• Title/Summary/Keyword: IR spectra

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Fabrication and Photocatalytic Properties of SiO2-TiO2 Composite Nanofibers (SiO2-TiO2계 복합 나노섬유의 제조 및 광활성 연구)

  • Hyun, Dong Ho;Lim, Tae-Ho;Lee, Sung Wook
    • Applied Chemistry for Engineering
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    • v.19 no.5
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    • pp.554-558
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    • 2008
  • $(1-x)SiO_2-(x)TiO_2$ composite fibers with various compositions of $TiO_2$ were prepared by electrospinning their sol-gel precursors of titanium (IV) iso-propoxide (TiP), and tetraethyl orthosilicate (TEOS). The surface morphology and structure of sintered composite fibers were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), simultaneous thermogravimetric analysis-differential scanning calorimetry (TGA-DSC) and Fourier transform infrared spectroscopy (FT-IR). As the content of $TiO_2$ in $(1-x)SiO_2-(x)TiO_2$ system was increased the average diameter of composite fibers was proportionally increased. Also, the transformation of $TiO_2$ from anatase to rutile form was inhibited by the highly dispersed $TiO_2$ around $SiO_2$ particles up to $0.6SiO_2-0.4TiO_2$ composite fibers even after calcination at $1000^{\circ}C$. The photocatalytic activity of $SiO_2-TiO_2$ composite fibers was examined for the methylene blue (MB) decomposition which was confirmed using UV-vis/DRS spectra. The experiments demonstrated that the MB in aqueous solution was successfully photodegraded using $SiO_2-TiO_2$ composite nanofibers under UV-visible light irradiation.

The Synthesis and the Electrochemical Properties of Al Doped $V_2O_5$ (Al이 도핑된 오산화바나듐의 합성 및 전기화학적 특성)

  • Park, Heai-Ku;Joung, Ok-Young;Lee, Man-Ho
    • Applied Chemistry for Engineering
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    • v.16 no.4
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    • pp.491-495
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    • 2005
  • Vanadium pentoxide xerogels with a doping ratio of $Al/V_2O_5$ ranging from 0.01 to 0.05 were synthesized by doping Al into $V_2O_5$ xerogel via the sol-gel process. By using the synthesized $Al_xV_2O_5$, the $Li/Al_xV_2O_5$ cells were assembled to investigate the chemical and electrochemical properties. Surface morphology of the $Al_xV_2O_5$ xerogel showed an anisotropic corrugated sheet-like matrix, and the interlayer distance was about $11.5{\AA}$. The IR spectra of the $Al_xV_2O_5$ revealed that the doped Al was coordinated to the vanadyl group in $V_2O_5$. The $Al_xV_2O_5$ xerogels showed enhanced reversibility and energy density compared with the $V_2O_5$ xerogel. The specific capacity of the $Al_{0.05}V_2O_5$ xerogel was more than 200 mAh/g at 10 mA/g discharge rate, and cycle efficiency was about 90% after the 31st cycling test between 1.9 V and 3.9 V.

Effects of Reaction Temperature, Time and Particle Size on the Physicochemical Properties of Chitosans (키토산 제조시 반응 온도와 시간 및 입자크기가 키토산의 물리화학적 특성에 미치는 영향)

  • Lee, Woo-Jin;Han, Beom-Ku;Park, In-Ho;Park, Seung-Heyon;Oh, Hoon-Il;Jo, Do-Hyun
    • Korean Journal of Food Science and Technology
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    • v.27 no.6
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    • pp.997-1002
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    • 1995
  • In order to study the effects of reaction temperature, time and particle size on the physicochemical properties of chitosan, commercially available chitin was treated with 50%(w/w) NaOH. To obtain 78% of deacetylation, a treatment of 6 hours at $100^{\circ}C$(Ch-100), 20 minutes at $120^{\circ}C$(Ch-120) or 10 minutes at $140^{\circ}C$(Ch-140) was necessary. The resulting chitosans showed a different viscosity; 180cps for Ch-100, 130cps for Ch-120, 30cps for Ch-140. The residence time at $80^{\circ}C$ also decreased the viscosity of the chitosan but the reduction in the particle size of chitin largely favored deacetylation and resulted in a higher viscosity of the chitosan. Compared with chitin, the capacity of water and oil absorption of chitosan was not significantly improved. However, the capacity of dye absorption was increased by 4 times by the deacetylation. In addition the IR spectra of chitosans showed less sharp absorption bands than that of chitin.

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Stability and Sensory Evaluation of Naphthoquinone Pigments from the Roots of Lithospermum erythrorhizon (자근(紫根)으로부터 분리한 Naphthoquinone류 색소의 pH 안정성 및 관능검사)

  • Chung, Mi-Sook;Lee, Mie-Soon
    • Korean Journal of Food Science and Technology
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    • v.26 no.2
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    • pp.152-156
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    • 1994
  • The purplish red pigment from the roots of Lithospermum erythrorhizon, a Korean edible wild plant, has been investigated concerning it's value as a natural colorant for Korean traditional foods. An attempt was made to isolate pigments and define their characteristics. Two compounds of isobutylshikonin and acetylshikonin were identified by melting point determination and spectra of UV, IR, and $^{1}H-NMR$. To examine the utility of these naphthoquinone pigments for foods, the effect of various pH values on stability were determined over a period of storage. Buffered solutions of acetylshikonin and isobutylshikonin at pH 3 and 5 showed stable purplish red. The absorption maxima if acetylshikonin and isobutylshikonin over the range of pH 3 to 7 were 518 nm and 520 nm, respectively. A bathochromic shift to 588 nm at pH 10 was observed on these two naphthoquinone pigments. Sensory evaluation was performed with acetylshikonin and isobutylshikonin of identical absorbance. These two pigments revealed purplish red color in Munsell system.

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Electrochemical Properties of Oxygen Adducts Tetradentate Schiff Base Cobalt (II) Complexes in Pyridine (Ⅲ) (Pyridine 용액에서 네자리 Schiff Base Cobalt (II) 착물들의 산소첨가 생성물에 대한 전기화학적 성질 (제 3 보))

  • Ky Hyung Cho;Seong Seob Seo;Dong Chul Chon
    • Journal of the Korean Chemical Society
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    • v.33 no.3
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    • pp.295-303
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    • 1989
  • Tetradentate Schiff base cobalt(II) complex; Co(SND) and Co(SOPD) were synthesized, and these complexes were allowed to react with dry oxygen to form oxygen adducts cobalt(III) complexes such as $[Co(SND)(Py)]_2O_2$ and $[Co(SOPD)(Py)]_2O_2$ in pyridine. These complexes have been identified by IR specta, T.G.A., magnetic susceptibilities measurements and elemental analysis. It has been found that the oxygen adducts coblat(III) complexes have hexacoordinated octahedral configuration with tetradentate Schiff base cobalt(II), pyridine and oxygen, and the mole ratio of oxygen to cobalt(II) complexes are 1;2. The redox reaction processes of $Co(SND)(Py)_2$ and $Co(SOPD)(Py)_2$ complexes were investigated by cyclic voltammetry with glassy carbon electrode in 0.1M TEAP pyridine. The result of redox reaction processes of Co(III)/Co(II) and Co(II)/Co(I) for $Co(SND)(Py)_2$ and $Co(SOPD)(Py)_2$ complexes are reversible or quasi reversible process but oxygen adducts complexes are irreversible processes. Redox process for oxygen of oxygen adducts complexes was quasi reversible and redox range of potential was $E_{pc}\;=\;-0.96{\sim}-1.03V$ and $E_{pa}\;=\;-0.78{\sim}-0.80V.$

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Synthetic Studies on the Nucleophilic Addition of 1-Methyl-5-mercapto-1,2,3,4-tetrazole to Vinylsulfilimines (Vinylsulfilimine유도체에 대한 1-methyl-5-mercapto-1,2,3,4-tetrazole의 친핵성 첨가물에 관한 연구)

  • Tae-Rin Kim;So-Young Lee;Sang-Yong Pyun
    • Journal of the Korean Chemical Society
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    • v.36 no.2
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    • pp.318-323
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    • 1992
  • Following seven new nucleophilic adducts of sulfilimine compounds were prepared by the addition of 1-methyl-5-mercapto-1,2,3,4-tetrazole to vinylsulfilimine derivatives; S-Phenyl-S-2-(1-methyl-1,2,3,4-tetrazole-5-thio)-ethyl-N-p-tosylsulfilimine, S-p-tolyl-S-2-(1-methyl-1,2,3,4-tetrazole-5-thio)-ethyl-N-p-tosylsulfilimine, S-m-tolyl-S-2-(1-methyl-1,2,3,4-tetrazole-5-thio)-ethyl-N-p-tosylsulfilimine, S-p-chlorophenyl-S-2-(1-methyl-1,2,3,4-tetrazole-5-thio)-ethyl-N-p-tosylsulfilimine, S-p-bromophenyl-S-2-(1-methyl-1,2,3,4-tetrazole-5-thio)-ethyl-N-p-tosylsulfilimine, S-p-methoxyphenyl-S-2-(1-methyl-1,2,3,4-tetrazole-5-thio)-ethyl-N-p-tosylsulfilimine and S-p-nitrophenyl-S-2-(1-methyl-1,2,3,4-tetrazole-5-thio)-ethyl-N-p-tosylsulfilimine. The structures of these adducts were confirmed by elemental analyses, MP, UV, IR-and NMR-Spectra.

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Photodecomposition of Concentrated Ammonia over Nanometer-sized TiO2, V-TiO2, and Pt/V-TiO2 Photocatalysts

  • Choi, Hyung-Joo;Kim, Jun-Sik;Kang, Mi-Sook
    • Bulletin of the Korean Chemical Society
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    • v.28 no.4
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    • pp.581-588
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    • 2007
  • To enhance the photodecomposition of concentrated ammonia into N2, Pt/V-TiO2 photocatalysts were prepared using solvothermal and impregnation methods. Nanometer-sized particles of 0.1, 0.5 and 1.0 mol% V-TiO2 were prepared solvothermally, and then impregnated with 1.0 wt% Pt. The X-ray diffraction (XRD) peaks assigned to V2O5 at 30.20 (010) and Pt metal at 39.80 (111) and 46.20 (200) were seen in the 1.0 wt% Pt/ 10.0 mol% V-TiO2. The particle size increased in the order: pure TiO2, V-TiO2 and Pt/V-TiO2 after thermal treatment at 500 °C, while their surface areas were in the reverse order. On X-ray photoelectron spectroscopy (XPS), the bands assigned to the Ti2p3/2 and Ti2p1/2 of Ti4+-O were seen in all the photocatalysts, and the binding energies increased in the order: TiO2 < Pt/V-TiO2 < V-TiO2. The XPS bands assigned to the V2p3/2 (517.85, 519.35, and 520.55 eV) and V2p1/2 (524.90 eV) in the V3+, V4+ and V5+ oxides appeared over V-TiO2, respectively, while the band shifted to a lower binding energy with Pt impregnation. The Pt components of Pt/ V-TiO2 were identified at 71.60, 73.80, 75.00 and 76.90 eV, which were assigned to metallic Pt 4f7/2, PtO 4f7/2, PtO2 4f7/2, and PtO 4f5/2, respectively. The UV-visible absorption band shifted closer towards the visible region of the spectrum in V-TiO2 than in pure TiO2 and; surprisingly, the Pt/V-TiO2 absorbed at all wavelengths from 200 to 800 nm. The addition of vanadium generated a new acid site in the framework of TiO2, and the medium acidic site increased with Pt impregnation. The NH3 decomposition increased with the amount of vanadium compared to pure TiO2, and was enhanced with Pt impregnation. NH3 decomposition of 100% was attained over 1.0 wt% Pt/1.0 mol% V-TiO2 after 80 min under illumination with 365 nm light, although about 10% of the ammonia was converted into undesirable NO2 and NO. Various intermediates, such as NO2, -NH2, -NH and NO, were also identified in the Fourier transform infrared (FT-IR) spectra. From the gas chromatography (GC), FT-IR and GC/mass spectroscopy (GC/MS) analyses, partially oxidized NO and NO2 were found to predominate over V-TiO2 and pure TiO2, respectively, while both molecules were reduced over Pt/V-TiO2.

Synthesis and Charaterization of Polymerizable Acryl's Emulsifier to prepare Green Glue (친환경 접착제 제조용 아크릴계 반응성 유화제의 합성)

  • Jeong, Noh-Hee;Park, Jong-Kwon;Kang, Yun-Seok
    • Journal of the Korean Applied Science and Technology
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    • v.33 no.1
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    • pp.51-57
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    • 2016
  • In this study, we synthesized reactive surfactant which have functional radical group for effective chemical reaction. Reactive surfactant have been synthesized using synthesis of polyoxyethylene lauryl ether(POE 23) which is nonionic surfactant and methacrylic acid, acrylic acid. benzene was used as the solvent, p-TsOH was used as the catalyst. synthesized surfactant was confirmed by FT-IR, $^1H$-NMR spectra, and elemental analysis. Evaluation of physical properties was measured HLB, cloud point, surface tension, the critical micelle concentration, emulsifying power. HLB number was evaluated 11.62 to 12.09 range. The Critical Micelle Concentration(cmc) values evaluated was $1{\times}10^{-4}{\sim}5{\times}10^{-4}mol/L$ by surface tension method. The cloud point was $35^{\circ}C$, $39^{\circ}C$ each. The emulsifymvcqa ing properties of the synthesized surfactants was lower than polyoxyethylene lauryl ether. In addition, soybean oil was better than benzene. The experimental results confirmed the ester bond, the yield of 93.27%, 94.49% was found.

Removal of Pb2+ Ions from Water by Surfactant-templated Mesoporous Silicates (계면활성제가 담지된 메조포러스 실리케이트에 의한 수중 납이온 제거)

  • Choi, Hyun Suk;Lee, Dong Gue;Cho, Guk Jin;Lee, Chae Young;Chung, Jin Suk;Yoo, Ik-keun;Shin, Eun Woo
    • Korean Chemical Engineering Research
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    • v.44 no.2
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    • pp.172-178
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    • 2006
  • Mesoporous silicate materials have been used as adsorbents for the removal of heavy metals from water by introducing functional groups such as thiol and amine. In this research, it was investigated whether surfactants used as templating agents in synthetic processes can act as adsorption sites for heavy metals. Three mesoporous silicates-SBA-15, MCM-41, and HMS were synthesized using, respectively, block copolymer, hexadecyltrimethylammoniumbromide (HDTMA), and dodecyamine as surfactants. X-ray diffraction and $N_2$ gas adsorption analysis confirmed that the mesoporous silicates were well prepared and FT-IR spectra resulted in the existence of the surfactants in as-synthesized mesoporous silicates and the removal of surfactants after calcination. The interactions between $Pb^{2+}$ ions and the mesoporous silicate materials with/without surfactants were observed. In adsorption kinetic experiments, it revealed that the calcined mesoporous silicates and the surfactant-loaded SBA-15 almost had no adsorption capacity for $Pb^{2+}$ ions. In contrast, the surfactant-loaded MCM-41 and HMS showed, respectively, the adsorption capacities of 26.60 and 115.16 mg/g which were acquired through the fits of adsorption kinetic data to the pseudo second order kinetic model. The adsorption capacities were comparable to those of other mesoporous adsorbents for heavy metals.

Synthesis and Spectroscopic Characterization of Manganese(II), Iron(III) and Cobalt(III) Complexes of Macrocyclic Ligand. Potential of Cobalt(III) Complex in Biological Activity

  • El-Tabl, Abdou S.;Shakdofa, Mohamad M.E.;El-Seidy, Ahmed M.A.
    • Journal of the Korean Chemical Society
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    • v.55 no.6
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    • pp.919-925
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    • 2011
  • A new series of manganese(II), iron(III) and cobalt(III) complexes of 14-membered macrocyclic ligand, (3,6,10,13,16,19-hexaazabicyclo[6.6.6]icosane-1,8-diamine) have been prepared and characterized by elemental analyses, IR, UV-VIS, $^1H$- and $^{13}C$- NMR spectra, magnetic susceptibilities, conductivities, and ESR measurements. Molar conductance measurements in DMF solution indicate that the complexes are electrolytes. The ESR spectrum for cobalt(III) complex in $CD_3OD+10%D_2O$ after exposure to $^{60}Co-{\gamma}$-rays at 77 K using a 0.2217 M rad $h^{-1}$ vicrad source showed $g_{\perp}$ > $g_{\parallel}$ > $g_e$, indicating that, the unpaired electron site is mainly present in the $d_z2$ orbital with covalent bond character. In this case, the ligand hyperfine tensors are nearly collinear with ${\gamma}$-tensors, so there is no major tendency to bend. Therefore, little extra delocalization via the ring lobe of the $dz^2$ orbital occurs. However, the ESR spectrum in solid state after exposure to $^{60}Co-{\gamma}$-rays at 77 K showed $g_{\parallel}$ > $g_{\perp}$ > $g_e$, indicating that, the unpaired electron site is mainly present in the $d_x2_{-y}2$ ground state as the resulting spectrum contains a large number of randomly oriented molecules provided that, the principle directions of g and A tensors. Manganese (II) complex 2, $[H_{12}LMn]Cl_4.2H_2O$, showed six isotropic lines characteristic to an unpaired electron interacting with a nucleus of spin 5/2, however, iron(III) complex 3, $[H_{12}LFe]Cl_5.H_2O$, showed spectrum of a high spin $^{57}Fe$ (I=1/2), $d^5$ configuration. The geometry of these complexes was supported by elemental analyses, IR, electronic and ESR spectral studies. Complex 1 showed exploitation in reducing the amount of electron adducts formed in DNA during irradiation with low radiation products.