• Journal of the Korean Magnetic Resonance Society
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• v.12 no.2
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• pp.96-102
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• 2008

Direct quantification of methanol in polymer electrolyte membrane (PEM) by solid-state nuclear magnetic resonance (NMR) spectroscopy was studied and the methanol concentrations in PEM produced by crossover and diffusion were compared. The error range of the quantification was not smaller than ${\pm}15%$ and the amount of the methanol crossed over in our direct methanol fuel cells (DMFCs) was less than the methanol diffused to PEM. The methanol concentration in the PEM of the DMFC operated at different current densities were equivalent.

• Korean Journal of Materials Research
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• v.3 no.4
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• pp.344-351
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• 1993

The crystal structunes of poly(ethylene terephthalate-eo-1, 4 cyciohexylene dimethylene terephthalate), P(ET CT), copolymers were studied by CPMAS solid state NMR spectroscopy. With the estimation of methylene resonance peaks, the bulkier CT component of the copolymer in the range of 0 20 mol% CT is excluded from the ET crystal lattice, whereas smaller ET component of the copolymer in the range of 66 100 mol% CT can be partially included into the CT crystal lattice. Those different crystallization behavior can be explained with the difference in chain bulkiness and crystal lattice dimension be tween two copolymer compurwnts.

• Journal of the Korean Chemical Society
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• v.40 no.10
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• pp.656-662
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• 1996

Using low temperature and atmospheric pressure method, we synthesized Na, TPA-ZSM-5 with Si/Al ratio of about 100. We employed 27Al and 29Si MAS NMR spectroscopy and FT-IR to investigate the crystallization process as a function of time. The chemical shift depends on the initial composition of reactants and changes during the course of synthesis different from those reported by others earlier. However, the chemical shift of our final product showed in the range of typical ZSM-5. And the defect site was removed by the calcine. From XRD and SEM data, the formation of ZSM-5 was also confirmed.

• Journal of the Korean Magnetic Resonance Society
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• v.11 no.2
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• pp.110-114
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• 2007

[ $^{31}P$ ] powder pattern spectra were measured to investigate the aspects of the interaction between the MLV (Multilamellar vesicle) and PMAP-23, a membrane of cathelicidin family and then CSAs(chemical shift anisotropy) were calculated to indentify the extent of perturbation of phospholipid mobility by the peptides. We found that acidic phospholipid interacts strongly with PMAP-23, and the analogues which modified to increase the amphipathic property showed that larger change of CSA. The analogue which introduced positive charge showed the same effects with amphipathic property.

• Analytical Science and Technology
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• v.10 no.3
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• pp.196-202
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• 1997

New vanadium(V) complex, $(NH_4)_2[VO_2NTA]$, has been synthesized and its structure has been determined by solution and solid-state NMR spectroscopies as well as X-ray crystallography. The unit cell of the monoclinic crystals contains four complexes with $a=6.923(1){\AA}$, $b=8.824(2){\AA}$, $c=19.218(11){\AA}$ and ${\beta}=91.60(3)^{\circ}$ in the space group of $P2_1/n$. The $[VO_2NTA]^{2-}$ anion has distorted octahedral geometry with cis-$VO_2$ moiety. It is confirmed that the octahedral geometry is retained in both of solution and solid-state complexes.

• Journal of Korea Technical Association of The Pulp and Paper Industry
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• v.44 no.4
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• pp.43-50
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• 2012

The crystallinity index is an important characteristic of cellulose. The crystallinity value is different depending on the adopted instrument. In this study, we determined a crystallinity index of cotton and wood celluloses using wide-angle X-ray scattering (WAXS), powder X-ray diffractometer (PXRD), and cross polarization/magic angle spinning solid-state $^{13}C$ nuclear magnetic resonance spectroscopy (CP/MAS solid-state $^{13}C$ NMR). The specimen was prepared in forms of powder, sheet and pallet. With the comparison of the obtained crystallinity indices of the cellulose, the effects of the analysis instrument, the sample preparation and analysis method were investigated. Among three instruments, the crystallinity indices by PXRD and NMR had a good relationship and reproducibility, and WAXS gave the crystallinity index with poor reproducibility. In the case of analysis methods of crystallinity indices, the Segal method showed higher value than that of the Ruland-Vonk method. We expect that this study would be applicable to evaluate the crystallinity index of various cellulose materials with accuracy and reproducibility.

• 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.

• 한국신재생에너지학회:학술대회논문집
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• 2011.05a
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• pp.146.2-146.2
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• 2011

Molecular behaviors and crystal structures of the binary hydrates of $CH_4$ and ethanol were identified by means of 13C solid-state NMR and powder XRD methods at various concentrations of ethanol. In addition, NMR peak areas were used to calculate cage occupancies for both guest species. Obtained results showed that more $CH_4$ molecules are captured into hydrate phase per unit mass of ethanol molecules because $CH_4$ molecule can occupy sII large cages more, and pure $CH_4$ hydrate can form more as well at lower ethanol concentrations. Even though tuning phenomenon was already reported for some aqueous hydrate promoters such as THF, aqueous ethanol solutions are found to play the same tuning role in the binary clathrate hydrates in this study.

• Journal of the Korean Magnetic Resonance Society
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• v.20 no.1
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• pp.27-35
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• 2016

NMR spectrometer has been regarded as essential tool for structure elucidation in variable scientific field as like organic synthesis, natural product and macro protein research. Also NMR can be applied for defining dynamic behavior like ligand and receptor binding. One of advantage of research with NMR is that to be great confident to confirm structure and the measured sample could be recovered. Nevertheless NMR also has a weak points than other spectroscopic methods that require a lot of time for interpreting acquired spectrum and running time due to low sensitivity. For last two decade Bruker has developed hardware and software solution for overcome those weak points. In order to overcome low sensitivity Bruker introduced Cryo and Micro diameter probe head technology. And researcher can reduce the time for routine spectrum processing and interpretation works due to lots of introductions in software solutions for quantification, identification and statistics analysis. With four examples, this article describing those new hardware and software solutions in field of recent pharmaceutical research as follows. - New Horizons for NMR in the Biopharmaceutical Industry - The development and application of solid-state NMR spectroscopy (SSNMR) in pharmaceutical analysis - Assisted NMR Data Interpretation in Synthetic Chemistry - Complete Analysis of New Psychoactive Substances Using NMR.

• Polymer(Korea)
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• v.38 no.2
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• pp.257-264
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• 2014

In this study, we modified silica nanoparticles with bis[3-(trimethoxysilyl)propyl]ethylenediamine (BTPED) silane coupling agent, which has two secondary amino groups in a molecule, to introduce amino groups on the silica surface. After modification of silica, we used acrylate group containing 3-(acryloyloxy)-2-hydroxypropyl methacrylate (AHM) to introduce polymerizable methacrylate groups by Michael addition reaction. We used Fourier transform infrared spectroscopy (FTIR), elemental analysis (EA) and liquid and solid state cross polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy (NMR) to understand the reactions between N-H groups of BTPED modified silica surface and acrylate groups of AHM monomer. We confirmed Michael addition reaction between BTPED modified silica and AHM completed in 2 hr reaction time. We also found increased methacrylate group introduction with increase of mol ratio of the acrylate group of AHM to N-H group of BTPED modified silica by increase of C=O peak area of measured FTIR spectra. These results were also supported by EA and solid state $^{13}C$ and $^{29}Si$ NMR results.