• Journal of the Korean Magnetic Resonance Society
• /
• v.19 no.1
• /
• pp.18-22
• /
• 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.

• Journal of the Korean Wood Science and Technology
• /
• v.29 no.4
• /
• pp.60-66
• /
• 2001

For examine anti-degradation factors of acetylated wood, acetylated wood was incubated on Trametes versicolor. The laccase activity was examined in broth culture and solid fermentation that contain acetylated chips. The change of acetyl groups and chemical composition in the acetylated wood having massloss analysed by $^{13}C$-CP/MAS NMR. The laccase activity was detected in broth culture. When the T. versicolor contact to acetylated wood directly, the laccase activity was very low and couldn't maintain during test periods. Through the analysing of $^{13}C$-CP/MAS NMR, the acetylation took place carbohydrates as well as lignin and hydroxyl group of amorphous region was more easily substituted that of crystalline region The spectral analyses of $^{13}C$-CP/MAS NMR were shown that introduced acetyl bond was stable against fungal attack.

• Bulletin of the Korean Chemical Society
• /
• v.32 no.10
• /
• pp.3644-3649
• /
• 2011

Multinuclear solid-state nuclear magnetic resonance (NMR) experiments were performed to investigate the local structure changes of nanoporous silica during hydrothermal treatment and surface modification with 3-aminopropyltriethoxysilane (3-APTES). The nanoporous silica was prepared by sol-gel polymerization using inexpensive sodium silicate as a silica precursor. Using $^1H$ magic angle spinning (MAS) NMR spectra, the hydroxyl groups, which play an important role in surface reactions, were probed. Various silicon sites such as $Q^2$, $Q^3$, $Q^4$, $T^2$, and $T^3$ were identified with $^{29}Si$ cross polarization (CP) MAS NMR spectra and quantified with $^{29}Si$ MAS NMR spectra. The results indicated that about 25% of the silica surface was modified. $^1H$ and $^{29}Si$ NMR data proved that the hydrothermal treatment induced dehydration and dehyroxylation. The $^{13}C$ CP MAS and $^1H$ MAS NMR spectra of 3-APTES attached on the surface of nanoporous silica revealed that the amines of the 3-aminopropyl groups were in the chemical state of ${NH_3}^+$ rather than $NH_2$.

• Journal of the Korean Magnetic Resonance Society
• /
• v.5 no.1
• /
• pp.19-28
• /
• 2001

Miscibility and morphology in blends of bisphenol-A type polycarbonate and poly (ester-ether) elastomer with different compositions are studied by solid-state NMR spectroscopy. $^{13}$ C Solid-state NMR of CP/MAS/TOSS/DD, CP/MAS/DD, inversion recovery CP/MAS/DD, and 2D rotor driven spin diffusion techniques are used to identify the miscibility, morphology, and transesterification in blends. The blends of PC /BT elastomer with 15% to 42% of soft segment seem to be single phase miscible mixing and those of PC/PBT and PC/PBT elastomer with 62% of soft segment are cocontinuous two phase immiscible mixing. No significant transesterification reactions are observed in blends with different compositions.

• Journal of the Korean Magnetic Resonance Society
• /
• v.12 no.1
• /
• pp.60-64
• /
• 2008

Cross-polarization (CP) signals were observed even from liquid samples such as neat toluene. Therefore, CP signals of liquid molecules in the presence of high surface materials do not necessarily mean the molecules are adsorbed on solid surface, especially when no signal from the tertiary observing nuclei such as carbons of the molecules is detected.

• Bulletin of the Korean Chemical Society
• /
• v.29 no.2
• /
• pp.405-407
• /
• 2008

Functionalized SAB-15 samples by octadecyltrimethoxysilane (OTC) were studied by 13C magic angle spinning (MAS) cross polarization (CP) nuclear magnetic resonance (NMR) spectroscopy. In the SBA-15 sample fully functionalized by 3-aminopropyltrimethoxysilane (APS) and OTC in 1:1 molar ratio, octadecyl chains were observed to have, on average, more trans conformation than those in the SBA-15 samples fully modified by OTC only. Our results confirm that long chain molecules tend to organize themselves better in the co-presence of short chain molecules on the surface of mesoporous materials by packing of the different length chains in an interdigitized fashion even when the short chains are long enough to have three carbons and a functional group at the ends. In addition, our results indicate that solid-state 13C CP MAS NMR spectroscopy is a simple and non-destructive method to probe the molecular structures of the domains composed of long alkyl chains.

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

• Journal of the Korean Magnetic Resonance Society
• /
• v.17 no.1
• /
• pp.19-23
• /
• 2013

The temperature dependences of the NMR spectrum and the spin-lattice relaxation times in $KH_2PO_4$ were investigated via single-crystal NMR and MAS NMR. The stretched-exponential relaxation that occurred because of the distribution of correlation times was indicative of the degree of the distribution of the double-well potential on the hydrogen bond. The behaviors responsible for the strong temperature dependences of the $^1H$ and $^{31}P$ spin-lattice relaxation times in the rotating frame $T_{1{\rho}}$ in $KH_2PO_4$ are likely related to the reorientational motion of the hydrogen-bond geometry and the $PO_4$ tetrahedral distortion.

• Korean Chemical Engineering Research
• /
• v.43 no.1
• /
• pp.71-75
• /
• 2005

$La_{0.5}Ca_{0.5}MnO_3$ colossal magnetoresistance (CMR) powders and pellets were synthesized by sol-gel process. The structural changes were investigated by FT-IR, CP/MAS $^{13}C$ solid state NMR spectroscopy and XRD. The particle characterization, microstructure of sintered samples, and cation composition of gel powders were studied by FE-SEM/EDS, TEM and ICP-AES. The structure refinement reveals that $La_{0.5}Ca_{0.5}MnO_3$ has orthorhombic, perovskite type unit cell. The magnetic characterizations were identified through measurement of magnetic moment by VSM.

• Bulletin of the Korean Chemical Society
• /
• v.30 no.9
• /
• pp.2007-2010
• /
• 2009

Donepezil hydrochloride is a reversible acetylcholinesterase inhibitor that is used in the treatment of Alzheimer’s disease to improve the cognitive performance. It shows different crystalline forms including hydrates. Therefore, it is very important to confirm the polymorphic forms in the formulations of pharmaceutical materials because polymorphs of the same drug often exhibit significant differences in solubility, bioavailability, processability and physical/chemical stability. In this paper, four different forms of donepezil hydrochloride were prepared and characterized using X-ray powder diffraction, Fourier transform infrared, and solid-state nuclear magnetic resonance (NMR) spectroscopy. This study showed that solid-state NMR spectroscopy is a powerful technique for obtaining structural information and the polymorphology of pharmaceutical solids.