• Title/Summary/Keyword: elemental analysis

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Metal-Dinitrosyl Complexes(III) : Synthesis and Structural Study of Homo-, Hetero-dinuclear Molybdenum and Tungsten Complexes, $[Cl(phen)(NO)_2M({\mu}-pyz)M'(NO)_2(phen)Cl][ClO_4]_2 $(phen = 1,10-phenanthroline, pyz = pyrazine) (금속-디니트로실 착물 (제 3 보) : 몰리브덴과 텅스텐의 호모 및 헤테로 이핵 착물, $[Cl(phen)(NO)_2M({\mu}-pyz)M'(NO)_2(phen)Cl][ClO_4]_2 (phen=1,10-phenanthroline,\;pyz=pyrazine)$의 합성 및 구조에 대한 연구)

  • Sang-Oh Oh;Seong-Jong Mo
    • Journal of the Korean Chemical Society
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    • v.37 no.7
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    • pp.655-661
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    • 1993
  • The neutral monomeric compounds $[Mo(NO)_2Cl_2(phen)]$ and $[W(NO)_2Cl_2(phen)]$ (phen= 1,10-phenanthroline) have been prepared by reactions of polymeric compounds $[{Mo(NO)_2Cl_2}n],\;[{W(NO)_2Cl_2}n]$ with chelate ligands. Additions of one equivalent of silver(I) perchlorate to these cis-dinitrosyl compounds in acetone solution produce $[Mo(NO)_2(phen)(S)Cl][ClO_4]\;and\;[W(NO)_2(phen)(S)Cl][ClO_4]$ (S = acetone). The homo- and hetero-dinuclear complexes, $[Cl(phen)(NO)_2M(pyz)M'(NO)_2(phen)Cl][ClO_4]_2$ (M = Mo, W) and $[Cl(phen)(NO)_2M(pyz)M'(NO)_2(phen)Cl][C1O_4]_2$ (M = Mo, M' = W) have been prepared by these monocationic complexes with pyrazine ligand respectively. These complexes characterized by elemental analysis, $1^H-\;and\;^{13}C-NMR$, infrared, and UV-visible spectroscopy are reported. The spectral data indicate that homo- and hetero-dinuclear complexes were symmetrical structures of $C_{2v}$.

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Polyacetylene Compounds from Panax ginseng C.A. Meyer (인삼의 Polyacetylene 화합물)

  • Shim Sang Chul;Chang Suk-Ku
    • Proceedings of the Ginseng society Conference
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    • 1988.08a
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    • pp.122-128
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    • 1988
  • Several major polyacetylene compounds were isolated from the petroleum-ether fraction of fresh Korean ginseng roots through solvent fractionation. partition and silica gel column chromatography. Further separation of acetylenic compounds was accomplished by bonded normal phase HPLC utilizing a moderately nonpolar microparticulate column. The preparative separation for the various spectral measurements was carried out by low pressure preparative liquid chromatography. The chemical structure of these polyacetylenes separated was determined by UV. IR/FTIR. $^{1}H$ NMR. mass spectral and elemental analysis. These are identified to be heptadeca-1-en-4.6-diyn-3.9.l0.-triol [1] heptadeca-1.9-dien-4.6-diyn-3-ol. heptadeca-1.8-dien-4.6-diyn-3.10-diol and the 4th was denatured polyacetylene. heptadeca-1.4-dien-6.8-diyn-3.10-diol. Two different p-substituted benzoates of panaxynol were synthesized for the determination of exciton chirality. The circular dichroism spectra in the UV region show that panaxynol p-bromobenzoate and p-dimethyl-aminobenzoate constitute negative exciton chirality [2]. Isolated major polyacetylene compounds were irradiated in aerated solution with 300 nm UV light to obtain the oxidized product at the allylic alcohol center to corresponding carbonyl compounds such as heptadeca-1-en-4.6-diyn-9.10-diol-3-one and heptadeca-1.9-dien-4.6-diyn-3-one. These photooxidation compounds have en-on-diyne chromophore and undergo nucleophilic addition reaction with methanol to yield ${\beta}-methoxy$ carbonyl compounds such as heptadeca-9-en-4.6-diyn-1-methoxy-3-one and heptadeca-4.6-diyn-1-methoxy-9.10-diol-3-one.

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Simulation of Energy Resolution of Time of Flight System for Measuring Positron-annihilation induced Auger Electrons (양전자 소멸 Auger 전자 에너지 측정을 위한 Time of Flight의 분해도 향상에 관한 이론적 연구)

  • Kim, J.H.;Yang, T.K.;Lee, C.Y.;Lee, B.C.
    • Journal of the Korean Vacuum Society
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    • v.17 no.4
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    • pp.311-316
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    • 2008
  • Since the presence of the chemical impurities and defect at surfaces and interfaces greatly influence the properties of various semiconductor devices, an unambiguous chemical characterization of the metal and semiconductor surfaces become more important in the view of the miniaturization of the devices toward nano scale. Among the various conventional surface characterization tools, Electron-induced Auger Electron Spectroscopy (EAES), X-ray Photoelectron Spectroscopy (XPS) and Secondary Electron Ion Mass Spectroscopy (SIMS) are being used for the identification of the surface chemical impurities. Recently, a novel surface characterizaion technique, Positron-annihilation induced Auger Electron Spectroscopy (PAES) is introduced to provide a unique method for the analysis of the elemental composition of the top-most atomic layer. In PAES, monoenergetic positron of a few eV are implanted to the surface under study and these positrons become thermalized near the surface. A fraction of the thermalized positron trapped at the surface state annihilate with the neighboring core-level electrons, creating core-hole excitations, which initiate the Auger process with the emission of Auger electrons almost simultaneously with the emission of annihilating gamma-rays. The energy of electrons is generally determined by employing ExB energy selector, which shows a poor resolution of $6{\sim}10eV$. In this paper, time-of-flight system is employed to measure the electrons energy with an enhanced energy resolution. The experimental result is compared with simulation results in the case of both linear (with retarding tube) and reflected TOF systems.

Template-free Hydrothermal Synthesis of High Phase Purity Mordenite Zeolite Particles Using Natural Zeolite Seed for Zeolite Membrane Preparation (제올라이트 분리막 제조를 위한 유기주형 없는 고순도 모데나이트 제올라이트 입자 수열합성에 관한 연구)

  • Lee, Du-Hyoung;Alam, Syed Fakhar;Lee, Hye-Rheon;Sharma, Pankaj;Cho, Churl-Hee;Han, Moon-Hee
    • Membrane Journal
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    • v.26 no.5
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    • pp.381-390
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    • 2016
  • In this study, the natural mordenite (MOR) zeolite seeds were used for the synthesis of high purity mordenite crystals. The effect of seed concentration and crystallization time on the phase purity and surface morphology of MOR crystals has also been reported. The diffraction, elemental and scanning analysis of MOR zeolite particles obtained from 100 g hydrothermal solution batch containing 3 g natural seed, hydrothermally treated at $140^{\circ}C$ for 72 h reveal the high phase-purity of as-synthesized sample having crystals of uniform size ($1-2{\mu}m$). Moreover, high seed concentration leads to the production of mesoporous MOR particles composed of needle shape primary nano crystallites. The gases adsorption performances of as-synthesized MOR particle were carried out at $25^{\circ}C$ and 0-1 bar. Surprisingly, MOR particles show good adsorption potential for $CO_2$ (97.19 mg/g) compared to other gases. Thus it confirms that high purity MOR particles can be synthesized without using any organic template which gives an advantage of separation performance at lower price.

Preparation of Nanocomposite Metal Powders in Metal-Carbon System by Mechanical Alloying Process (기계적 합금화 방법에 의한 금속-카본계에서의 나노복합금속분말의 제조)

  • Kim, Hyun-Seung;Lee, Kwang-Min
    • Korean Journal of Materials Research
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    • v.8 no.4
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    • pp.328-336
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    • 1998
  • In metal-carbon system with no mutual solubility between matrix and alloying elements as solid or liquid phases, Cu-C-X nanocomposite metal powders were prepared by high energy ball milling for solid-lubricating bronze bearings. Elemental powder mixtures of Cu-lOwt.%C- 5wt. %Fe and Cu- lOwt. %C- 5wt. %Al were mechanically alloyed with an attritor in an argon atmosphere, and then microstructural evolution of the Cu-C-X nanocomposite metal powders was examined. It has been found that after 10 hours of MA, the approximately 10$\mu\textrm{m}$ sized Cu-C- X nanocomposite metal powders can be produced in both compositions. Morphological characteristics and microstructural evolution of the Cu-C-X powders have shown a similar MA procedure compared to those of metal-metal system. As a result of X - ray diffraction analysis, diffraction peaks of Cu and C were broaden and peak intensities were decreased as a function of MA time. Especially, the gradual disappearance of C peaks in the X- ray spectra is proved to be due to the lower atomic scattering factor of C. The calculated Cu crystallite sizes in Cu- C- X nanocomposite metal powders by Williamson- Hall equation were about lOnm size, on the other hand, the observed ones by TEM were in the range of 10 to 30nm.

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Analysis on the post-irradiation examination of the HANARO miniplate-1 irradiation test for kijang research reactor

  • Park, Jong Man;Tahk, Young Wook;Jeong, Yong Jin;Lee, Kyu Hong;Kim, Heemoon;Jung, Yang Hong;Yoo, Boung-Ok;Jin, Young Gwan;Seo, Chul Gyo;Yang, Seong Woo;Kim, Hyun Jung;Yim, Jeong Sik;Kim, Yeon Soo;Ye, Bei;Hofman, Gerard L.
    • Nuclear Engineering and Technology
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    • v.49 no.5
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    • pp.1044-1062
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    • 2017
  • The construction project of the Kijang research reactor (KJRR), which is the second research reactor in Korea, has been launched. The KJRR was designed to use, for the first time, U-Mo fuel. Plate-type U-7 wt.% Mo/Al-5 wt.% Si, referred to as U-7Mo/Ale5Si, dispersion fuel with a uranium loading of $8.0gU/cm^3$, was selected to achieve higher fuel efficiency and performance than are possible when using $U_3Si_2/Al$ dispersion fuel. To qualify the U-Mo fuel in terms of plate geometry, the first miniplates [HANARO Miniplate (HAMP-1)], containing U-7Mo/Al-5Si dispersion fuel ($8gU/cm^3$), were fabricated at the Korea Atomic Energy Research Institute and recently irradiated at HANARO. The PIE (Post-irradiation Examination) results of the HAMP-1 irradiation test were analyzed in depth in order to verify the safe in-pile performance of the U-7Mo/Al-5Si dispersion fuel under the KJRR irradiation conditions. Nondestructive analyses included visual inspection, gamma spectrometric mapping, and two-dimensional measurements of the plate thickness and oxide thickness. Destructive PIE work was also carried out, focusing on characterization of the microstructural behavior using optical microscopy and scanning electron microscopy. Electron probe microanalysis was also used to measure the elemental concentrations in the interaction layer formed between the U-Mo kernels and the matrix. A blistering threshold test and a bending test were performed on the irradiated HAMP-1 miniplates that were saved from the destructive tests. Swelling evaluation of the U-Mo fuel was also conducted using two methods: plate thickness measurement and meat thickness measurement.

Kinetic Study on the Oxidation Reaction of Alcohols by Cr(VI)-Quinoline Compound (크롬(VI)-퀴놀린 화합물에 의한 알코올류의 산화반응에 대한 반응속도론적 연구)

  • Park, Young-Cho;Kim, Soo-Jong
    • Journal of Convergence for Information Technology
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    • v.11 no.9
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    • pp.109-114
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    • 2021
  • Cr(VI)-quinoline compound[(C9H7NH)2Cr2O7] was synthesized by the reaction between of quinoline and chromium(VI) trioxide, and structure was FT-IR, elemental analysis. The oxidation ability of benzyl alcohol greatly depends upon the dielectric constant of the used organic solvent, where carbon tetrachloride was worst and N,N'-dimethylformamide was best solvent. Noticeably, in N,N'-dimethylformamide solvent, Cr(VI)-quinoline compound oxidized substituted benzyl alcohols. The Hammett reaction constant(ρ)=-0.69(303K). As a resuit, Cr(VI)-quinoline compound was found as efficicent oxidizing agent that converted benzyl alcohol, allyl alcohol, primary alcohol and secondary alcohols to the corresponding aldehydes or ketones. Cr(VI)-quinoline compound was selective oxidizing agent of benzyl alcohol, allyl alcohol and primary alcohol in the presence of secondary alcohol ones.

Corrosion Behaviors of Dental Implant Alloy after Micro-sized Surface Modification in Electrolytes Containing Mn Ion

  • Kang, Jung-In;Son, Mee-Kyoung;Choe, Han-Cheol
    • Journal of Korean Dental Science
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    • v.11 no.2
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    • pp.71-81
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    • 2018
  • Purpose: The purpose of this study was to investigate the corrosion behaviors of dental implant alloy after microsized surface modification in electrolytes containing Mn ion. Materials and Methods: $Mn-TiO_2$ coatings were prepared on the Ti-6Al-4V alloy for dental implants using a plasma electrolytic oxidation (PEO) method carried out in electrolytes containing different concentrations of Mn, namely, 0%, 5%, and 20%. Potentiodynamic method was employed to examine the corrosion behaviors, and the alternatingcurrent (AC) impedance behaviors were examined in 0.9% NaCl solution at $36.5^{\circ}C{\pm}1.0^{\circ}C$ using a potentiostat and an electrochemical impedance spectroscope. The potentiodynamic test was performed with a scanning rate of $1.667mV\;s^{-1}$ from -1,500 to 2,000 mV. A frequency range of $10^{-1}$ to $10^5Hz$ was used for the electrochemical impedance spectroscopy (EIS) measurements. The amplitude of the AC signal was 10 mV, and 5 points per decade were used. The morphology and structure of the samples were examined using field-emission scanning electron microscopy and thin-film X-ray diffraction. The elemental analysis was performed using energy-dispersive X-ray spectroscopy. Result: The PEO-treated surface exhibited an irregular pore shape, and the pore size and number of the pores increased with an increase in the Mn concentration. For the PEO-treated surface, a higher corrosion current density ($I_{corr}$) and a lower corrosion potential ($E_{corr}$) was obtained as compared to that of the bulk surface. However, the current density in the passive regions ($I_{pass}$) was found to be more stable for the PEO-treated surface than that of the bulk surface. As the Mn concentration increased, the capacitance values of the outer porous layer and the barrier layer decreased, and the polarization resistance of the barrier layers increased. In the case of the Mn/Ca-P coatings, the corroded surface was found to be covered with corrosion products. Conclusion: It is confirmed that corrosion resistance and polarization resistance of PEO-treated alloy increased as Mn content increased, and PEO-treated surface showed lower current density in the passive region.

Effect of Low Temperature Heat Treatment on the Physical and Chemical Properties of Carbon Anode Materials and the Performance of Secondary Batteries (저온 열처리가 탄소 음극재의 물리·화학적 특성 및 이차전지 성능에 미치는 영향)

  • Whang, Tae Kyung;Kim, Ji Hong;Im, Ji Sun;Kang, Seok Chang
    • Applied Chemistry for Engineering
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    • v.32 no.1
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    • pp.83-90
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    • 2021
  • In this study, effects of the physical and chemical properties of low temperature heated carbon on electrochemical behavior as a secondary battery anode material were investigated. A heat treatment at 600 ℃ was performed for coking of petroleum based pitch, and the manufactured coke was heat treated with different heat temperatures at 700~1,500 ℃ to prepare low temperature heated anode materials. The physical and chemical properties of carbon anode materials were studied through nitrogen adsorption and desorption, X-ray diffraction (XRD), Raman spectroscopy, elemental analysis. Also the anode properties of low temperature heated carbon were considered through electrochemical properties such as capacity, initial Coulomb efficiency (ICE), rate capability, and cycle performance. The crystal structure of low temperature (≤ 1500 ℃) heated carbon was improved by increasing the crystal size and true density, while the specific surface area decreased. Electrochemical properties of the anode material were changed with respect to the physical and chemical properties of low temperature heated carbon. The capacity and cycle performance were most affected by H/C atomic ratio. Also, the ICE was influenced by the specific surface area, whereas the rate performance was most affected by true density.

Characterization of Charcoals prepared by Korean Traditional Kiln (우리나라 전통 숯가마로부터 생산된 숯의 특성분석)

  • An, Ki Sun;Kwak, Lee Ku;Kim, Hong Gun;Ryu, Seung Kon
    • Korean Chemical Engineering Research
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    • v.60 no.2
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    • pp.208-216
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    • 2022
  • Surface morphology and adsorption characteristics of black and white charcoals prepared from Korean traditional kiln were quantitatively analyzed. TGA and elemental analysis of charcoals were different from produced kiln, and thermal degradation temperature and carbon content of white charcoals were apparently higher than those of black charcoals. Surface morphology shows the activation progressed through the longitudinal direction of woods and new micropores were developed to radial direction on the surface of macropores as the furthermore activation resulting in the pore connection. BET adsorption isotherms show that there are low-pressure hysteresis due to the no desorption of adsorbates, which resulted in unique Type of charcoals overlapping Type I and Type IV. Such a low-pressure hysteresis is occurred from expansion of adsorbates, which were embedded in the micropore entrances and did not get out during the desorption run. The characteristics of charcoals such as specific surface area and pore size distribution did not show correct values depending on not only produced company but also sampling sites of one piece of charcoal. Therefore, it is not easy to suggest the quantitative characteristics of charcoals prepared from Korean traditional kiln. On the other hand, preparation the quality standard of charcoal is necessary for their special uses such as adsorbent.