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Synthesis and Characterization of C-meso and C-racemic Isomers of a Reinforced Tetraaza Macrocycle and Their Copper(II) Complexes

  • Jeong, Gyeong Rok;Kim, Juyoung;Kang, Shin-Geol;Jeong, Jong Hwa
    • Bulletin of the Korean Chemical Society
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    • v.35 no.7
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    • pp.2043-2048
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    • 2014
  • Two isomers of a new tetraaza macrotricycle 2,2,4,9,9,11-hexaazamethyl-1,5,8,12-tetraazatricyclo[$10.2.2^{5.8}$]-octadecane ($L^2$) containing additional N-$CH_2CH_2$-N linkages, C-meso-$L^2$ and C-racemic-$L^2$, have been prepared by the reaction of 1-bromo-2-chloroethane with C-meso-$L^1$ or C-racemic-$L^1$ ($L^1$ = 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane). Both C-meso-$L^2$ and C-racemic-$L^2$ react with copper(II) ion to form $[Cu(C-meso-L^2)]^{2+}$ or $[Cu(C-racemic-L^2)]^{2+}$ in dehydrated ethanol, but do not with nickel(II) ion under similar conditions. Crystal structure of [Cu(C-racemic-$L^2$)($H_2O$)]$(ClO_4)_2$ shows that the complex has distorted square-pyramidal coordination geometry with an apically coordinated water molecule. Unexpectedly, the Cu-N distances [2.016(3)-2.030(3) ${\AA}$] of [Cu(C-racemic-$L^2$)($H_2O$)]$(ClO_4)_2$ are longer than those [1.992(3)-2.000(3) ${\AA}$] of [Cu(C-racemic-$L^1$)($H_2O$)]$(ClO_4)_2$. As a result, $[Cu(C-racemic-L^2)(H_2O)]^{2+}$ exhibits weaker ligand field strength than $[Cu(C-racemic-L^1)(H_2O)]^{2+}$. The copper(II) complexes readily react with CN- ion to yield the cyano-bridged dinuclear complex $[Cu_2(C-meso-L^2)_2CN]^{3+}$ or $[Cu_2(C-racemic-L^2)_2CN]^{3+}$. Spectra and chemical properties of $[Cu(C-meso-L^2)]^{2+}$ and $[Cu_2(C-meso-L^2)_2CN]^{3+}$ are not quite different from those of $[Cu(C-racemic-L^2)]^{2+}$ and $[Cu_2(C-racemic-L^2)_2CN]^{3+}$, respectively.

Preparation of Zinc Oxide by Hydrothermal Precipitation and Degradation of Tartrazine (수열 합성법에 의한 Zinc Oxide의 제조 및 Tartrazine 분해 특성)

  • Na, Seok-Eun;Jeong, Sang-Gu;Jeong, Ga-Seop;Kim, Si-Young;Ju, Chang-Sik
    • Korean Chemical Engineering Research
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    • v.49 no.6
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    • pp.752-757
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    • 2011
  • The effects of reaction temperature, reactant concentration, pH of solution and mixing order of reactants on the particle shape and size distribution of zinc oxide were investigated in the preparation of zinc oxide from ammonium hydroxide and zinc acetate by the method of aqueous hydrothermal precipitation method, and the photocatalytic ability of zinc oxide synthesized was measured from the degradation of tartrazine under UV irradiation. The average particle size was increased with pH of solution but decreased with zinc acetate concentration and reaction temperature. The optimum condition for the synthesis of minimum sized zinc oxide was pH 11.2, concentration of zinc acetate 0.6 M and reaction temperature $90^{\circ}C$, and its average particle size was 3.133 ${\mu}$m. 97% of tartrazine was degraded by zinc oxide in sixty minutes.

A study on the Ni formation by reduction of NiO nano crystals (NiO 나노 결정의 환원 반응에 의한 Ni 형성 거동에 관한 연구)

  • Kim, Chang-Sam;Kang, Seung-Min
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.19 no.5
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    • pp.246-250
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    • 2009
  • The Ni formation behavior from the reduction of NiO nano crystals in the $H_2/N_2$ gas mixtures. The NiO nano crystals were synthesized by heat-treating nickel nitrate$(Ni(NO_3)_2\cdot6H_O)$ in the air at $500^{\circ}C$, and had an octahedral shape and the particle size of 200~500 nm. The NiO nano-crystals had well-developed (111) planes which is hardly formed in normal synthetic conditions. The reduction process was carried out at 300 and $600^{\circ}C$ for 15 and 60 minutes, respectively. When the NiO nano-crystals were reduced at $300^{\circ}C$, the Ni particles sustained the same octahedral shape as NiO, while Ni particles were to agglomerate at $600^{\circ}C$.

Effects of Combined Treatment of Clove Bud Essential Oil and Mild Heat on Inactivation of Escherichia coli O157:H7 Inoculated onto Red Oak Leaves (Clove Bud Essential Oil과 Mild Heat 병합처리에 의한 Red Oak Leaf에 접종된 Escherichia coli O157:H7 제어 효과)

  • Park, Su-Jong;Park, Jun-Beom;Kang, Ji-Hoon;Song, Kyung Bin
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.46 no.10
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    • pp.1265-1269
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    • 2017
  • This study was performed to evaluate the effects of combined treatment of clove bud essential oil (CBEO) and mild heat (MH) on inactivation of Escherichia coli O157:H7 inoculated onto red oak leaves. Combined treatment of 0.2% CBEO with MH at $50^{\circ}C$ exhibited the highest inhibitory effect against E. coli O157:H7 among treatments, resulting in 1.45 log reduction compared with water washing treatment. In addition, inhibitory effect of the combined treatment was maintained during storage of red oak leaves at $4^{\circ}C$ for 9 days, showing 1.67~2.25 log reductions compared with non-treated samples. Thus, these results indicate that combined treatment with CBEO/MH can be used to ensure the microbiological safety of fresh leaf vegetables such as red oak leaves during storage.

Epidemiological analysis of Escherichia coli O157 : H7 by pulsed-field gel electrophoresis and multiplex polymerase chain reaction

  • Jung, Byeong-yeal;Jung, Suk-chan;Cho, Dong-hee;Kim, Jong-yeom;Kim, Bong-hwan
    • Korean Journal of Veterinary Research
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    • v.39 no.2
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    • pp.338-342
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    • 1999
  • Twenty three strains of Escherichia (E) coli O157 : H7 isolated from Korea, Japan, USA were analyzed by pulsed-field gel electrophoresis (PFGE) of XbaI-digested chromosomal DNA and multiplex polymerase chain reaction. Various PFGE patterns of E. coli O157 : H7 were found on the same farm. Most of the E, coli O157 : H7 strains had shiga-like toxin (slt) II gene only (43.5%) or both slt I and slt II genes(30.4%). eaeA gene was highly conserved in the E. coli O157 : H7. There was no correlation between PFGE and slt gene patterns. The results indicate that various genotypes of E. coli O157 : H7 have spread throughout the country and genomic DNA patterns generated by PFGE are highly specific for different strains and have significant value in epidemiologic investigations of infectious disease outbreaks.

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Catalytic Conversion of Cellulose to Cellulose Acetate Propionate (CAP) Over SO42-/ZrO2 Solid Acid Catalyst

  • Leng, Yixin;Zhang, Yun;Huang, Chunxiang;Liu, Xiaocheng;Wu, Yuzhen
    • Bulletin of the Korean Chemical Society
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    • v.34 no.4
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    • pp.1160-1164
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    • 2013
  • The solid super acid catalyst $SO{_4}^{2-}$/$ZrO_2$ was prepared by impregnation method using $ZrO_2$ as the catalyst support. Catalyst forming was taken into consideration in order to separate catalyst from the mixture of cellulose acetate propionate (CAP). $Al_2O_3$ and sesbania gum powder were selected as binding agent and auxiliary agent respectively. The catalytic properties were evaluated through esterification of cellulose with acetic anhydride, propionic anhydride and characterized by XRD, FTIR and $NH_3$-TPD. In this paper, the effects of concentration of $H_2SO_4$ impregnated, calcination temperature, esterification temperature and esterification time on the yield, acyl content and viscosity of CAP were investigated. The results showed that $SO{_4}^{2-}/ZrO_2$ successfully catalyzed CAP synthesis over catalysts impregnated in 0.75 mol/L $H_2SO_4$ and calcined at $500^{\circ}C$. The yield, acetyl content and propionyl content of CAP reached the maximum value of 105.3%, 29.9% and 25.8% reacted at $50^{\circ}C$ for 8 h.

Hydrogen Permeation of SiC-CeO2 Composite Membrane by Dip-coating Process

  • Park, Jihye;Jung, Miewon
    • Journal of the Korean Ceramic Society
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    • v.50 no.6
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    • pp.485-488
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    • 2013
  • A SiC-$CeO_2$ composite membrane was successfully fabricated using an ally-hydridopolycarbosilane (AHPCS) binder and treated by dip-coating at 60 times with a $CeO_2$ sol solution. The dip-coated SiC membrane was calcined at 773 K and then sintered at 1173 K under an air atmosphere. The coated membrane was characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and a BET surface analysis. The difference in permeation performance between $H_2$ and CO gases was measured by varying the temperature. The permeation flux of $H_2$ on the SiC membrane with layered $CeO_2$ was obtained as $8.45{\times}10^{-6}\;mol/m^2sPa$ at room temperature. The CO permeation flux was $2.64{\times}10^{-6}\;mol/m^2sPa$ at room temperature. The reaction enthalpy (${\Delta}H^{\circ}$) for the hydrogen permeation process was calculated as -7.82 J/mol by Arrhenius plots.

Study on the Synthesis by Mechanical Grinding and Solid-State Reaction Method and the Electochemical Properties of $LiNiO^2$ (기계적 혼합과 고상법에 의한 $LiNiO^2$의 합성과 전기화학적 특성 연구)

  • 윤순도;이재천;박혜령;송명엽
    • 한국전기화학회:학술대회논문집
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    • 2004.06a
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    • pp.281-286
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    • 2004
  • [ $LiOH{\cdot}H^2O$ ]와 $Ni(OH)^2$를 기계적으로 혼합하여 고상법으로 $LiNiO^2$를 합성하고, $LiNiO^2$의 전기화학적 특성을 조사하였다. 기계적 혼합을 위해 SPEC mill을 사용하였으며, 1시간 동안 milling하여 공기 중 $450^{\circ}C$에서 5시간 동안 전처리한 후 $750^{\circ}C$에서 30시간 동안 산소를 흘려주면서 하소한 시료가 가장 좋은 전기화학적 특성을 나타내었다. $2.7\~4.15V$에서 0.1C로 충${\cdot}$방전시 초기방전용량은 그다지 높지 않았으나(145.8mAh/g) 좋은 싸이클 성능을 나타내었으며, $2.7\~4.2V$에서 0.1C로 충${\cdot}$방전시 높은 초기방전용량(164.7mAh/g)을 나타내었으나 싸비클 성능은 그리 좋지 않았는데, 이는 충${\cdot}$방전시 육방구조$(H^2)$에서 육방구조$(H^3)$로의 상전이가 영향을 주는 것으로 사료된다. 초기방전용량과 방전용량은 Cation mixing을 나타내는 $I^{003}/I^{104}$값보다 hexagonal ordering을 나타내는 R-factor에 더 의존하는 것으로 사료된다.

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Isolation and Characterization of Bacteria Able to Grow with Phenol at High Concentrations for Bioremediation (생물학적 환경정화를 위한 고농도 페놀에서 생육할 수 있는 세균의 분리 및 특성)

  • 박연규;손홍주
    • Korean Journal of Environmental Biology
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    • v.19 no.1
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    • pp.87-92
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    • 2001
  • For the biological treatment of industrial wastewater containing high concentration of phenol, isolation and characterization of phenol - degrading bacterium were carried out. A bacterial strain P2 capable of degrading phenol was isolated from contaminated soils by enrichment culture technique and identified as the genus Rhodococcus by morphological, cultural, biochemical characteristics, and Biolog system. The optimal medium composition and cultural conditions for the growth and degradation of phenol by Rhodococcus sp. P2 were 0.1% of (NH$_4$)$_2$SO$_4$, 0.2% of KH$_2$PO$_4$, 0.25% of Na$_2$HPO$_4$ㆍ12$H_2O$, 0.2% of MgSO$_4$ㆍ7$H_2O$, and 0.008% of CaC1$_2$ㆍ2$H_2O$ along with initial pH 8.5 at 3$0^{\circ}C$. Rhodococcus sp. P2 could grow with phenol as the sole carbon source up to 1,800 ppm in batch cultures, but did not grow in medium containing above 2,000 ppm of phenol. When 800 ppm phenol was given in the optimal media, Rhodococcus sp. P2 completely degraded it within 24 h. Meanwhile, 1,800 ppm of phenol was degraded within 9 days. Rhodococcus sp. P2 could utilize toluene, n-hexane, xylene and benzene as sole carbon source .

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Synthesis of solar light responsive ZnO/TaON photocatalysts and their photocatalytic activity (태양광 응답형 ZnO/TaON 나노 복합체의 제조 및 광촉매 특성 평가)

  • Kim, Tae-Ho;Jo, Yong-Hyeon;Lee, Su-Wan
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2014.11a
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    • pp.256-257
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    • 2014
  • The effects of the preparation conditions of ZnO-modified TaON on the photocatalytic activity for degradation of rhodamine B dye (Rh. B) under simulated solar light were investigated. The ZnO/TaON nanocomposite were prepared by loading particulate $Ta_2O_5$ with ZnO using different ZnO contents, followed by thermal nitridation at 1123 K for 5 h under $NH_3$ flow (20 ml min.1). The asprepared samples were characterized by XRD, UV-Vis-DRS, and SEM-EDX. The results revealed that the band gap energy absorption edge of as prepared nanocomposite samples was shifted to a longer wavelength as compared to ZnO and $Ta_2O_5$, and the 60 wt% ZnO/TaON nanocomposite exhibited the highest percentage (99.2 %) of degradation of Rh. B and the highest reaction rate constant ($0.0137min^{-1}$) in 4 h which could be attributed to the enhanced absorption of the ZnO/TaON nanocomposite photocatalyst. Hence, these results suggest that the ZnO/TaON nanocomposite exhibits enhanced photocatalytic activity for the degradation of rhodamine B under simulated solar light irradiation in comparison to the commercial ZnO, $Ta_2O_5$, and TaON.

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