• 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.

• 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.

• 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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• 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.

• 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.

• Bulletin of the Korean Chemical Society
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• 제19권2호
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• pp.178-183
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• 1998

Carbon-13 CP-MAS NMR techniques were used to investigate dynamics of new combined type liquid crystalline polymers, poly[oxy-1,4-phenyleneoxy-2-{6-(4-(4-butylphenylazo)phenoxy)hexyloxy}terephthaloyl] and poly[oxy-1,4-phenyleneoxy-2-{10-(4-(4-butylphenylazo)phenoxy)decyloxy}terephthaloyl]. Noticeable mobility change of either aromatic groups or methylene groups is not detected between 25 ℃ and 82 ℃ from 13C spinlattice relaxation time in the rotating frame (T1ρ(C)) and contact time array experiments. However, line shape analysis shows the increase of mobility of methylene carbons in poly[oxy-1,4-phenyleneoxy-2-{6-(4-(4-butylphenylazo)phenoxy)hexyloxy}terephthaloyl] at higher temperature. The dynamics of side chanis does not seem to be affected in our experimental temperature range by the length of aliphatic chain which is connecting the side chain group to the main chain.

• 분석과학
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• 제17권2호
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• pp.173-179
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• 2004

Ethylene glycol의 polymerization-complex route를 통한 졸-겔 합성법으로 안정하고 균일한 barium titanate 분말 및 박막을 제조하였다. 출발 용액으로 킬레이팅 리간드인 acetylacetone을 barium과 titanium 용액에 치환시켜 합성한 복합 산화물 졸 용액을 사용했을 때 박막을 만들 수 있었다. 졸 용액의 입자 분포도는 안정한 gaussian 분포를 보였으며, $1100^{\circ}C$에서 열처리한 겔 분말의 입자 크기는 40~77 nm이었다. 열분석 및 FT-IR, $^{13}C$ CP/MAS NMR 스펙트라와 XRD 결과로부터 (Ba-Ti)-oxycarbonate 중간상을 거쳐 $BaTiO_3$ 분말이 형성됨을 알 수 있었다. Quartz에 스핀 코팅으로 제조한 박막은 치밀하고 균열 없는 미세 조직을 보였다. $1100^{\circ}C$에서 열처리한 박막 표면의 입자 크기는 220 nm였으며 치밀한 입자 성장을 관찰할 수 있었다.

• 한국세라믹학회지
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• 제40권5호
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• pp.434-440
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• 2003

초거대 자기 저항 물질인 페로브스카이트 L $a_{0.8}$C $a_{0.2}$Mn $O_3$의 분말을 졸-겔방법으로 제조하였다. Lanthanum(III), Calcium(II) 그리고 Manganese(III) 2,4-Pentanedionate를 Propionic acid와 methane떠 혼합용매를 사용하고 PEG (l5 wt%) 용액을 첨가 하여 안정한 졸용액을 합성하였고 FT-IR spectroscopy로 반응의 진행 정도를 관찰하였다. L $a_{0.8}$C $a_{0.2}$Mn $O_3$ 겔 분말에 대해 온도를 변화시키면서 열처리하여 FT-IR, CP/MAS $^{13}$C solid state NMR spectroscopy와 XRD등을 이용해 구조변화를 관찰하였다. 열분석은 TG/DTA로 측정하였으며, FE-SEM을 통해 입자크기와 균일도를 관찰하였고, 양이온 조성 비율을 알아보기 위해 ICP-AES를 측정하였다. 자성 특성을 규명하기 위해 VSM을 이용하여 자기 모멘트를 측정하였으며, 상자기성 에서 강자기성으로 전이되는 큐리온도( $T_{c}$)를 관찰하였다.

• 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.