. The permanent magnet basically needs not to spend on operation and maintenance and its cost of manufacture is much cheaper than the superconducting magnet. Therefore, the permanent magnet may be the only choice for the static magnetic field device if we want to use the magnetic resonance instrument as an analyzer for production by reducing price. A new probe magnet was developed on the basis of the permanent magnet ring in this paper to provide a technological way for reducing the manufacturing cost, weight and volume of the existing nuclear magnetic resonance instrument (including MRI) probe.

Chemical Shift and Quadrupolar Interactions in Solids

  • Kim Jin-Eun
    • 한국자기공명학회논문지
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    • 제10권1호
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    • pp.1-37
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    • 2006
  • General expressions for solid state NMR lines are described for transitions under static, magic angle spinning, and variable angle spinning conditions in the case where the principal axis system for the anisotropic chemical shift tensor is noncoincident with that of the quadrupole coupling tensor. It is demonstrated that solid state NMR powder pattern simulation program VMAS based on the conventional grid point method of integrating over the Euler angle space is fast enough in comparison with the POWDER simulation package and Gauss-point method.

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NMR 분광법의 원리와 지구환경과학에의 응용 (Theory of NMR Spectoscopy and Its Application in Geoenvironmental Sciences)

  • 김영규
    • 암석학회지
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    • 제10권3호
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    • pp.233-245
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    • 2001
  • NMR분광법은 현재 화학에서 빼 놓을 수 없는 아주 중요한 연구방법의 하나지만 또한 지질학의 연구에 있어서도 초전도 자석의 발달과 함께 그 중요성이 부각되고 있다. 지질학에 있어서 NMR의 연구 대상 원소로는 광물의 주 구성 성분이며 여러 가지 구조적 정보를 갖고 있는 $^{29}Si$, $^{27}Al$ 등이 유용하게 사용되며 이들은 각각 다른 여러 정보들을 제공한다. 이 밖에도 $^{23}Na$와 같은 알칼리금속과 더불어 다양한 핵종들이 지질학에서 NMR로 연구되고 있다. NMR을 이용하여 다양한 방면의 연구들이 가능한데 NMR은 XRD, TEM보다도 더욱 작은 미시적인 (분자적 관점에서의) 구조 연구에 사용될 수 있다. 이러한 연구를 통해 Al, Si 질서-무질서, 산소원자와의 배위수, 인근의 다른 양이온의 분포 등을 포함한 구조적 정보를 알 수 있다. 또한 NMR의 또 다른 장점은 정적인 미시 구조뿐만 아니라 분자들의 움직임(dynamics)에 대한 정보도 알 수 있다는 것이다. 이러한 동적인 정보는 기존의 어느 방법으로도 알기 어려웠던 부분이고 NMR을 통하여 분자들의 상호 교환 속도와 활성화 에너지 등에 대한 폭 넓은 이해가 가능할 수 있다. 이 밖에 NMR을 이용하여 비정질 물질에 대한 구조와 더불어 지표면에서 산출되는 유기물에 대한 성분 및 구조도 아주 중요하게 연구될 수 있는 분야이다.

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113Cd and 133Cs NMR Study of Nucleus-Phonon Interactions in Linear-Chain Perovskite-Type CsCdBr3

  • Park, Sung Soo;Lim, Ae Ran
    • 한국자기공명학회논문지
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    • 제20권4호
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    • pp.109-113
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    • 2016
  • Resonance frequencies from the $^{113}Cd$ and $^{133}Cs$ nuclear magnetic resonance (NMR) spectra for the $CsCdBr_3$ single crystal were measured at varying temperatures by the static NMR method. The temperature-dependent changes of these frequencies are related to the changing structural geometry of the ${CdBr_6}^{4-}$ units, which affects the environment of $^{133}Cs$. The spin-lattice relaxation rates ($1/T_1$) for the $^{113}Cd$ and $^{133}Cs$ nuclei were measured in order to obtain detailed information about the dynamics of $CsCdBr_3$ crystals. The dominant relaxation mechanisms for $^{113}Cd$ and $^{133}Cs$ nuclei are direct single-phonon and Raman spin-phonon processes, respectively.

Development of 600-MHz 19F-7Li Solid-State NMR Probe for In-Situ Analysis of Lithium Ion Batteries

  • Jeong, Ji-Ho;Park, Yu-Geun;Choi, Sung-Sub;Kim, Yongae
    • Bulletin of the Korean Chemical Society
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    • 제34권11호
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    • pp.3253-3256
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    • 2013
  • Lithium is a highly attractive material for high-energy-concentration batteries, since it has low weight and high potential. Rechargeable lithium-ion batteries (LIBs), which have the extremely high gravimetric and volumetric energy densities, are currently the most preferable power sources for future electric vehicles and various portable electronic devices. In order to improve the efficiency and lifetime, new electrode compounds for lithium intercalation or insertion have been investigated for rechargeable batteries. Solid-state nuclear magnetic resonance (NMR) is a very useful tool to investigate the structural changes in electrode materials in actual working lithium-ion batteries. To detect the in-situ microstructural changes of electrode and electrolyte materials, $^7Li-^{19}F$ double-resonance solid-state NMR probe with a static solenoidal coil for a 600-MHz narrow-bore magnet was designed, constructed, and tested successfully.

Carbon-13 Nuclear Magnetic Resonance Spectroscopic Studies of $^{13}CO$ Adsorbed on Platinum Particles in L-Zeolites

  • 한옥희;Gustavo Larsen;Gary L. Haller;Kurt W. Zilm
    • Bulletin of the Korean Chemical Society
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    • 제19권9호
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    • pp.934-942
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    • 1998
  • $^13CO$ chemisorbed on platinum particles in L-zeolite has been investigated by static and magic angle spinning NMR spectroscopy. The representative spectra are composed of a broad asymmetric peak with a center of gravity at 230±30 ppm and a sharp symmetric peak at 124±2 ppm which is tentatively assigned to physisorbed $CO_2$, on inner walls of L-zeolite. Overall, the broad resonance component is similar to our previous results of highly dispersed (80-96%) CO/Pt/silica or CO/Pt/alumina samples, still showing metallic characters. The principal difference is in the first moment value. The broad peak in the spectra is assigned to CO linearly bound to Pt particles in the L-zeolites, and indicates a distribution of isotropic shifts from bonding site to bonding site. The NMR results reported here manifest that the Pt particles inside of the L-zeolites channels are not collectively the same with the ones supported on silica or alumina with similar dispersion in terms of Pt particle shape and/or ordering of Pt atoms in a particle. As a result, Pt particles of CO/Pt/L-zeolite were agglomerated accompanying CO desorption upon annealing. There were no definite changes in the NMR spectra due to differences of exchanged cations. Comparison of our observation on CO/Pt/L-zeolite with Sharma et al.'s reveals that even when the first moment, the linewidtb, and the relaxation times of the static spectra and the dispersion measured by chemisorption are similar, the properties of Pt particles can be dramatically different. Therefore, it is essential to take advantage of the strengths of several techniques together in order to interpret data reliably, especially for the highly dispersed samples.

Evaluation of Selective Saturation and Refocousing Pulses in Chemical Shift NMR Imaging

  • Shin, Yong-Jin;Park, Young-Sik
    • 한국자기공명학회논문지
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    • 제4권1호
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    • pp.64-73
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    • 2000
  • There are several methods to achieve selective NMR image of differing chemical species with the three most popular methods of Dixon's, CHESS, and SECSI. A major problem common to all chemical shift imaging methods is the uniformity of the static magnetic field and distortions introduced when RF coils are loaded with a conducting specimen. Without magnetic field shimming, these methods cannot be used to acquire selectively image protons in fat and water which are separated by approximately 3.0ppm. Experiments with a phantom, with linewidths of 2.5 to 3.5ppm, were quantitatively evaluated for the three methods and a new chemical shift imaging method. In this study the new chemical shift imaging method (modified CHESS+SECSI technique) which included a selective saturation and refocusing pulse, was developed to determine the ratios of water and fat in different samples.

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