• Title/Summary/Keyword: spectroscopic studies

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In-situ Raman Spectroscopic Study of Nickel-base Alloys in Nuclear Power Plants and Its Implications to SCC

  • Kim, Ji Hyun;Bahn, Chi Bum;Hwang, Il Soon
    • Corrosion Science and Technology
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    • v.3 no.5
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    • pp.198-208
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    • 2004
  • Although there has been no general agreement on the mechanism of primary water stress corrosion cracking (PWSCC) as one of major degradation modes of Ni-base alloys in pressurized water reactors (PWR's), common postulation derived from previous studies is that the damage to the alloy substrate can be related to mass transport characteristics and/or repair properties of overlaid oxide film. Recently, it was shown that the oxide film structure and PWSCC initiation time as well as crack growth rate were systematically varied as a function of dissolved hydrogen concentration in high temperature water, supporting the postulation. In order to understand how the oxide film composition can vary with water chemistry, this study was conducted to characterize oxide films on Alloy 600 by an in-situ Raman spectroscopy. Based on both experimental and thermodynamic prediction results, Ni/NiO thermodynamic equilibrium condition was defined as a function of electrochemical potential and temperature. The results agree well with Attanasio et al.'s data by contact electrical resistance measurements. The anomalously high PWSCC growth rate consistently observed in the vicinity of Ni/NiO equilibrium is then attributed to weak thermodynamic stability of NiO. Redox-induced phase transition between Ni metal and NiO may undermine the integrity of NiO and enhance presumably the percolation of oxidizing environment through the oxide film, especially along grain boundaries. The redox-induced grain boundary oxide degradation mechanism has been postulated and will be tested by using the in-situ Raman facility.

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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Six new dammarane-type triterpene saponins from Panax ginseng flower buds and their cytotoxicity

  • Li, Ke-Ke;Li, Sha-Sha;Xu, Fei;Gong, Xiao-Jie
    • Journal of Ginseng Research
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    • v.44 no.2
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    • pp.215-221
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    • 2020
  • Background: Panax ginseng has been used for a variety of medical purposes in eastern countries for more than two thousand years. From the extensive experiences accumulated in its long medication use history and the substantial strong evidence in modern research studies, we know that ginseng has various pharmacological activities, such as antitumor, antidiabetic, antioxidant, and cardiovascular system-protective effects. The active chemical constituents of ginseng, ginsenosides, are rich in structural diversity and exhibit a wide range of biological activities. Methods: Ginsenoside constituents from P. ginseng flower buds were isolated and purified by various chromatographic methods, and their structures were identified by spectroscopic analysis and comparison with the reported data. The 3-(4,5-dimethyl-2-thiazolyl)-2,5-diphenyl-2H- tetrazolium bromide method was used to test their cytotoxic effects on three human cancer cell lines. Results: Six ginsenosides, namely 6'-malonyl formyl ginsenoside F1 (1), 3β-acetoxyl ginsenoside F1 (2), ginsenoside Rh24 (6), ginsenoside Rh25 (7), 7β-hydroxyl ginsenoside Rd (8) and ginsenoside Rh26 (10) were isolated and elucidated as new compounds, together with four known compounds (3-5 and 9). In addition, the cytotoxicity of these isolated compounds was shown as half inhibitory concentration values, a tentative structure-activity relationship was also discussed based on the results of our bioassay. Conclusion: The study of chemical constituents was useful for the quality control of P. ginseng flower buds. The study on antitumor activities showed that new Compound 1 exhibited moderate cytotoxic activities against HL-60, MGC80-3 and Hep-G2 with half inhibitory concentration values of 16.74, 29.51 and 20.48 μM, respectively.

Identification of a novel triterpene saponin from Panax ginseng seeds, pseudoginsenoside RT8, and its antiinflammatory activity

  • Rho, Taewoong;Jeong, Hyun Woo;Hong, Yong Deog;Yoon, Keejung;Cho, Jae Youl;Yoon, Kee Dong
    • Journal of Ginseng Research
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    • v.44 no.1
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    • pp.145-153
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    • 2020
  • Background: Panax ginseng Meyer (Araliaceae) is a highly valued medicinal plant in Asian regions, especially in Korea, China, and Japan. Chemical and biological studies on P. ginseng have focused primarily on its roots, whereas the seeds remain poorly understood. This study explores the phytochemical and biological properties of compounds from P. ginseng seeds. Methods: P. ginseng seeds were extracted with methanol, and 16 compounds were isolated using various chromatographic methods. The chemical structures of the isolates were determined by spectroscopic data. Antiinflammatory activities were evaluated for triterpene and steroidal saponins using lipopolysaccharide-stimulated RAW264.7 macrophages and THP-1 monocyte leukemia cells. Results: Phytochemical investigation of P. ginseng seeds led to the isolation of a novel triterpene saponin, pseudoginsenoside RT8, along with 15 known compounds. Pseudoginsenoside RT8 exhibited more potent antiinflammatory activity than the other saponins, attenuating lipopolysaccharide-mediated induction of proinflammatory genes such as interleukin-1β, interleukin-6, inducible nitric oxide synthase, cyclooxygenase-2, and matrix metalloproteinase-9, and suppressed reactive oxygen species and nitric oxide generation in a dose-dependent manner. Conclusion: These findings indicate that pseudoginsenoside RT8 has a pharmaceutical potential as an antiinflammatory agent and that P. ginseng seeds are a good natural source for discovering novel bioactive molecules.

Inhibitory actions of the antidepressant/antipanic drug phenelzine on brain GABA transaminase

  • Yoo, Byung-Kwon;Hong, Joung-Woo;Suk, Jae-Wook;Ahn, Jee-Yin;Yoo, Jeong-Suk;Lee, Kil-Soo;Cho, Sung-Woo;Choi, Soo-Young
    • Archives of Pharmacal Research
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    • v.19 no.6
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    • pp.480-485
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    • 1996
  • Brain GABA transaminase is inactivated by preincubation with antidepressant/antipanic drug pheneizine (${\beta}$ethylphenylhydrazine) (mixing molar ratio 10:1) at pH 7.4. The reaction of enzyme with phenelzine was monitored by absorption and fluorescence spectroscopic methods. The inactive enzyme was fully reconstituted by addition of cofactor pyridoxal-5-phosphate. This result implies that the blocking of 1 mol of pyridoxal-5-phosphate per enzyme dimer is needed for inactivation of the enzyme. The time course of the reaction is significantly affected by the substrate .alpha.-ketoglutarate, which afforded complete protection against the loss of catalytic activity. The kinetic studies shows that phenelzine reacts with the cofactor of enzyme with a second-order rate constant of $2.1{\times}10^3M^{-1}s^{-1}$. It is postulated that the antidepressant/antipanic drug phenelzine is able to elevate the neurotransmitter GABA levels in central nervous system by inhibitory action on GABA degradative enzyme GABA transaminase.

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Spectroscopic and Microstructural Analysis of Phase Transformation of Mg-PSZ/$Al_2O_3$ Fibers Prepared by Sol-Gel Method

  • Eun, Hee-Tai;Whang, Chin-Myung
    • The Korean Journal of Ceramics
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    • v.2 no.2
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    • pp.102-110
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    • 1996
  • The Mg-PSZ/$Al_2O_3$ fibers were fabricated by the sol-gel method. The added $Al_2O_3$ amounts were varied from 5 to 20 mol%. The phase transformation studies of a drawn Mg-PSZ/$Al_2O_3$ fibers were investigated by use of X-ray diffraction, IR and Raman spectroscopy. Microstructure and tensile strength of fibers were subjected to scanning electron microscopy and tensile strength tester. When $Al_2O_3$ was added to the Mg-PSZ fibers, it was found out from the analysis of XRD patterns and Raman spectra that a small amount of crystalline spinel($MgAl_2O_4$) started to form due to the reaction between $Al_2O_3$ and MgO, at $1000^{\circ}C$, and the phase transformation temperature of $ZrO_2$ crystal phase at different sintering temperatures increased. Also, the rapid grain growth with average size of 2.0 ${\mu}m$ shown in Mg-PSZ fiber at $1500^{\circ}C$ was considerably suppressed to 0.39 ${\mu}m$ by adding $Al_2O_3$ at the same temperature. When the Mg-PSZ/$Al_2O_3$ fibers containing 5 mol% $Al_2O_3$ were sintered $800^{\circ}C$ for 1 hr, average tensile strength of fibers was 0.9 GPs at diameters of 20 to 30 ${\mu}m$, but as the sintering temperatures was increased to $1000^{\circ}C$ for 1 hr, average tensile strength of fibers increased to 1.2 GPa in the same diameter range.

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Structural and Physicochemical Studies on DA-5018, a New Capsaicin Derivative (새로운 Capsaicin 유도체 DA-5018의 구조 및 물리화학적 성질 연구)

  • Kim, Heung-Jae;Lee, Jong-Jin;Lee, Eung-Doo;Shim, Hyun-Joo;Lee, Sang-Deuk;Ok, Kwang-Dae;Kim, Won-Bae;Park, No-Sang
    • Journal of Pharmaceutical Investigation
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    • v.27 no.2
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    • pp.119-123
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    • 1997
  • The physicochemical and structural properties of new capsaicin derivative, DA-5018, were examined. The reference standard of this compound was obtained by the recrystallization. A method for the determination of the dissociation constant of the compound is described. pH-solubility and distribution coefficient were determined by chromatographic method. Fundamental properties on thermal behaviors were investigated by TG, DTA and DSC. Structural analysis based on spectroscopic method coincided with the chemical structure of DA-5018. Approximate dissociation constant of the compound determined by UV spectral method was 9.35. Solubilities and partition coefficients in various pH buffer solution appeared pH-dependency. No crystal transition or further transition was found in the thermal analysis. This compound showed good stability, but pH 13 buffer and acetone made some degradative products.

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Studies on the Patterning of Polyimide LB Film and Its Application for Bioelectronic Device (폴리이미드 LB 필름을 이용한 패터닝 및 생물전자 소자로의 응용에 관한 연구)

  • 오세용;박준규;정찬문;최정우
    • Polymer(Korea)
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    • v.26 no.5
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    • pp.634-643
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    • 2002
  • Ultrathin film of polyamic acid having benzene and sulfonyloxyimide moieties was prepared using the Langmuir-Blodgett (LB) technique, and then photosensitive polyimide LB film was obtained by the thermal treatment of precursor polyamic acid multilayers at 200$\^{C}$ for 1 hr. The polyamic acid was synthesized by condensation polymerization under THF and pyridine cosolvent. All monomers and polymers were identified through elemental analysis, FT-IR and $^1$H-NMR spectroscopic measurements. The microarray patterning of photosensitive polyimide LB film on a gold substrate was generated with a deep UV lithography technique. The well-characterized monolayer of cytochrome c was immobilized on the microarray patterns using two different self-assembly processes. Physical and electrochemical properties of the self-assembled cytochrome c monolayer were investigated based on cyclic voltammetry and atomic force microscopy (AFM). Also, its application in bioelectronic device was examined.