• Title/Summary/Keyword: Solid-state NMR

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Synthesis and Hydration Property of 3CaO.${3Al_2}{O_3}$.$CaSO_4$ Clinker by Solid State Reaction (고상반응에 의한 3CaO.${3Al_2}{O_3}$.$CaSO_4$ 클링커의 제조 및 수화)

  • 전준영;김형철;조진상;송종택
    • Journal of the Korean Ceramic Society
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    • v.37 no.5
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    • pp.459-465
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    • 2000
  • 3CaO.3Al2O3.CaSO4(C4A3)clinker was prepared by solid state reaction and then its hydration property was investigated. C4A3 clinker was fired at various temperatures in the range of 700~135$0^{\circ}C$. The hydration of it was studied by XRD, DSC, Solid-state 27Al MAS NMR and SEM. According to the results, the Ca4A3 clinker was produced by reacting calcium aluminates with CaSO4 and Al2O3 and C4A3 was formed as a main phase after calcining at 120$0^{\circ}C$. The hydration products were mainly calcium monosulfoaluminate hydrate and Al(OH)3, and they were produced after 2hrs of hydration. However the hydration rate was about 74% at 3days.

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1H Solid-state NMR Methodology Study for the Quantification of Water Content of Amorphous Silica Nanoparticles Depending on Relative Humidity (상대습도에 따른 비정질 규산염 나노입자의 함수량 정량 분석을 위한 1H 고상 핵자기 공명 분광분석 방법론 연구)

  • Oh, Sol Bi;Kim, Hyun Na
    • Korean Journal of Mineralogy and Petrology
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    • v.34 no.1
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    • pp.31-40
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    • 2021
  • The hydrogen in nominally anhydrous mineral is known to be associated with lattice defects, but it also can exist in the form of water and hydroxyl groups on the large surface of the nanoscale particles. In this study, we investigate the effectiveness of 1H solid-state nuclear magnetic resonance (NMR) spectroscopy as a robust experimental method to quantify the hydrogen atomic environments of amorphous silica nanoparticles with varying relative humidity. Amorphous silica nanoparticles were packed into NMR rotors in a temperature-humidity controlled glove box, then stored in different atmospheric conditions with 25% and 70% relative humidity for 2~10 days until 1H NMR experiments, and a slight difference was observed in 1H NMR spectra. These results indicate that amount of hydrous species in the sample packed in the NMR rotor is rarely changed by the external atmosphere. The amount of hydrogen atom, especially the amount of physisorbed water may vary in the range of ~10% due to the temporal and spatial inhomogeneity of relative humidity in the glove box. The quantitative analysis of 1H NMR spectra shows that the amount of hydrogen atom in amorphous silica nanoparticles linearly increases as the relative humidity increases. These results imply that the sample sealing capability of the NMR rotor is sufficient to preserve the hydrous environments of samples, and is suitable for the quantitative measurement of water content of ultrafine nominally anhydrous minerals depending on the atmospheric relative humidity. We expect that 1H solid-state NMR method is suitable to investigate systematically the effect of surface area and crystallinity on the water content of diverse nano-sized nominally anhydrous minerals with varying relative humidity.

Quantification of Methanol Concentration in the Polymer Electrolyte Membrane of Direct Methanol Fuel Cell by Solid-state NMR

  • Kim, Seong-Soo;Paik, Youn-Kee;Kim, Sun-Ha;Han, Oc-Hee
    • 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.

Syndecan-4 cytoplasmic domain could disturb the multilamellar vesicle

  • Kim, Suhk-Mann
    • Journal of the Korean Magnetic Resonance Society
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    • v.13 no.1
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    • pp.1-6
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    • 2009
  • Syndecan-4 cytoplasmic domain was tested to confirm the interactions with the bilayer membrane using $^{31}P$ solid-state NMR measurements. Syndecan-4 was known as a coreceptor with integrins in the cell adhesion. The syndecan-4 V region is not understood of its functional roles and tested its ability of the interaction with multilamellar vesicles. The $^{31}P$ powder pattern was dramatically changed and showed isotropic peak which imply the bilayer membrane changed its topology to the micelle-like structure. Especially, phosphatidylcholine membrane was affected this effect more than phosphatidylethanolamine membrane.

Twist Boat Conformation of Thiane S-Oxide Both in Solid State and in Solution

  • Jeon, Dong-Ju;Kim, Ikyon
    • Bulletin of the Korean Chemical Society
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    • v.29 no.7
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    • pp.1369-1373
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    • 2008
  • A stable twist boat conformation of thiane S-oxide 1a in solid state and in solution was unambiguously determined by single crystal X-ray crystallography and solution NMR analyses. On the contrary, the thiane Sdioxide 2 which was obtained from the oxidation of corresponding thiane S-oxide 1a was confirmed to adopt a regular chair conformation.

Analyses of Two Different Versions of HETCOR Techniques for Solids

  • Kim, Se-Hun;Han, Doug-Young
    • Journal of the Korean Magnetic Resonance Society
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    • v.12 no.2
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    • pp.81-88
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    • 2008
  • Solid HETCOR (Hetero-Correlation) requires homo-dipolar decoupling between proton spins during the evolution and the mixing period in 2D-NMR. There are two different ways of achieving it with pulse sequences. One is based on the multiple pulse (MP) sequence where thousands of intense radio frequency (rf) pulses are used to remove the homo-dipolar interaction between protons. The other is utilizing the so-called Lee-Goldburg (LG) off-resonance scheme where a continuous rf-irradiation is used. In this report, the advantage of one technique to the other, is analyzed. LG version is evaluated better in S/N and easier in setup procedure with the same experimental time.

Interactions of Membrane and PMAP-23 Studied by $^{31}P$ solid-state NMR Spectroscopy

  • Kim, Si-Won;Kim, Suhk-Mann
    • 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.

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X-Ray and NMR Studies of Vanadium(V)-Nitrilotriacetate Complex (바나듐(V)-니크릴로트리아세테이트 착물의 X-선 및 핵자기공명 연구)

  • Lee, Man-Ho;Jeong, Woo-Won
    • 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.

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