• Title/Summary/Keyword: Spectroscopic characterization

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Synthesis and Characterization of New Polyesters Having Unsaturated Groups from Bis [4-(alkyloxy)benzilidene]succinic Anhydride (Bis[4-(alkyloxy)benzilidene]succinic anhydride로부터 유도된 불포화기를 가지는 새로운 폴리에스터의 합성)

  • 김용석;진왕철;정진철
    • Polymer(Korea)
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    • v.26 no.4
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    • pp.439-444
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    • 2002
  • Several monomeric benzilidene anhydrides (2a~d) haying n-alkyloxy groups with various n-alkyl chain lengths were prepared by Stobbe condensation of diethyl succinate with 4-(n-alkyloxy)benzaldehyde (1a,b) followed by hydrolysis by the succinates and cyclodehydration of the benzilidenated succinic acids. Configurational isomerism of the monomer was investigated by spectroscopic means. It was found that monomers (2a~d) exist in (Z,Z)-isomeric structure. Polymerization was carried out in bulk at 150~$210^{\circ}C$ range in nitrogen flow. The chemical structure and thermal properties of the polymers were characterized by spectroscopic means, TGA and DSC. Their properties highly depended on their chemical structures in accordance with a side chain length.

Spectroscopic, Thermal and Biological Studies of Zn(II), Cd(II) and Hg(II) Complexes Derived from 3-Aminopyridine and Nitrite Ion

  • Dhaveethu, Karuthakannan;Ramachandramoorthy, Thiagarajan;Thirunavukkarasu, Kandasamy
    • Journal of the Korean Chemical Society
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    • v.57 no.6
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    • pp.712-720
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    • 2013
  • Microwave assisted syntheses of Zn(II), Cd(II) and Hg(II) complexes with 3-aminopyridine (3AP) and nitrite ($NO_2{^-}$) ions have been reported. The metal complexes were characterized by elemental analyses, molar conductance, IR, Far-IR, electronic, NMR ($^1H$, $^{13}C$), thermal and electron impact mass spectral studies. The spectroscopic studies reveal the composition, the nature of nitrite ligand in the complexes, electronic transitions, chemical environments of C and H atoms thermal degradation of the complexes. On the basis of characterization data, distorted tetrahedral geometry is suggested for Zn(II), Cd(II) and Hg(II) complexes. The organic ligand (3AP) and their metal complexes were screened against gram negative pathogenic bacteria and fungi in vitro. The results are compared with our previous report J. Korean Chem. Soc. 2013, 57, 341 on 4-aminopyridine and nitrite ion complexes of the same metal ions.

Synthesis, Spectroscopic Studies and Biological Applications of Organotin(IV) Derivatives of 3-[N-(4-Nitrophenyl)-amido]propenoic Acid and 3-[N-(4-Nitrophenyl)-amido]propanoic Acid

  • Shahid, Khadija;Shahzadi, Saira;Ali, Saqib;Mazhar, M.
    • Bulletin of the Korean Chemical Society
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    • v.27 no.1
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    • pp.44-52
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    • 2006
  • New organotin(IV) derivatives with general formulae R_2SnL_2 and R_3SnL, where R = methyl, n-butyl, n-octyl and phenyl and HL is either 3-[N-(4-nitrophenyl)amido]-propenoic acid or 3-[N-(4-nitrophenyl)amido] propanoic acid have been synthesized in 1 : 2 and 1 : 1 molar ratio by different methods. The FTIR spectra clearly demonstrated that the organotin(IV) moieties react with [O,O] atoms of the ligands. The bonding and coordination behavior in these complexes are discussed on the basis of multinuclear (^1H,\,^{13}C,\,^{119}Sn) NMR and mass spectrometric studies. Antibacterial, and antifungal screening tests were performed for these compounds and reported here. These values were compared to those of the precursors and it was found that diorganotin(IV) complexes exhibit less activity as compared to triorganotin(IV) complexes . LD_{50} data were obtained by Brine Shrimp assay method. Insecticidal activity was performed for selective compounds by contact toxicity method.

Antifungal Effects of Silver Phytonanoparticles from Yucca shilerifera Against Strawberry Soil-Borne Pathogens: Fusarium solani and Macrophomina phaseolina

  • Ruiz-Romero, Paola;Valdez-Salas, Benjamin;Gonzalez-Mendoza, Daniel;Mendez-Trujillo, Vianey
    • Mycobiology
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    • v.46 no.1
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    • pp.47-51
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    • 2018
  • In the present study, the characterization and properties of silver nanoparticles from Yucca shilerifera leaf extract (AgNPs) were investigated using UV-visible spectroscopic techniques, zeta potential, and dynamic light scattering. The UV-visible spectroscopic analysis showed the absorbance peaked at 460 nm, which indicated the synthesis of silver nanoparticles. The experimental results showed silver nanoparticles had Z-average diameter of 729 nm with lower stability (195.1 mV). Additionally, our dates revealed that AgNPs showed broad spectrum antagonism ($p{\leq}.05$) against Fusarium solani (83.05%) and Macrophomina phaseolina (67.05%) when compared to the control after nine days of incubation. Finally, AgNPs from leaf extracts of Y. shilerifera may be used as an agent of biocontrol of microorganism of importance. However, further studies will be needed to fully understand the agronanotechnological potentialities of AgNPs from Yucca schidigera.

Synthesis and Characterization of Thallium (Ⅲ) Complexes with Tetracyanoquinodimethane, TI$(TCNQ)_3$ and $TICI_2(TCNQ)_{2.5}$

  • 김미경;김영인;문성배;최성낙
    • Bulletin of the Korean Chemical Society
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    • v.17 no.5
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    • pp.424-428
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    • 1996
  • TlCl2(TCNQ)2.5 and Tl(TCNQ)3 were obtained from the reaction of LiTCNQ (TCNQ=tetracyanoquinodimethane) and TlX3 (X=Cl and NO3). These compounds were characterized by spectroscopic(IR, UV, EPR), electrochemical methods, and electrical conductivity measurements. Thermal analysis (TG, DSC) was also conducted. The room temperature electrical conductivities of these compounds are in the range of semiconductors. Spectroscopic studies indicate that Tl(TCNQ)3 has fully ionized TCNQ- ions in a form of simple salt, whereas TlCl2(TCNQ)2.5 is consisted of TCNQ- and TCNQ0 as a complex salt. EPR values of TCNQ- radical anion are 1.999 in both compounds and the signal attributable to metal ion is not observed, suggesting that any unpaired electrons are localized on TCNQ radicals, and metal atoms have diamagnetic state. Ligand decomposition and reduction process are simultaneously progressed in both compounds above at 200 ℃. The endothermic activation energy of TlCl2(TCNQ)2.5 is shown somewhat larger than that of Tl(TCNQ)3, it may be due to Tl-Cl bond strength. The mid-peak potentials of these compounds are very similar to those of TCNQ and the values of Epa and Epc are almost equal to 1. The wave of thallium ion is not detected in cyclic voltammogram, hence the redox processes of the complexes might be mainly localized to the TCNQ ligand rather than thallium ion.

Synthesis and Characterization of Tetrathiafulvalene Charge Transfer Compounds with Iron and Antimony Halides

  • Kim Young In;Choi Sung Nak;Jung Woo Sung
    • Bulletin of the Korean Chemical Society
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    • v.15 no.6
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    • pp.465-468
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    • 1994
  • The charge transfer compounds $(TTF)_4FeCl_3{\cdot}CH_3OH,\;(TTF)_4SbCl_4\;and\;(TTF)_5(SbBr_4)_2{\cdot}CH_3COCH_3$ were prepared from reactions of the TTF (tetrathiafulvalene) and metal halides. The compounds were characterized by spectroscopic (UV,IR, EPR and XPS) methods, magnetic susceptibility and electrical conductivity measurements. The d.c electrical conductivities of the pressed pellets are in the order of $10^{-1}-10^{-3} Scm^{-1}$, which lies in the range of semiconductor region at room temperature. It means that the partially ionized TTF has stacked in low-dimensional chain in each compound. Spectroscopic properties also indicate that TTF molecules are partially ionized and charge transfer has occurred from (TTF)n to Fe(III) center in $(TTF)_4FeCl_3{\cdot}CH_3OH$ whereas to the $-SbX_4^-$ entity in $(TTF)_4SbCl_4\;and\;(TTF)_5(SbBr_4)_2{\cdot}CH_3COCH_3$. The EPR g values are consistent with TTF radical formation and EPR linewidths suggest the delocalization of unpaired electrons along TTF stacks. A signal arised from metal (Fe and Sb) ions were not detected in EPR spectra, indicating that metal ion is in the diamagnetic state in each compound. The diamagnetic state was also examined by the magnetic susceptibility measurement. The magnetic properties reveal the significant interaction between the $TTF^+$ radical cations in the stacks. The oxidation state of metal ions was also investigated by XPS spectra.

Spectroscopic Characterization of Humic Substances Present in Landfill Leachates with Respect to Landfilling Age (매립 연령에 따른 침출수중에 존재하는 휴믹물질의 분광학적 특성 분석)

  • Kang, Kihoon;Shin, Hyun-Sang;Park, Heekyung
    • Journal of Korean Society of Environmental Engineers
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    • v.22 no.6
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    • pp.1113-1126
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    • 2000
  • Humic substances present in landfill leachates were extracted and their characteristics were analyzed with respect to landfilling age as a basic study to evaluate the effect of humic substances on the transport and transformation of other pollutants in pollution plume contaminated by landfill leachate. Element analysis of the extracted humic substances were performed. The information on the functional groups of the humic substances molecules were obtained from the spectroscopic analysis using UV-visible, FT/IR, and fluorescence spectroscopy. The structural characteristics of the humic substances were also analyzed by $^1H$ and $^{13}C$ NMR spectroscopy. From the results of the analyses it was found that the structure of the humic substances present in landfill leachates was more aliphatic than aromatic relative to other common humic substances extracted from natural soils and water. The results indicate that the degree of humification of the humic substances were relatively low. The degree of humification, however, was increased as the landfilling age was increased.

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Electrical/Optical Characterization of PZT Thin Films Deposited through Sol-Gel Processing

  • Hwang, Hee-Soo;Kwon, Kyoeng-Woo;Choi, Jeong-Wan;Do, Woo-Ri;Hwang, Jin-Ha
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.08a
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    • pp.361-361
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    • 2012
  • PZT (Pb(Zr,Ti)O3) thin films have been used widely in the MEMS application, due to their inherent ferroelectric and piezoelectric properties. Such ferroelectricity induces much higher dielectric constants compared to those of the nonperovskite materials. In this work, the PZT thin films were deposited onto Indium-Tin-oxide (ITO) substrates through the spin-coating of PZT sols. The deposited PZT thin films were characterized in terms of the electrical and optical properties with special emphases on conductivity and optical constants. The detailed analysis techniques incorporate the dc-based current-voltage characteristics for the electrical properties, spectroscopic ellipsometry for optical characterization, atomic force microscopy for surface morphology, X-ray Photoelectron Spectroscopy for chemical bonding, Energy-dispersive X-ray Spectrometry for chemical analyses and X-ray diffraction for crystallinity. The ferroelectric phenomena were confirmed using capacitance-voltage measurements. The integrated physical/chemical features are attempted towards energy-oriented applications applicable to next-generation high-efficiency power generation systems.

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Symmetric Bis-Azospiropyrans: Synthesis, Characterization and Colorimetric Study

  • Nourmohammadian, Farahnaz;Abdi, Ali Ashtiani
    • Bulletin of the Korean Chemical Society
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    • v.34 no.6
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    • pp.1727-1734
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    • 2013
  • Synthesis and characterization of some novel symmetric bis-azospiropyrans are reported in this study. These bis-azospiropyrans are bifunctional chromophores with two spiropyrans linked by a bis-azo extended aromatic system that produce more color strength (large molar absorption coefficient in mero forms) due to appending two azospiropyran chromophores on one molecule. Comparing to the molar absorption coefficients of the conventional spiropyran chromophores (${\varepsilon}=0.31{\times}10^4\;M^{-1}{\cdot}cm^{-1}$) and mono-azospiropyran chromophores ($1.35{\times}10^4\;M^{-1}{\cdot}cm^{-1}$), the novel synthesized photochromes showed astonishingly increased molar absorption coefficients ($2.3-3.8{\times}10^4\;M^{-1}{\cdot}cm^{-1}$) at the same conditions. Such high molar absorption coefficients confers high sensitivity to light and more color intensity of mero form, that leads to improvement of their light sensitivity and better discrimination of spiro (OFF) form from mero (ON) ones in molecular switches. The structures were deduced from their MS, FT-IR, and $^1H$-NMR spectroscopic data and CHN analysis. All the synthesized photochemically bifunctional compounds revealed fluorescent emission in their colorless form which was faded out after exposing to UV light. Fluorescence quantum yield values of the mero forms were 0.25-0.81 and two high fluorescence quantum yield values (0.60 and 0.81) were found in these series.

Spectroscopic characterization of N,N'-bis(salicylidene)pentane-1,3-diamine nickel(II) complex

  • Kim, Gilhoon;Won, Hoshik
    • Journal of the Korean Magnetic Resonance Society
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    • v.18 no.2
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    • pp.74-81
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    • 2014
  • The $N_2O_2$ tetradentate Schiff base ligand, N,N'-bis(salicylidene)pentane-1,3-diamine (Salpn), coupled with 1:2 concentration ratio of 1,3-diaminopentane and salicylaldehyde was used to produce a series of macrocyclic Nikel(II) complexes. In the metal complexation, it was observed that Salpn macrocyclic ligand can adopt more than a metal ion giving an unique multinuclear metal complexes including Ni(II)Salpn and $Ni(II)_3(Salpn)_2$. Characteristic IR ${\upsilon}(M-O)$ peaks for Ni(II)Salpn and $Ni(II)_3(Salpn)_2$ were observed to be $1028cm^{-1}$ and $1024cm^{-1}$, respectively. Characteristic UV-Vis absorption ${\lambda}_{max}$ peaks for $Ni(II)_3(Salpn)_2$ were observed to be 241nm and 401 nm. Structural characterization of $Ni(II)_3(Salpn)_2$ by NMR exhibits that the salicylidene ring moiety has two different resonance signals originated from the magnetically asymmetric diligand and trinuclear bis complex. Complete NMR signal assignments and characterizations elucidating structural features of $Ni(II)_3(Salpn)_2$ were described in detail.