• Journal of the Korean Magnetic Resonance Society
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• v.14 no.2
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• pp.88-104
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• 2010

Human melanocortin-4 receptor (hMC4R) has a critical role in part of energy homeostasis, and their heterozygous mutations related in genetic cause of severe human obesity. In order to study the structure and function of these membrane proteins, it is important to prepare the samples. However, the preparation of transmembrane peptide is seriously difficult and time-consuming. Overexpression and purification of membrane proteins was reported to be difficult due to their innate insoluble and toxic properties. Among the many difficulties, the most important is the difficulty in obtaining sufficient quantities of purified protein. Recently, we succeed to produce large amounts of the second transmembrane domain from the wild-type hMC4R (wt-TM2) and D90N mutant hMC4R (m-TM2) and proposed the structural difference of them in membrane-like environments. In this paper, we demonstrate the optimization procedures to express and purify wt-TM2 or m-TM2 peptides, and solution NMR studies in different detergents to get high-resolution spectra were also described.

• Journal of the Korean Ceramic Society
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• v.45 no.5
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• pp.297-302
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• 2008

To direct the evolution of nanostructure and immobilize ${\gamma}-Al_2O_3$ catalyst, nanocrystalline La-doped-$Al_2O_3$ powder were prepared by the sol-gel process with addition of an amphiphilic block copolymer template (pluronic P123: $(poly(ethyleneoxide)_{20}-poly(propyleneoxide)_{70}-poly(ethyleneoxide)_{20})$. The dried gel is amorphous, whereas heating at temperature above $700^{\circ}C$ leads to the formation of nanocrystalline ${\gamma}$ and ${\delta}-Al_2O_3$ and these two phases is kept until $1100^{\circ}C$. ${\alpha}-A1_2O_3 $starts to form at $1200^{\circ}C$ with $LaAl_{11}O_{18}$. The surface morphology and crystal structure has been observed by field emission scanning electron microscope (FE-SEM) and X-ray diffraction (XRD). Solid state $^{27}Al$ MAS NMR indicates two types of local environment, i.e. octahedral and tetrahedral sites. The surface area and pore size was compared among these powders using the BET nitrogen adsorption measurements.

• YAKHAK HOEJI
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• v.38 no.3
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• pp.300-310
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• 1994

Physicochemical properties for the inclusion complex of chenodeoxycholic acid(CDCA) and it's $7{\beta}-hydroxy$ epimer ursodeoxycholic acid(UDCA) with ${\beta}-cyclodextrin({\beta}-CyD)$ were studied. The formation of the complex in the solid state were confimed by polarized microscopy and differential scanning calorimetry(DSC). Proton nuclear magnetic resonance$(^1H-NMR)$spectroscopy showed that CDCA and UDCA form an inclusion complex with ${\beta}-CyD$ in aqueous solution. The 1 : 1 stoichiometry of the complex was dextermined by the continuous variation method. From DSC and $^1H-NMR$ studies, there were not any differences between CDCA and UDCA. Complex of CDCA and UDCA showed increase in solubility and dissolution compared with CDCA and UDCA alone, respectively. Solubility pattern of UDCA complex was pH independent but, CDCA complex was like that of CDCA. Dissolution rate increased markedly in case of UDCA complex compared with CDCA complex, especially in acidic pH value.

• Journal of the Korean Chemical Society
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• v.43 no.5
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• pp.511-516
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• 1999

Shiff Base ligand such as [NOIPH] have been synthesized from 2-hydroxy-1-naphthaldehyde and arometic amine. Co(II), Ni(II), and Cu(II) complexes from the reaction metal salts with Tridentate Schiff Base [NOIPH] were sythesized. The ligand and metal(II) complexes were characterized by the elementary analysis, IR, UV-Vis, NMR spectra, and thermogravimetric analysis. Metal(II) complexes in solid state have been shown that the mole raio of Schiff base [NOIPH] as $N_2O$ type to Metal(II) is 2:1 and the metal(II) complexes of $N_2O$ ligand type were four-coordinated configuration.

• Journal of the Mineralogical Society of Korea
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• v.32 no.1
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• pp.41-49
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• 2019

Probing the Na environments in Na silicate and aluminosilicate glasses is essential to the macroscopic properties of melts in the Earth. In particular, exploring the atomic structure of Na silicate and aluminosilicate glasses reveals Na-O distance, which plays an important role in transport properties of melts. Here we report the local environment around Na using $^{23}Na$ magic angle spinning (MAS) NMR. We also obtain $^{23}Na$ isotropic chemical shift (${\delta}_{iso}$) of Na silicate and aluminosilicate glasses with varying composition using Dmfit program. The Q mas 1/2 model simulates the experimental results with three simulated peaks while the CzSimple model simulates with one peak. The ${\delta}_{iso}$ decreases with increasing $SiO_2$ content in Na silicate and aluminosilicate glasses. The ${\delta}_{iso}$ increases with increasing $Na_2O$ content in Na-Ca silicate and Na aluminosilicate glasses when the $SiO_2$ content is fixed. Considering the ${\delta}_{iso}$ of Na aluminosilicate glasses available in the previous studies, together with the current simulation results, we confirm that the ${\delta}_{iso}$ has positive correlation with Al / (Al + Si). Those experimental results were reproduced better using Q mas 1/2 model. The disorder of Na in Na silicate and aluminosilicate glasses can be revealed through the simulation of 1D $^{23}Na$ MAS NMR spectra using Dmfit program in a short time.

• Journal of the Korean Magnetic Resonance Society
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• v.14 no.2
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• pp.55-75
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• 2010

An ion-exchanged reaction of $MnCl_2$ with Al-incorporated solid core/mesoporous shell silica (AlSCMS) followed by calcinations generated manganese species, where average oxidation state of manganese ion is 3+, in the mesoporous materials. Dehydration results in the formation of $Mn^{2+}$ ion species, which can be characterized by electron spin resonance (ESR). The chemical environments of the manganese centers in Mn-AlSCMS were investigated by diffuse reflectance, UV-VIS and ESR spectroscopic methods. Upon drying at 323 K, part of manganese is oxidized to higher oxidation state ($Mn^{3+}$ and $Mn^{4+}$) and further increase in (average) oxidation state takes place upon calcinations at 823 K. It was found that the manganese species on the wall of the Mn-AlSCMS were transformed to tetrahedral $Mn^{3+}$ or $Mn^{4+}$ and further changed to square pyramid by additional coordination to water molecules upon hydration. The oxidized $Mn^{3+}$ or $Mn^{4+}$ species on the surfaces were reversibly reduced to $Mn^{2+}$ or $Mn^{3+}$ species or lower valances by thermal process. Mn(II) species I with a well resolved sextet was observed in calcined, hydrated Mn-AlSCMS, while Mn (II) species II with g = 5.1 and 3.2 observed in dehydrated Mn-AlSCMS. Both species I and II are considered to be non-framework Mn(II).

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.34 no.3
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• pp.79-85
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• 2024

We investigated the crystal structural property and chemical bonding nature of cellulose nanocrystal extracted directly from cotton cellulose using high-pressure homogenizer. The nanowire-like cellulose nanocrystals were randomly distributed in the form of a dense mesh. Based on calculating the interplanar distance of the Bragg-diffracted crystal plane observed through X-ray diffraction (XRD) analysis, it was found that the cellulose nanocrystals formed by high-pressure homogenizer had a monoclinc crystal structure, corresponding to the cellulose Iβ sub-polymorph. Solid-state nuclear magnetic resonance (NMR) analysis for the quantitatively evaluation of the amorphous region in cellulose nanocrystals revealed that the crystallinity index of cellulose nanocrystals was calculated to be 53.06 %. The O/C ratio of the surface of cellulose nanocrystal was estimated to be 0.82. Further analysis showed that chemical bonds of C-C bond or C-H bond, C-O bond, O-C-O bond or C=O bond, and O-C=O bond were the main chemical bonding states of the cellulose nanocrystal surface.

• The Korean Journal of Ceramics
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• v.4 no.4
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• pp.323-330
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• 1998

Mixed oxide compounds of potential usefulness for fibre coatings (hexagonal celsian, $BaAl_2Si_2O_8$ and lanthanum hexaluminate, $LaAl_{11}O_{18}$) or for matrix materials (yttrium aluminium garnet, $Y_3Al_5O_{12}$) were prepared by hybrid sol-gel synthesis and their thermal crystallisation was monitored by thermal analysis, X-ray diffraction and multinuclear solid state MAS NMR. All the gels convert to the crystalline phase below about $12200^{\circ}C$, via amorphous intermediates in which the Al shows and NMR resonance at 36-38 ppm sometimes ascribed to Al in 5-fold coordination. Additional information about the structural changes during thermal treatment was provided by $^{29}Si$, $^{137}Ba$ and $^{89}Y$ MAS NMR spectroscopy, showing that the feldspar framework of celsian begins to be established by about $500^{\circ}C$ but the Ba is still moving into its polyhedral lattice sites about $400^{\circ}C$ after the sluggish onset of crystallization. Lanthanum hexaluminate and YAG crystallise sharply at 1230 and $930^{\circ}C$ respectively, the former via $\gamma-Al_2O_3$, the latter via $YAlO_3$. Yttrium moves into the garnet lattice sites less than $100^{\circ}C$ after crystallisation.

• Bulletin of the Korean Chemical Society
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• v.30 no.3
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• pp.608-612
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• 2009

The local structures of the boron and vanadium sites in the ternary glass $xV_2O_5-B_2O_3-yNa_2O$ were studied by $^{11}B\;and\;^{51}V$ magic angle spinning (MAS) nuclear magnetic resonance (NMR). With increasing x, the mole ratios of the $BO_3\;and\;BO_4$ structures were enhanced, as were the quadrupole asymmetry parameters for the $BO_3$ structures, while the quadrupole coupling constants for the sites were reduced. However, the opposite trends were observed with increasing y, implying that $V_2O_5$ and $Na_2O$ play opposite roles. The $VO_4,\;VO_5\;and\;VO_6$ structures with all oxygens bonded to the vanadium neighbors were identified. Vanadiums bonded to the greater number of oxygens were more populated at higher contents of $Na_2O\;and\;V_2O_5$. In addition, the $VO_4$ structures with at least one oxygen bonded to boron instead of vanadium were detected at low $Na_2O$ contents. The electron densities of various vanadium oxide structures were affected by the weight densities and vanadium ion densities. The $VO_4$ structures were more likely to be vanadium oxide structures right next to $V4^{+}$ ions.

• Analytical Science and Technology
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• v.17 no.2
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• pp.173-179
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• 2004

The $BaTiO_3$ powders and thin films were prepared by an alkoxide modified sol-gel process (polymerization-complex route) using ethylene glycol. The stable starting (Ba-Ti)-mixed metal organic sol was made by addition of acetylacetone. The $BaTiO_3$ powders, which had a particle size of 40~77 nm, were crystallized from an amorphous to a tetragonal phase on annealing at 700 and $1100^{\circ}C$ for 1 h. From FT-IR, solid-state $^{13}C$ CP/MAS NMR spectroscopy and X-ray diffractometry, the trace of the Ba-Ti-oxycarbonate phase first appeared at $400^{\circ}C$. Hydrolyzed sol was spin coated on a quartz wafer at 3500 rpm for 60 s and pyrolyzed at $1100^{\circ}C$ for 1 h. After heat treatment, the coated layer became dense and smooth.