• Title/Summary/Keyword: elemental analysis

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Studies on the Metal Complexes with the Tetradentate Schiff Base Ligand (네자리 Schiff Base 리간드의 금속착물에 관한 연구)

  • Chjo Ki Hyung;Oh Sang-Oh;Kim Chan-ho
    • Journal of the Korean Chemical Society
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    • v.18 no.3
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    • pp.194-201
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    • 1974
  • The tetradentate schiff base ligand, N,N'-bis(salicylaldehyde)-m-phenylenediimine has been prepared from salicylaldehyde and m-phenylenediamine by Duff-reaction. The schiff base ligand has been reacted with Cu(II), Ni(II), Co(II), and Zn(II) to form new complexes; Cu(II)$[C_{20}H_{14}O_2N_2]{\cdot}2H_2O, Ni(II)[C_{20}H_{14}O_2N_2]{\cdot}2H_2O, Co(III)[C_{20}H_{14}O_2N_2]{\cdot}2H_2O and Zn(II)2[C_{20}H_{14}O_2N_2]{\cdot}4H_2O$. It seems to be that the Cu(II), Ni(II) and Co(II) complexes have hexacoordinated configuration with the schiff base and two molecules of water, while Zn(II) complex has tetracoordinated configuration with the schiff base and four molecules of water. The mole ratio of tetradentate schiff base ligand to Cu(II), Ni(II) and Co(II) are 1:1 but to Zn(II) is 1:2. These complexes have been identified by visible spectra, infrared spectra, T.G.A. and elemental analysis.

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Studies on the Cu (II), Ni (II) and Zn (II) Complexes with Tridentate Schiff Base Ligand (I) (세자리 Schiff Base 리간드의 Cu (II), Ni (II) 및 Zn (II) 착물에 관한 연구 (제1보))

  • Chjo Ki Hyung
    • Journal of the Korean Chemical Society
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    • v.18 no.3
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    • pp.189-193
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    • 1974
  • The tridentate schiff base, salicylidene imino-o-thiolbenzene, has been synthetized from salicylaldehyde and o-amino thiolbenzene by Duff reaction. The schiff base has been reacted with Cu(II), Ni(II), and Zn(II), to form new complexes; Cu(II)$[C_{13}H_9ONS]{\cdot}3H_2O$, Ni(II)$[C_{13}H_9ONS]{\cdot}3H_2O,\;Zn(II)[C_{13}H_9ONS]{\cdot}3H_2O$ It appears that the Cu(II)-complex has tetra-coordinated configuration with the schiff base and one molecule of water, while the Ni(II) and Zn(II)-complexes have hexacoordinated configuration with the schiff base and three molecules of water. The mole ratio of tridentate schiff base ligand to metals was 1:1. These complexes have been identified by infrared spectra, visible spectra, TGA, DTA and elemental analysis.

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Photocycloaddition Reaction of 4',5'-Dihydropsoralen to Tetramethylethylene (4',5'-디히드로소랄렌과 테트라메틸에틸렌의 광고리화 첨가반응에 관한 연구)

  • Sang Chul Shim;Jong Sung Koh
    • Journal of the Korean Chemical Society
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    • v.26 no.3
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    • pp.172-178
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    • 1982
  • A psoralen-DNA monoadduct analogue, 4',5'-dihydropsoralen (DHP) is synthesized and its photophysical properties such as fluorescence quantum yield (0.08), phosphorescence quantum yield (0.013), fluorescence lifetime (0.95ns), and phosphorescence lifetime(0.039s) were measured in ether solution and in frozen matrix state at 77K. The photocycloaddition reaction of DHP with tetramethylethylene(TME) was carried out in solution and in the frozen state. The major photoadduct was isolated and characterized by elemental analysis and physical methods such as UV, IR, NMR, and mass spectrometry. The major DHP-TME photoadduct was proved to be an 1 : 1 $C_4$-cycloadduct formed through 2 + 2 cycloaddition of the pyrone double bond of DHP to TME.

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Synthesis and Characterization of Molybdenum and Tungsten Oxo-Nitrosyl Complexes Containing ${Mo(NO)_2}^{2+}$ Unit with Isobutyl- and n-Butylamidoxime (이소부틸과 부틸아미드옥심으로한 ${Mo(NO)_2}^{2+}$ 단위체가 포함하는 몰리브덴과 텅스텐 산소-니트로실 착물의 합성과 성질)

  • Roh, Soo Gyun;Oh, Sang Oh
    • Journal of the Korean Chemical Society
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    • v.39 no.5
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    • pp.393-398
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    • 1995
  • The oxo-nitrosyl complexes (n-Bu4N)2[M4O12Mo(NO)2{RC(NH2)NHO}2{RC(NH)NO}2] (M=Mo, W; R=(CH3)2CH, n-CH3CH2CH2) have been prepared by the reactions of monomeric complex containing {Mo(NO)2}2+ and polyoxometalates with isobutyl- and n-butylamidoxime. The prepared complexes were characterized by elemental analysis, infrared, 1H NMR, 13C NMR and UV-visible spectroscopy. These complexes contain two {M2O5}2+ [M=Mo, W] cores and a central {Mo(NO)2}2+ core. The {Mo(NO)2}2+ unit was the formally cis type and C2v symmetry in geometric structure. The two {M2O5}2+ cores and a central {Mo(NO)2}2+ core were not nearly interacted with electronic localization, which were identified by spectroscopy.

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Preparation of Cucurbituril Anchored Silica Gel by Cross Polymerization and Its Chromatographic Applications

  • Cheong, Won-Jo;Go, Joung-Ho;Baik, Yoon-Suk;Kim, Sung-Soon;Nagarajan, Erumaipatty R;Selvapalam, Narayanan;Ko, Young-Ho;Kim, Ki-Moon
    • Bulletin of the Korean Chemical Society
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    • v.29 no.10
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    • pp.1941-1945
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    • 2008
  • A new chromatographic stationary phase has been prepared by cross polymerization between allylsilica and perallyloxycucurbit[6]uril and characterized by elemental analysis and FT-IR spectroscopy. The double endcapping has been proven to improve the separation efficiency of the cucurbituril-based stationary phase material. The first end-capping was carried out when allylsilica was made. The second end-capping was done as the final step of the whole process, and the use of a mixture of hexamethyldisilazane (HMDS) and trimethylchlorosilane (TMCS) as an end-capping reagent was found better than the use of only HMDS or TMCS. Our stationary phase has shown generally good results in separation of nonpolar and polar analytes. This phase showed even better separation performance than the commercial C18 phase for the case where hostguest chemistry was properly incorporated in solute retention.

Synthesis and Electrochemical Characterization of Silica-Manganese Oxide with a Core-shell Structure and Various Oxidation States

  • Ryu, Seong-Hyeon;Hwang, Seung-Gi;Yun, Su-Ryeon;Cho, Kwon-Koo;Kim, Ki-Won;Ryu, Kwang-Sun
    • Bulletin of the Korean Chemical Society
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    • v.32 no.8
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    • pp.2683-2688
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    • 2011
  • Silica-manganese oxides with a core-shell structure were synthesized via precipitation of manganese oxides on the $SiO_2$ core while varying the concentration of a precipitation agent. Elemental analysis, crystalline property investigation, and morphology observations using low- and high-resolution electron microscopes were applied to the synthesized silica-manganese oxides with the core-shell structure. As the concentration of the precipitating agent increased, the manganese oxide shells around the $SiO_2$ core sequentially appeared as $Mn_3O_4$ particles, $Mn_2O_3+Mn_3O_4$ thin layers, and ${\alpha}-MnO_2$ urchin-like phases. The prepared samples were assembled as electrodes in a supercapacitor with 0.1 M $Na_2SO_4$ electrolyte, and their electrochemical properties were examined using cyclic voltammetry and charge-discharge cycling. The maximum specific capacitance obtained was 197 F $g^{-1}$ for the $SiO_2-MnO_2$ electrode due to the higher electronic conductivity of the $MnO_2$ shell compared to those of the $Mn_2O_3$ and $Mn_3O_4$ phases.

Preparation and capacitance properties of graphene based composite electrodes containing various inorganic metal oxides

  • Kim, Jeonghyun;Byun, Sang Chul;Chung, Sungwook;Kim, Seok
    • Carbon letters
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    • v.25
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    • pp.14-24
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    • 2018
  • Electrochemical properties and performance of composites performed by incorporating metal oxide or metal hydroxide on carbon materials based on graphene and carbon nanotube (CNT) were analyzed. From the surface analysis by field emission scanning electron microscopy and field emission transmission electron microscopy, it was confirmed that graphene, CNT and metal materials are well dispersed in the ternary composites. In addition, structural and elemental analyses of the composite were conducted. The electrochemical characteristics of the ternary composites were analyzed by cyclic voltammetry, galvanostatic charge-discharge tests, and electrochemical impedance spectroscopy in 6 M KOH, or $1M\;Na_2SO_4$ electrolyte solution. The highest specific capacitance was $1622F\;g^{-1}$ obtained for NiCo-containing graphene with NiCo ratio of 2 to 1 (GNiCo 2:1) and the GNS/single-walled carbon $nanotubes/Ni(OH)_2$ (20 wt%) composite had the maximum specific capacitance of $1149F\;g^{-1}$. The specific capacitance and rate-capability of the $CNT/MnO_2/reduced$ graphene oxide (RGO) composites were improved as compared to the $MnO_2/RGO$ composites without CNTs. The $MnO_2/RGO$ composite containing 20 wt% CNT with reference to RGO exhibited the best specific capacitance of $208.9F\;g^{-1}$ at a current density of $0.5A\;g^{-1}$ and 77.2% capacitance retention at a current density of $10A\;g^{-1}$.

Empirical relationship between band gap and synthesis parameters of chemical vapor deposition-synthesized multiwalled carbon nanotubes

  • Obasogie, Oyema E.;Abdulkareem, Ambali S.;Mohammed, Is'haq A.;Bankole, Mercy T.;Tijani, Jimoh. O.;Abubakre, Oladiran K.
    • Carbon letters
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    • v.28
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    • pp.72-80
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    • 2018
  • In this study, an empirical relationship between the energy band gap of multi-walled carbon nanotubes (MWCNTs) and synthesis parameters in a chemical vapor deposition (CVD) reactor using factorial design of experiment was established. A bimetallic (Fe-Ni) catalyst supported on $CaCO_3$ was synthesized via wet impregnation technique and used for MWCNT growth. The effects of synthesis parameters such as temperature, time, acetylene flow rate, and argon carrier gas flow rate on the MWCNTs energy gap, yield, and aspect ratio were investigated. The as-prepared supported bimetallic catalyst and the MWCNTs were characterized for their morphologies, microstructures, elemental composition, thermal profiles and surface areas by high-resolution scanning electron microscope, high resolution transmission electron microscope, energy dispersive X-ray spectroscopy, thermal gravimetry analysis and Brunauer-Emmett-Teller. A regression model was developed to establish the relationship between band gap energy, MWCNTs yield and aspect ratio. The results revealed that the optimum conditions to obtain high yield and quality MWCNTs of 159.9% were: temperature ($700^{\circ}C$), time (55 min), argon flow rate ($230.37mL\;min^{-1}$) and acetylene flow rate ($150mL\;min^{-1}$) respectively. The developed regression models demonstrated that the estimated values for the three response variables; energy gap, yield and aspect ratio, were 0.246 eV, 557.64 and 0.82. The regression models showed that the energy band gap, yield, and aspect ratio of the MWCNTs were largely influenced by the synthesis parameters and can be controlled in a CVD reactor.

Interface Analysis of Cu(In,Ga)Se2 and ZnS Formed Using Sulfur Thermal Cracker

  • Cho, Dae-Hyung;Lee, Woo-Jung;Wi, Jae-Hyung;Han, Won Seok;Kim, Tae Gun;Kim, Jeong Won;Chung, Yong-Duck
    • ETRI Journal
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    • v.38 no.2
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    • pp.265-271
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    • 2016
  • We analyzed the interface characteristics of Zn-based thin-film buffer layers formed by a sulfur thermal cracker on a $Cu(In,Ga)Se_2$ (CIGS) light-absorber layer. The analyzed Zn-based thin-film buffer layers are processed by a proposed method comprising two processes - Zn-sputtering and cracker-sulfurization. The processed buffer layers are then suitable to be used in the fabrication of highly efficient CIGS solar cells. Among the various Zn-based film thicknesses, an 8 nm-thick Zn-based film shows the highest power conversion efficiency for a solar cell. The band alignment of the buffer/CIGS was investigated by measuring the band-gap energies and valence band levels across the depth direction. The conduction band difference between the near surface and interface in the buffer layer enables an efficient electron transport across the junction. We found the origin of the energy band structure by observing the chemical states. The fabricated buffer/CIGS layers have a structurally and chemically distinct interface with little elemental inter-diffusion.

Studies on the Molybdenum Complexes with Tridentate Schiff Base Ligand (I) (세자리 Schiff Base 리간드의 몰리브덴 착물에 관하여 (제1보))

  • Ki Hyung Chjo
    • Journal of the Korean Chemical Society
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    • v.17 no.3
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    • pp.169-173
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    • 1973
  • The tridentate schiff base ligand, salicyliden amino-o-hydroxy benzene, has derived from salicylaldehyde and o-amino phenol. This ligand reacts with a series of Mo (VI), Mo (V), Mo (IV), and Mo (III) oxidated states and forms a new complexes; [Mo O$_2(H_2O)\;(C_{13}H_9O_2N)]$, [MoO Cl$(H_2O)\;(C_{13}H_9O_2N)]$, [Mo(SCN)$_2(H_2O)\;(C_{13}H_9O2_N)]$$[Mo(H_2O)_2\;(C_{13}H_9O_2N)]_2O$. The Mo (VI), Mo(V) and Mo(Ⅳ) ions in these complexes are octahedron, hexa coordinate, and the mole ratio of these ions to the ligand are 1 : 1, but Mo (III) Complex is a Mo-O-Mo oxygen bridge bond and polynuclear, and the mole ratio of Mo (III) to the ligand 1 : 1 above facts are identified from the data of Infrared spectra, visible spectra, and elemental analysis.

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