• Title/Summary/Keyword: Static NMR

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

  • Lim, Ae Ran;Lee, Kwang-Sei
    • Journal of the Korean Magnetic Resonance Society
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    • v.19 no.1
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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
    • Journal of the Korean Magnetic Resonance Society
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    • v.19 no.1
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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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    • v.34 no.3
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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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    • v.22 no.1
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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
    • Journal of the Korean Magnetic Resonance Society
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    • v.10 no.1
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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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Theory of NMR Spectoscopy and Its Application in Geoenvironmental Sciences (NMR 분광법의 원리와 지구환경과학에의 응용)

  • 김영규
    • The Journal of the Petrological Society of Korea
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    • v.10 no.3
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    • pp.233-245
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    • 2001
  • With the advent of super-conducting magnet, NMR spectroscopy becomes a very important tool in geology as well as in chemistry. $^{29}Si$ and $^{27}Al$ which are the main components of minerals and contain structural informations, are useful major targets for the NMR study in geology, but some other elements including alkali cations such as $^{23}Na$ are also one of them. NMR can be applied to many different fields. For example, it can be applied to study smaller range of structure (in molecular level) than XRD and TEM. NMR provides us with structural informations such as order-disorder in Al and Si distribution, oxygen coordination number, and distribution of other cations. Another important information that we can obtain from NMR is not only the static structural informations, but also the molecular dynamics. This dynamic informations of molecules also enable us to figure out the frequency of molecular motion and activation energy. Structure of amorphous minerals and chemistry and structure of natural organic materials are also studied by NMR.

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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
    • Journal of the Korean Magnetic Resonance Society
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    • v.20 no.4
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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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    • v.34 no.11
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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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    • v.19 no.9
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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
    • Journal of the Korean Magnetic Resonance Society
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    • v.4 no.1
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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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