• 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.

• Journal of the Korean Wood Science and Technology
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• 제29권4호
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• pp.60-66
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• 2001

아세틸화 목재를 부후균에 노출시켜 laccase의 생성을 액체배양기와 고체배양기상에서 검토하고 $^{13}C$-CP/MAS NMR 분석을 통하여 목재 내 화학성분의 변화와 치환 도입된 아세틸기의 변화를 검토하여 보았다. 액체배양기상에서 laccase의 활성은 glucose를 탄소원으로 할 때 보다 높게 나타났으며, 고체배양기상에서는 laccase 의 활성이 원활히 이루어지지 않았다. $^{13}C$-CP/MAS NMR의 분석 결과 리그닌 뿐만 아니라 셀룰로오스부분에서도 아세틸화가 이루어 졌음을 알 수 있었다. 부후된 아세틸화 목재의 분석 결과, 아세틸기의 목재내 결합이 목재 부후균 T. versicolor에 대해서 안정적이었다.

• Bulletin of the Korean Chemical Society
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• 제32권10호
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• pp.3644-3649
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• 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 $NH_2$.

• 한국자기공명학회논문지
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• 제5권1호
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• pp.19-28
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• 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.

• 한국자기공명학회논문지
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• 제12권1호
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• pp.60-64
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• 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
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• 제29권2호
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• pp.405-407
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• 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.

• 한국고분자학회:학술대회논문집
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• 한국고분자학회 2006년도 IUPAC International Symposium on Advanced Polymers for Emerging Technologies
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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.

• 한국자기공명학회논문지
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• 제17권1호
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• pp.19-23
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• 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
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• 제43권1호
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• pp.71-75
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• 2005

초거대 자기 저항 물질인 $La_{0.5}Ca_{0.5}MnO_3$의 분말과 pellet을 졸-겔 법으로 제조하였다. 열처리 온도를 변화시켜 얻은 시료에 대해 FT-IR과 CP/MAS $^{13}C$ solid state NMR spectroscopy 그리고 XRD 등을 이용해 구조변화를 관찰하였다. 양이온 조성 비율을 알아보기 위해 ICP-AES를 이용하였으며, 입자크기와 균일도를 FE-SEM/EDS로, 미세구조와 격자 패턴은 TEM으로 관찰하였다. VSM을 이용하여 자기적 특성을 살펴보았으며 큐리온도($T_c$)는 236 K에서 측정되었다.

• Bulletin of the Korean Chemical Society
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• 제30권9호
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• pp.2007-2010
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• 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.