• Title/Summary/Keyword: triple ions

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Synthesis of Ultrafine NiO/YSZ Composite Powder for Anode Material of Solid Oxide Fuel Cells (고체산화물 연료전지의 양극재료용 초미분체 NiO/YSZ 복합체 재료합성 연구)

  • 최창주;김태성;황종선;김선재
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 1999.05a
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    • pp.422-425
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    • 1999
  • Ultrafine NiO/YSZ (Yttria-Stabilized Zirconic) composite powders were prepared by using a glycine nitrate process (GNP) for anode material of solid oxide fuel cells. The specific surface areas of synthesized NiO/YSZ composite powders were examined with controlling pH of a precursor solution and the content of glycine. The binding of glycine with metal ions occurring in the precursor solution was analyzed by using FTIR. The characteristics of synthesized composite powders were examined with X-ray diffractometer, a BET method with $N_2$ absorption, scanning and transmission electron microscopies. Strongly acid precursor solution increased the specific surface area of the synthesized composite powders. This is suggested to be caused by the increased binding of metal ions and glycine under a strong acid solution of pH=0.5 that lets glycine consist of mainly the amine group of NH$_3$$^{+}$ After sintering and reducing treatment of NiO/YSZ composite powders synthesized by GNP, the Ni/YSZ pellet showed ideal microstructure very fine Ni Particles of 3-5${\mu}{\textrm}{m}$ were distributed uniformly and fine pores around Ni metal particles were formed, thus, leading to an increase of the triple phase boundary among gas, Ni and YSZ.Z.

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Simultaneous Determination of Anthraquinone, Flavonoids, and Phenolic Antidiabetic Compounds from Cassia auriculata Seeds by Validated UHPLC Based MS/MS Method

  • Girme, Aboli;Saste, Ganesh;Chinchansure, Ashish;Joshi, Swati;Kunkulol, Rahul;Hingorani, Lal;Patwardhan, Bhushan
    • Mass Spectrometry Letters
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    • v.11 no.4
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    • pp.82-89
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    • 2020
  • A systematic isolation and characterization study for Cassia auriculata (CA) seeds resulted in identifying antidiabetic compounds 1,3,8-trihydroxyanthraquinone and quercetin, quercetin-3-O-rutinoside, gallic acid, caffeic acid, ferulic acid, and ellagic acid. The ultra-high-performance liquid chromatography based triple quadrupole mass spectrometry methodology was developed and validated for simultaneous identification and confirmation of these compounds from CA seeds. Multiple reaction monitoring (MRM) based quantification method was developed with MRM optimizer software for MS1 and MS2 mass analysis. The method was optimized on precursor ions and product ions with the ion ratio of each compound. The calibration curves of seven bioactive analytes showed excellent linearity (r2 ≥ 0.99). The quantitation results found precise (RSD, < 10 %) with good recoveries (84.58 to 101.42%). The matrix effect and extraction recoveries were found within the range (91.66 to 102.11%) for the CA seeds. This is the first MS/MS-based methodology applied to quantifying seven antidiabetic compounds in CA seeds and its extract for quality control purposes.

Chmical Shift Variation of Bovine Angiogenin Upon Binding with Phosphate ions

  • Baek, Sun-Hee;Kang, Dong-Il;Lee, Jee-Young;Shin, Hang-Cheol;Kim, Yang-Mee
    • Journal of the Korean Magnetic Resonance Society
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    • v.10 no.2
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    • pp.155-162
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    • 2006
  • Angiogenin is unique among angiogenic molecules in that it is a member of the pancreatic ribonuclease superfamily and, in fact, is a ribonucleolytic enzyme. Its enzymatic activity is extremely weak compared to that of the digestive RNases but is critical for its capacity to induce neovascularization. In this study, we completed the backbone resonance assignment of bovine angiogenin using triple resonance NMR experiments of $^{15}N\;and/or\;^{13}C$ isotope labeled protein and investigated the chemical shift variation upon binding with inhibitor phosphate ion and determine the phosphate binding site.

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Linkage Positions of Oligosaccharides by Low Energy Collision Tandem Mass Spectrometry: Effect of the Addition of Metal Cations (저에너지 충돌 탄뎀 질량분석법을 이용한 올리고당의 연결부위 연구: 금속양이온의 첨가가 미치는 영향)

  • Yoo Yoon, Eunsun
    • Journal of the Korean Chemical Society
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    • v.40 no.8
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    • pp.557-564
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    • 1996
  • FAB CAD MS/MS(Fast Atom Bombardment Collision Activated Dissociation Mass Spectrometry/Mass Spectrometry) was used to study different degree of bond stability according to the linkage positions of alkali cationized $(Na^+, Li^+, K^+, NH_4^+)$ stereoisomeric and synthetic oligosaccharides. The alkali metal cations were much more stable, requiring over -40 eV of collision energy vs. only -10 eV for the protonated forms. Of the cations, the potassium cationized trisaccharides were more stable than the others. They would not yield fragment ions under the conditions of collision available in triple quadrupole. Other cationized species exhibited decreasing stability in the series $Nap^+>Li^+>NH_4^+$ using 0.8 mTorr argon pressure in the collision cell. Metal cations of the oligosaccharides maintained charge principally on the amino sugar as shown by shift of all the fragment ions containing the amino sugar. The reason for the higher stability of the metal cationized form is the formation of crown ether-like bond around metal cations, N-acetyl group on GlcNAc and oxygens on fucose moiety. Depending on the metal sizes and the conformation of linkage-isomeric region, cationized species gave linkage dependent fragment patterns and exhibited stability in the series 1-6 > 1-4 > 1-3 linkage.

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Sorption of $UO^{2+}_2$ onto Goethite and Kaolinite: Mechanistic Modeling Approach

  • Jinho Jung;Lee, Jae-Kwang;Cho, Young-Hwan;Keum, Dong-Kwon;Hahn, Pil-Soo
    • Nuclear Engineering and Technology
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    • v.31 no.2
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    • pp.182-191
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    • 1999
  • The sorption of UO$_{2}$$^{2+}$ onto goethite and kaolinite under various experimental conditions was successfully interpreted using surface complexation modeling (SCM). The SCM approach used in this work is the triple-layer model (TLM) in which weakly bonded ions are modeled as outer-sphere (ion-pair) complexes and strongly bonded ions as inner-sphere (surface coordination) complexes. The change of ionic strength did not affect the U(VI) sorption onto goethite, thus the formation of inner-sphere surface complexes, (FeO)$_2$UO$_2$ and (FeO)$_2$(UO$_2$)$_3$OH$_{5}$ was assumed to simulate the effects of ionic strength and goethite concentration. On the other hand, the U(VI) sorption onto kaolinite showed ionic strength dependence, thus the formation of AlO-UO$_{2}$$^{2+}$(outer-sphere complex) and SiO(UO$_2$)$_3$OH$_{5}$ (inner-sphere complex) was assumed to simulate the experimental data. In the presence of carbonates, the sorption of U(VI) onto kaolinite decreased in the weakly alkaline pH range. This was well simulated assuming the formation of a outer-sphere surface complex, A1OH$^{2+}$- (UO$_2$)$_2$CO$_3$OH$_3$. Since SCM approach uses thermodynamic data such as surface complexation constants, it is more predictive than empirical modeling approach in which conditional values such as partition coefficient are used. used.

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Novel Erbium(III)-Encapsulated Complexes Based on ${\pi}$-Extended Anthracene Ligands Bearing G3-Aryl-Ether Dendron: Synthesis and Photophysical Studies

  • Baek, Nam-Seob;Kim, Yong-Hee;Roh, Soo-Gyun;Lee, Dong-Hyun;Seo, Kang-Deuk;Kim, Hwan-Kyu
    • Macromolecular Research
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    • v.17 no.9
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    • pp.672-681
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    • 2009
  • A series of inert and photo-stable Er(III)-encapsulated complexes based on ${\pi}$-extended dendritic anthracene ligands bearing G3-aryl-ether dendron ([G3-AnX]-$CO_2H$), which retain different ${\pi}$-bridging systems, such as single (X= S), double (X= D) and triple (X= T) bonds was designed and synthesized to establish the structure-property relationship. The near infrared emission intensities of Er(III)-encapsulated complexes were enhanced dramatically by increasing the ${\pi}$-conjugated extension of anthracene ligands. The time-resolved luminescence spectra show monoexponential decays with a lifetime of $2.0{\sim}2.4ms$ for $Er^{3+}$ ions in thin films, and calculated intrinsic quantum yields of $Er^{3+}$ ions are in the range of $0.025{\sim}0.03%$. As a result, all Er(III)-encapsulated dendrimer complexes exhibit the near IR emission with the following order: $Er^{3+}-[G3-AnD]_3$(terpy) > $Er^{3+}-[G3-AnS]_3$(terpy) ${\approx}$ $Er^{3+}-[G3-AnT]_3$(terpy), because $Er^{3+}-[G3-AnD]_3$(terpy) has a higher relatively spectral overlap J value and energy transfer efficiency. In addition, the lack of detectable phosphorescence and no significant spectral dependence of the ${\pi}$-extended anthracene moieties on the solvent polarity support energy transfer from their singlet state to the central $Er^{3+}$ ion taking place in $Er^{3+}-[G3-AnX]_3$(terpy).

SiAlON Bulk Glasses and Their Role in Silicon Nitride Grain Boundaries: Composition-Structure-Property Relationships

  • Hampshire, Stuart;Pomeroy, Michael J.
    • Journal of the Korean Ceramic Society
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    • v.49 no.4
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    • pp.301-307
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    • 2012
  • SiAlON glasses are silicates or alumino-silicates, containing Mg, Ca, Y or rare earth (RE) ions as modifiers, in which nitrogen atoms substitute for oxygen atoms in the glass network. These glasses are found as intergranular films and at triple point junctions in silicon nitride ceramics and these grain boundary phases affect their fracture behaviour. This paper provides an overview of the preparation of M-SiAlON glasses and outlines the effects of composition on properties. As nitrogen substitutes for oxygen in SiAlON glasses, increases are observed in glass transition temperatures, viscosities, elastic moduli and microhardness. These property changes are compared with known effects of grain boundary glass chemistry in silicon nitride ceramics. Oxide sintering additives provide conditions for liquid phase sintering, reacting with surface silica on the $Si_3N_4$ particles and some of the nitride to form SiAlON liquid phases which on cooling remain as intergranular glasses. Thermal expansion mismatch between the grain boundary glass and the silicon nitride causes residual stresses in the material which can be determined from bulk SiAlON glass properties. The tensile residual stresses in the glass phase increase with increasing Y:Al ratio and this correlates with increasing fracture toughness as a result of easier debonding at the glass/${\beta}-Si_3N_4$ interface.

Manufacture Properties of the Ultrafine NiO/YSZ Solid Oxide Composite (초미분체 NiO/YSZ 고체산화물 복합재료의 제조특성)

  • 최창주;김창석;오무송;김태성
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2001.07a
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    • pp.1080-1083
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    • 2001
  • Ultrafine NiO/YSZ composite powders were prepared by using a glycine nitrate process for anode material of solid oxide fuel cells. The specific surface areas of synthesized NiO/YSZ composite powders were examined with controlling pH of a precursor solution and the content of glycine. The characteristics of synthesized composite powders were examined with X-ray diffractometer, a BET method with N$_2$absorption, scanning and transmission electron microscopy. The strongly acid precursor solution increased the specific surface area of the synthesized composite powders. This is suggested to be caused by the increased binding of metal ions and glycine under a strong acid solution of pH=0.5 that lets glycine consist of mainly the amine group of NH$_3$$\^$+/. After sintering and reducing treatment of NiO/YSZ composite powders synthesized by GNP, the Ni/YSZ pellet showed ideal micro-structure very fine Ni parties of 3-5${\mu}$m were distributed uniformly and fine pores around Ni metal particles were formed, thes, leading to an increase of the triple phase boundary among gas Ni and YSZ.

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A Study on the Fabrication of Fe-Co Magnetic Fluid from the Waste Pickling Liquor of Steel

  • Kim, Young-Sam;Lee, Jong-Heon
    • Proceedings of the IEEK Conference
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    • 2001.10a
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    • pp.149-153
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    • 2001
  • This paper describes on the fabrication of Fe-Co hydrophilic magnetic fluids from the waste pickling liquor of steel. By adding with HNO$_3$in the waste liquor oxidation is proceeded from Fe$^{3+}$ion at 6$0^{\circ}C$ with air blowing. Ultra-fine Co-ferrite particles with the mean particle size of 50 $\AA$ were produced at pH 12 after adjusting the ratio of Fe$^{3+}$Co$^{2+}$=7/3(wt%) and Fe-Co particles with the mean particle size of 94 $\AA$ were produced by reducing the Co-ferrite particle with H$_2$at the temperature of 50$0^{\circ}C$. After triple adsorption of oleic acid dodecyl benzene sulfonate(D.B.S.) and tetra methyl ammonium(T.M.A.) ions on the surface of Fe-Co particles Fe-Co hydrophilic magnetic fluid was produced by dispersing the Fe-Co particles in ethylene glycol solution. The magnetization of the Fe-Co hydrophilic magnetic fluid increased with increasing the Fe-Co concentration. The magnetic fluid containing 70% (g/cc) Fe-Co showed 73 emu/g in magnetization at the magnetic intensity of 10 kOe.kOe.e.

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Optimization of Reflectron for Kinetic and Mechanistic Studies with Multiplexed Multiple Tandem (MSn) Time-of-flight Mass Spectrometry

  • Bae, Yong-Jin;Yoon, So-Hee;Moon, Jeong-Hee;Kim, Myung-Soo
    • Bulletin of the Korean Chemical Society
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    • v.31 no.1
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    • pp.92-99
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    • 2010
  • Photoexcitation of a precursor ion inside a cell floated at high voltage installed in a tandem time-of-flight (TOF) mass spectrometer provides triple tandem mass spectrometric information and allows kinetic and mechanistic studies. In this work, the factors affecting, or downgrading, the performance of the technique were identified. Ion-optical and computational analyses showed that an optimum instrument could be designed by utilizing a reflectron with linear-plus-quadratic potential inside. Theoretical predictions were confirmed by tests with instruments built with different ion-optical layout. With optimized instruments, masses of intermediate ions in the consecutive dissociation of a precursor ion could be determined with the maximum error of $\pm5$ Da. We also observed excellent agreement in dynamical parameters (critical energy and entropy) for the dissociation of a model peptide ion determined by instruments with different ion-optical layout operated under optimum conditions. This suggests that these parameters can be determined reliably by the kinetic method developed previously when properly designed and operated tandem TOF instruments are used.