• Journal of Photoscience
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• v.9 no.2
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• pp.110-113
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• 2002

We demonstrate here a dynamic structure of bacteriorhodopsin (bR) as revealed by $^{13}$ C NMR studies on [3_$^{13}$ C]_,[1-$^{13}$ C]Ala- and/or Val-labeled wild type and a variety of site-directed mutants at ambient temperature. For this purpose, well-resolved (up to twelve) I$^{13}$ C NMR peaks were assigned with reference to the displacement of peaks due to the conformation-dependent I$^{13}$ C chemical shifts and reduced peak-intensities due to site-directed mutations. Revealed bR structure was not rigid as anticipated from 2D crystals of hexagonal array but a dynamically heterogeneous, undergoing a variety of local fluctuations depending upon specific site with frequency range of 10$^2$ -10$^{8}$ Hz. In particular, dynamics- dependent suppression of peaks turned out to be very sensitive to the motion of 10$^{-4}$ s and 10$^{-5}$ s interfered with frequency of magic angle spinning and proton decoupling, respectively. It is also noteworthy that such dynamic feature is strongly dependent upon the manner of 2D crystalline packing: $^{13}$ C NMR peaks of monomeric bR yielded either highly broadened or completely suppressed signals, depending upon the type of $^{13}$ C-labeled amino-acid residues.

• Journal of Korean Ophthalmic Optics Society
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• v.1 no.1
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• pp.1-14
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• 1996

The mixed alkali silicate glasses doped 0.1 mol% $Fe_2O_3$ are fabricated for studying the effect of transition metal oxides, which is related to the $Li^-$ ion movement in Magic-Angle-Spinning NMR. We have investigated the spin-lattice relaxation times in the room temperature and measured the $^7Li$ MAS-NMR spectrum with temperature. When the $Fe_2O_3$ oxides are added in alkali silicate glasses, the width of spectrum is changed a little but the line shape is hardly varied. For this reason, we can think that the mixed alkali effects are shown sufficiently in the spin-spin relaxation processes. However, it is not mixed alkali effects in this case. The activation energy of $Li^-$ ions are diminished in mixed alkali glasses. From the analysis of $Li^-$ diffusion environment, spin-lattice relaxation time and the nuclear magnetization, it is confirmed that the alkali mixed effects are not shown in $^7Li$ spin-lattice relaxation processes.

• Polymer(Korea)
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• v.36 no.3
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• pp.372-379
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• 2012

In this study, we treated silica nanoparticles with bis[3-(trimethoxysilyl)propyl]amine (BTMA) silane coupling agent to modify their surfaces. We investigated the effects of BTMA hydrolysis time, BTMA concentration and BTMA treatment time on the degree of silanization reaction of silica nanoparticles. We used Fourier transform infrared spectroscopy (FTIR), elemental analysis (EA) and solid state cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy (NMR) to obtain quantitative data. We found the decrease of isolated Si-OH peak intensity at 3747 $cm^{-1}$ and the increase of $-CH_2 $stretching and bending peaks with increasing hydrolysis time, concentration and treatment time of BTMA. EA analysis results also supported this trend. We found a strong effect of BTMA concentration on the degree of silanization of the silica particles, but weak effects of the hydrolysis time and the treatment time.

• Polymer(Korea)
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• v.37 no.6
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• pp.777-783
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• 2013

We used dipodal type bis[3-(trimethoxysilyl)propyl]amine (BTMA) silane coupling agent to modify silica nanoparticles to introduce secondary amino groups on the silica surface. These grafted N-H groups were reacted with glycidyl methacrylate (GMA) to introduce polymerizable methacrylate groups on the silica surface. After modification reaction, we used several analytical techniques such as Fourier transform infrared spectroscopy (FTIR), elemental analysis (EA) and solid state $^{13}C$ cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy (NMR) to analyze the effects of reaction time, reaction temperature and used GMA concentration on the modification degree between N-H groups on the silica surface and epoxide groups of GMA. We found increased introduction of methacrylate groups on the silica surface by ring opening reaction of epoxide groups of GMA with N-H groups on BTMA treated silica with increased reaction time, reaction temperature and used GMA concentration within our experimental conditions.

• Progress in Medical Physics
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• v.21 no.1
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• pp.35-41
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• 2010

The purpose of this study is to quantitate regional neurochemical profile of regional normal adult mice brain and assess regional metabolic differences by using ex vivo $^1H$ high-resolution magic angle spinning nuclear magnetic resonance spectroscopy ($^1H$ HR-MAS NMRS). The animals were matched in sex and age. The collected brain tissue included frontal cortex, temporal cortex, thalamus, and hippocampus. Quantitative 1D spectra were acquired on 40 samples with the CPMG pulse sequence (8 kHz spectral window, TR/TE = 5500/2.2 ms, NEX = 128, scan time: 17 min 20 sec). The mass of brain tissue and $D_2O$+TSP solvent were 8~14 mg and 7~13 mg. A total of 16 metabolites were quantified as follow: Acet, NAA, NAAG, tCr, Cr, tCho, Cho, GPC + PC, mIns, Lac, GABA, Glu, Gln, Tau and Ala. As a results, Acet, Cho, NAA, NAAG and mIns were showed significantly different aspects on frontal cortex, hippocampus, temporal cortex and thalamus respectively. The present study demonstrated that absolute metabolite concentrations were significantly different among four brain regions of adult mice. Our finding might be helpful to investigate brain metabolism of neuro-disease in animal model.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.21 no.1
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• pp.15-20
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• 2011

[ $^7Li$ ]Magic Angle Spinning (MAS) NMR spectroscopy has been used to study the lithium local environments in $Li_4P_2O_7$ and$LiFePO_4$ materials. The purpose of this study was to know the structure of the solid electrolyte interphase (SEI) in lithium ion cells composed of $LiFePO_4$ as cathode material. $Li_4P_2O_7$ and $LiFePO_4$ were prepared by a solid-state reaction. The $^7Li$ MAS NMR experiments were carried out at variable temperatures in order to observe the local structure changes at the temperatures in $Li_4P_2O_7$ system. The $^7Li$ MAS NMR spectra of in $Li_4P_2O_7$ indicate that the lithium local environments in $Li_4P_2O_7$ were not changed in the temperature range between $27^{\circ}C$ and $97^{\circ}C$ Through this work, we confirmed that the small amount of $Li_4P_2O_7$ less than 5.0 wt% in $LiFePO_4$ could be clearly measured by the $^7Li$ MAS NMR spectroscopy at high spinning rate over than 11 kHz.

• Journal of the Korean Magnetic Resonance Society
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• v.9 no.1
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• pp.67-73
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• 2005

$^{27}AI$ triple quantum magic angle spinning (3QMAS) NMR spectra of several mordenite (MOR) sample were simulated with the point charge model method and compared with experimental 3QMAS spectra. Signal positions from different tetrahedral (T) sites in 3QMAS spectra are mainly governed by local structures of T sites such as T-O-T angles and T-O bond lengths. When preparation methods, cations in addition to Si/Al rations vary, the local structures of T sites in MOR change enough to alter signal patterns in 3QMAS of MOR. This inhibits to study the of Al distribution variation over 4 different T sites in mordenite during process such as dealumination by 3QMAS spectra.

• Proceedings of the Polymer Society of Korea Conference
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• 2006.10a
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• pp.305-305
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• 2006

The molecular structure and dynamics of inclusion compounds (ICs) consisting of n-perfluoroalkane (PFA) guests and ${\Box}-cyclodextrin$ (${\Box}-CD$) host were investigated using $^{19}F$ magic angle spinning (MAS) and $^{1}H{\to}^{19}F$ cross polarization (CP) / MAS NMR spectroscopy with the aid of thermal analyses, FT-IR spectroscopy, X-ray diffraction, and $^{1}H{\to}^{19}F$ CP/MAS technique revealed that $C_{9}F_{20}$ molecules included in ${\Box}-CD$ undergo vigorous molecular motion and partly come out of the ${\Box}-CD$ channel above $80^{\circ}C$. In case of $C_{20}F_{42}/{\Box}-CD$, an exothermic peak is observed by differential scanning calorimetry (DSC) at ca. $40^{\circ}C$ which suggests that ${\Box}-CD$ molecules become mobile and commence rearrangements that form more ordered structures at higher temperatures.

• Bulletin of the Korean Chemical Society
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• v.30 no.5
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• pp.1077-1079
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• 2009

To minimize the variance in the quantification of solid-state phases in powder samples, gently placing polycrystalline samples one next to another directly in a sample holder is better than trying to mix them homogeneously prior to transferring to a sample holder. However, the solid-state cross polarization-magic angle spinning (CP-MAS) nuclear magnetic resonance (NMR) spectroscopy results demonstrated that it is essential in this sampling method to place all the samples in the location of consistent signal sensitivity. The same sampling method may be employed in other spectroscopic quantification techniques of solid-state phases if the method to limit the sample to the location with uniform signal sensitivity in the sample holder is adapted to each technique.

• 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.