• Title/Summary/Keyword: Spectroscopic characterization

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Synthesis and Characterization of Ir(H)(CO)(PEt3})22-C60)

  • Lee, Chang-Yeon;Lee, Gae-Hang;Kang, Hong-Kyu;Park, Bo-Keun;Park, Joon-T.
    • Bulletin of the Korean Chemical Society
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    • v.28 no.11
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    • pp.1958-1962
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    • 2007
  • The title complex, Ir(H)(CO)(PEt3)2(η 2-C60) (2), has been prepared by the reaction of excess C60 (4 equiv) with a tetrairidium complex Ir4(CO)8(PEt3)4 (1) in refluxing chlorobenzene in 40% yield as green crystals. Compound 2 has been characterized by cyclic voltammetry (CV), spectroscopic methods (mass, IR, 1H and 31P NMR), and a single crystal X-ray diffraction study. The molecular structure reveals that the iridium atom of 2 is coordinated by two axial ligands of a hydrogen atom and a carbonyl group, and three equatorial ligands of two phosphorus atoms and an η 2-C60 moiety. The CV study exhibits three reversible one-electron redox waves for the successive reductions of 2, together with additional four redox waves due to free C60 reductions, which was formed by decomposition of 2 in the reduced states. The three reversible redox waves of 2 are shifted to more negative potentials by ca. 270 mV compared to free C60, reflecting both metal-to-C60 π-back-donation and the electron-donating nature of the two phosphorus ligands.

Synthesis and Characterization of Molybdeum Complexes with Schiff-Bases(II), Dioxobis(N-aryl-3-methoxysalicyaldiminato) Molybdenum(VI) Complexes (몰리브덴의 시프-염기착물의 합성과 그 성질 (제2보). 다이옥소비스(질소-아릴-3-메톡시살리실알디미나토)몰리브데늄(VI) 착물)

  • O, Sang O;Gu, Bon Gwon
    • Journal of the Korean Chemical Society
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    • v.29 no.3
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    • pp.257-264
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    • 1985
  • Dioxobis(3-methoxysalicyaldehydato)molybdeum(VI) complex has been synthesized by reactions of 3-methoxysalicylaldehyde and ammonium paramolybdate in methanol solution. With appropriate primary amine, the resulting complex gave schiff-base complexes, MoO$_2$(CH$_3$O-sal-N-R)$_2$ in which C=O oxide ligands had been replaced by nitrogen. The properties and possible molecular structure of these complexes were discussed by elemental analysis, spectroscopic studies and electric conductivities measurements. It was found that the Mo(VI) complexes contain a cis-MoO$_2$ group since their infrared spectra two Mo=O band at about 900cm$^{-1}$ and the combining ratios for MoO$_2$-ligand are 1 : 2. Also, electronic spectra of molybdenyl complexes assigned to ligand-to-metal charge transfer transition. All of these complexes are yellow or orange, depolar compound and slightly soluble in alcohol, dichloromethane, chloroform and N,N-dimethylformamide.

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Synthesis and Characterization of Molybdenum (V)-1, 6-Diaminohexane-N, N, N', N'-tetraacetic Acid Derivatives Complexes (몰리브덴 (V) 와 1, 6-Diaminohexane-N, N, N', N'-tetraacetic Acid 계 착물합성과 그 성질)

  • Sang Oh Oh;Sig Young Choi
    • Journal of the Korean Chemical Society
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    • v.33 no.1
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    • pp.90-96
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    • 1989
  • A new series of $dioxo-di-{\mu}-oxo-dimolybdate(V)(*image)$, has been prepared by the reaction of pyridinum oxoisothiocyanato-molybdate(V) with 1, 6-diaminohexane-N, N, N', N'-tetraacetic acid derivatives containing amine carboxyl groups. The properties and possible molecular structure of these complexes were discussed by elemental analysis, spectroscopic studies and magnetic susceptibility measurements. The infrared spectra of these complexes show two strong Mo=$O_t$ stretching modes in the $900-965cm^{-1}$, MoO$_2$Mo stretching bands at around 450∼500 and $740-765 cm^{-1}$ to symmetrical and asymmetrical O-bridge stretching, a coordinated $COO^-$ asymmetrical band in the $1600-1635 cm^{-1}$. The complexes synthesized were yellow or orange and diamagnetic.

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Synthesis and Characterization of Molybdenum(V)-Iminodiaceticacid Derivatives Complexes (몰리브덴(V)와 이미노디아세틱액시드계 착물 합성과 그 성질)

  • Sang-Oh Oh;Sik-Young Choi
    • Journal of the Korean Chemical Society
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    • v.31 no.6
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    • pp.520-526
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    • 1987
  • A new series of $dioxo-di-\mu-oxo-dimolybdate(V)$, has been prepared by reaction of pyridinum oxoisothiocyantomolybdate (V) with iminodiacetic acid derivatives containing amine carboxyl groups. The properties and possible molecular structure of these complexes were discussed by elemental analysis, spectroscopic studies and magnetic susceptibility measurements. The infrared spectra of these complexes all show two strong $Mo=O_t$ stretching bands in the 900∼$980cm^{-1}$, $MoO_2Mo$ very prominent strectching bands at around 410~425 and 735~$750cm^{-1}$ to symmetrical and asymmetrical O-bridge stretching, a coordinated $coo^-$ asymmetrical band in the 1585∼$1,640cm^{-1}$. Also, d-d transition of molybdenyl complexes corresponding to $^2B_2{\to}^2B_1$ occured in the 24,800~$28,000cm^{-1}$ region, charge transfer transition corresponding to ligand-to-molybdenum in the 32,500~33,800, 42,000~$47,500cm^{-1}$ region. The complexes synthesized were yellow or orange and diamagnetic.

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The Effect of Powder Oxidation on the Thermoelectric Properties of β-FeSi2 (β-FeSi2의 열전변환특성에 미치는 분말산화의 영향)

  • ;Kunihito Koumoto
    • Journal of the Korean Ceramic Society
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    • v.40 no.11
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    • pp.1106-1112
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    • 2003
  • For the purpose of making clear the role of oxygen in the thermoelectric properties of FeSi$_2$, thermoelectric measurements and spectroscopic characterization were conducted for the oxidized specimens fabricated from ($\alpha$+$\varepsilon$)-phases and/or $\beta$-phase. Addition of oxygen to FeSi$_2$ prevented both densification during sintering and transformation from metallic phases to semiconducting phase during annealing treatment. In an specimens, electrical conductivity and thermal conductivity decreased with oxidation time. The Seebeck coefficient was positive and small for pure FeSi$_2$. And/or the oxidized specimens fabricated from ($\alpha$+$\varepsilon$)-phases. However, it was negative and showed a maximum peak at about 500 K for the oxidized FeSi$_2$ fabricated from $\beta$-phase. The value of maximum peak increased with oxidation time.

Characterization of saturation of CR-39 detector at high alpha-particle fluence

  • Ghazaly, M. El;Hassan, Nabil M.
    • Nuclear Engineering and Technology
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    • v.50 no.3
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    • pp.432-438
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    • 2018
  • The occurrence of saturation in the CR-39 detector reduces and limits its detection dynamic range; nevertheless, this range could be extended using spectroscopic techniques and by measuring the net bulk rate of the saturated CR-39 detector surface. CR-39 detectors were irradiated by 1.5 MeV high alpha-particle fluence varying from $0.06{\times}10^8$ to $7.36{\times}10^8\;alphas/cm^2$ from Am-241 source; thereafter, they were etched in a 6.25N NaOH solution at a temperature of $70^{\circ}C$ for different durations. Net bulk etch rate measurement of the 1.5 MeV alpha-irradiated CR-39 detector surface revealed that rate increases with increasing etching time and reaches its maximum value at the end of the alpha-particle range. It is also correlated with the alpha-particle fluence. The measurements of UV-Visible (UV-Vis) absorbance at 500 and 600 nm reveal that the absorbance is linearly correlated with the fluence of alpha particles at the etching times of 2 and 4 hour. For extended etching times of 6, 10, and 14.5 hour, the absorbance is saturated for fluence values of $4.05{\times}10^8$, $5.30{\times}10^8$, and $7.36{\times}10^8\;alphas/cm^2$. These new methods pave the way to extend the dynamic range of polymer-based solid state nuclear track detectors (SSNTDs) in measurement of high fluence of heavy ions as well as in radiation dosimetry.

New Transition Metal Mediated Alkylation Reaction of arachno-$S_{2}B_{7}H_{8}$, Insertion Reaction of arachno-$S_{2}B_{7}H_{8}^{-}$ with $(CO)_{5}M$ {${C(R_{1})(R_{2})}$} $(M=Cr,\;W;\;R_{1}=CH_{3},\;C_{6}H_{5};\;R_{2}=OCH_{3},\;SC_{6}H{5})$: Synthesis and Characterization of arachno-$4-RCH_{2}-6,8-S_{2}B_{7}H_{8}\;(R=CH_{3},\;IIa;\;C_{6}H_{5},\;IIb)$

  • Hee-Joo Jeon;Jae-Jung Ko;Kang-bong Lee;Sang Ook Kang
    • Bulletin of the Korean Chemical Society
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    • v.14 no.1
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    • pp.113-117
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    • 1993
  • Good yield synthetic routes for the production of new B-alkyl-dithiaborane clusters are reported. The syntheses of the B-alkyl-dithiaboranes are based on the use of Fischer-type carbene reagents to activate the B-H bonds of dithiaborane for alkyl-addition reactions and are the first examples of transition-mediated reactions of dithiaborane to be reported. Thus, reactions employing arachno-$S_2B_7H_8$- and $(CO)_5M{C(R_1)R_2}$ (M = Cr, W; $R_1 = CH_3,\;C_6H_5;\; R_2 = OCH_3,\;SC_6H_5)$ were found to yield the intermidiate anions I, $[(CO)_5M{C(R_1)R_2S_2B_7H_8}]^-$, which upon protonation gave the corresponding neutral, air-sensitive cluster arachno-4-$RCH_2-6,8-S_2B_7H_8(R=CH_3,\;IIa;\;C_6H_5,\;IIb)$ range from 30 to 35% yield. Complexes IIa and IIb are isoelectronic with arachno-6,8-$S_2B_7H_9$ and, on the basis of the spectroscopic data, are proposed to adopt a similar arachno cage geometry in which an $RCH_2$ units are substituted to 4 position boron atom of the arachno-6,8-$S_2B_7H_9$.

Synthesis, Characterization, and Catalytic Properties of Gp 6 Metal Complexes of 1-N,N-dimethylaminomethyl-$1^{\prime}$,2-bis(diphenylphosphino)ferrocene (FcNPP). X-ray Crystal Structure of W$(CO)_4({\eta}^2-FcNPP(O)-P,N)$

  • Kim, Tae-Jeong;Kim, Yong-Hoon;Kim, Eun-Jin;Oh, Sang-Ho;Kim, Hong-Seok;Jeong, Jong-Hwa
    • Bulletin of the Korean Chemical Society
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    • v.15 no.5
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    • pp.379-386
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    • 1994
  • Reactions of 1',2-bis(diphenylphosphino)-l-(N,N-dimethylaminomethyl)ferrocene (FcNPP) with $M(CO)_6$ (M=Cr, Mo, W) in the presence of TMNO (Trimethylamine oxide) in a stoichiometric ratio of 1 : 1.5 : 3.5 produced a series of Gp 6 metal carbonyl derivatives with a variety of coordination modes: M(CO)$_4({\eta}^2$-FcNPP-P,P) (M=Cr, Mo, W), $M(CO)_5({\eta}^1-FcNPP-P) (M=Mo, W)\;,\; M_2(CO)_9({\eta}^1\;,\;{\eta}^2-FcNPP-P,P,N) (M=Cr, Mo)\;,\;M_2(CO)_{10}({\eta}^1\;,\;{\eta}^1-FcNPP-P,P) (M=Cr, Mo, W)\;, and\;W(CO)_4({\eta}^2-FcNPP(O)-P,N)$. All these complexes were characterized by microanalytical and spectroscopic techniques. In one case, the structure of W(CO)$_4({\eta}^2$-FcNPP(O)-P,N) was determined by X-ray crystallography. Crystals are monocinic, space group P$2_{1/C}$, with a=10.147(2), b=19.902(3), c=19.821(4) ${\AA},\;{\beta}=96.88(2)^{\circ},\;V=3974(l){\AA}^3$, Z=4, and $D_{calc}=1.64 g cm^{-3}$. The geometry around the central tungsten metal is a distorted octahedron, with the nitrogen and phosphorus atoms being cis to each other. Some of these complexes exhibited catalytic activities in the allylic oxidation and epoxidation of cholesterly acetate. Other oxidation products were also formed with the different chemical yields and product distribution depending upon the ligand and the central metal.

Polarization Phase-shifting Technique for the Determination of a Transparent Thin Film's Thickness Using a Modified Sagnac Interferometer

  • Kaewon, Rapeepan;Pawong, Chutchai;Chitaree, Ratchapak;Bhatranand, Apichai
    • Current Optics and Photonics
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    • v.2 no.5
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    • pp.474-481
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    • 2018
  • We propose a polarization phase-shifting technique to investigate the thickness of $Ta_2O_5$ thin films deposited on BK7 substrates, using a modified Sagnac interferometer. Incident light is split by a polarizing beam splitter into two orthogonal linearly polarized beams traveling in opposite directions, and a quarter-wave plate is inserted into the common path to create an unbalanced phase condition. The linearly polarized light beams are transformed into two circularly polarized beams by transmission through a quarter-wave plate placed at the output of the interferometer. The proposed setup, therefore, yields rotating polarized light that can be used to extract a relative phase via the self-reference system. A thin-film sample inserted into the cyclic path modifies the output signal, in terms of the phase retardation. This technique utilizes three phase-shifted intensities to evaluate the phase retardation via simple signal processing, without manual adjustment of the output polarizer, which subsequently allows the thin film's thickness to be determined. Experimental results show that the thicknesses obtained from the proposed setup are in good agreement with those acquired by a field-emission scanning electron microscope and a spectroscopic ellipsometer. Thus, the proposed interferometric arrangement can be utilized reliably for non-contact thickness measurements of transparent thin films and characterization of optical devices.

Transition Metal Complexes Derived From 2-hydroxy-4-(p-tolyldiazenyl)benzylidene)-2-(p-tolylamino)acetohydrazide Synthesis, Structural Characterization, and Biological Activities

  • Alhakimi, Ahmed N.;Shakdofa, Mohamad M.E.;Saeed, S. El-Sayed;Shakdofa, Adel M.E.;Al-Fakeh, Maged S.;Abdu, Ashwaq M.;Alhagri, Ibrahim A.
    • Journal of the Korean Chemical Society
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    • v.65 no.2
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    • pp.93-105
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    • 2021
  • Mononuclear Cu(II), Ni(II), Co(II), Mn(II), Zn(II), Fe(III), Ru(III), and UO2(II) complexes of 2-hydroxy-4-(p-tolyldiazenyl)benzylidene)-2-(p-tolylamino)acetohydrazide (H2L) were prepared by direct method. The ligand and its complexes were isolated in solid state and characterized by analytical techniques such as elemental and thermal analyses, molar conductance, magnetic susceptibility measurements and spectroscopic techniques such as UV-Visible, IR, 1H-NMR and 13C-NMR. The spectral data indicated that the ligand acted as neutral/monobasic bidentate or monobasic/dibasic tridentate ligand bonded to the metal ions through the oxygen atom of ketonic or enolic carbonyl group, azomethine nitrogen atom and deprotonated/protonated phenolic oxygen atom forming either tetragonally distorted octahedral or octahedral. Antimicrobial activities of the ligand and its complexes were evaluated against Escherichia coli, Bacillus subtilis and Aspergillus niger by well diffusion method. The results of antifungal activity showed that the Fe(III) complex (10) exhibited higher antifungal against Aspergillus niger than the other complexes. However, the results of antibacterial activity revealed that Cu(II) complex (4) is the most active against Escherichia coli while the Cu(II) complex (5) and Fe(III) complex (10) exhibited higher antibacterial effect on Bacillus subtilis than the other complexes.