• Title/Summary/Keyword: 6H_2O$

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One-Pot Reaction Involving Two Different Amines and Formaldehyde Leading to the Formation of Poly(Macrocyclic) Cu(II) Complexes

  • Lee, Yun-Taek;Kang, Shin-Geol
    • Bulletin of the Korean Chemical Society
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    • v.33 no.8
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    • pp.2517-2522
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    • 2012
  • New polynuclear poly(hexaaza macrocyclic) copper(II) complexes $[1](ClO_4)_{2n}{\cdot}(H_2O)_{2n}$, $[2](ClO_4)_{2n}{\cdot}(H_2O)_{2n}$, and $[3](ClO_4)_{2n}{\cdot}(H_2O)_{2n}$ have been prepared by the one-pot reaction of formaldehyde with ethylenediamine and 1,2-bis(2-aminoethoxy)ethane, 1,3-diaminopropane, or 1,6-diaminohexane in the presence of the metal ion. The polymer complexes contain fully saturated 14-membered hexaaza macrocyclic units (1,3,6,8,10,13-hexaazacyclotetradecane) that are linked by $N-(CH_2)_2-O-(CH_2)_2-O-(CH_2)_2-N$, $N-(CH_2)_3-N$, or $N-(CH_2)_6-N$ chains. The mononuclear complex $[Cu(H_2L^5)](ClO_4)_4$ ($H_2L^5$ = a protonated form of $L^5$) bearing two $N-(CH_2)_2-O-(CH_2)_2-O-(CH_2)_2-NH_2$ pendant arms has also been prepared by the metal-directed reaction of ethylenediamine, 1,2-bis(2-aminoethoxy)ethane, and formaldehyde. The polymer complexes were characterized employing elemental analyses, FT-IR and electronic absorption spectra, molar conductance, X-ray diffraction (XRD), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and scanning electron micrograph (SEM). Electronic absorption spectra of the complexes show that each macrocyclic unit of them has square-planar coordination geometry with a 5-6-5-6 chelate ring sequence. The polymer complexes as well as $[Cu(H_2L^5)]^{4+}$ are quite stable even in concentrated $HClO_4$ solutions. Synthesis and characterization of the polynuclear and mononuclear copper(II) complexes are reported.

Structural Characterization of Crown Ether Complexed Potassium Ion $(C_{12}H_{24}O_6{\cdot}K)_2K[Co(OH)_6Mo_6O_{18}]{\cdot}12H_2O$

  • Osamu Nagano;Uk Lee;Hikaru Ichida;Yukiyoshi Sasaki
    • Bulletin of the Korean Chemical Society
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    • v.11 no.1
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    • pp.15-19
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    • 1990
  • The crystal structure of $(C_{12}H_{24}O_6{\cdot}K)_2K[Co(OH)_6Mo_6O_{18}]{\cdot}12H_2O$ has been determined by X-ray diffraction. Crystal data as follows ; monoclinic, space group $C_2/m,\;a\;=\;22.512(4)\;{\AA},\;b\;=\;18.304(4)\;{\AA},\;c\;=\;7.641(1)\;{\AA},\;{\beta}\;=\;90.52(2)\;{\AA}$, and Z = 2. A final conventional R value of 0.044 was obtained by least-squares refinement of 4173 independent observed $[{\mid}Fo{\mid}{\geq}3{\sigma}({\mid}Fo{\mid})]$ reflections. The $[Co(OH)_6Mo_6O_}{18}]^{-3}$ polyanion shows the well-known Anderson-structure and has approximate 3m symmetry. A $[Co(OH)_6Mo_6O_{18}]^{-3}$ polyanion is located between two crown ether complexed cations forming a sandwich structure. One potassium ion interacts with the crown ether via electrostatic interactions. The other potassium ion only interacts with the water molecules and terminal oxygen atoms of the polyanion.

The [M(cod)(PPh$_3)_2] PF_6$ (M = Rh, Ir; cod = 1,5-cyclooctadiene) Mediated Activiation of Aldehyde C-H Bond

  • Ko, Jae-Jung;Joo, Wan-Chul
    • Bulletin of the Korean Chemical Society
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    • v.8 no.5
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    • pp.372-376
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    • 1987
  • Acetone solution of quinoline-8-carbaldehyde reacts with $[Rh(cod)(PPh_3)_2] PF_6$and $[Ir(cod)(PPh_3)_2] PF_6$ to yield $[Rh(NC_9H_6CO)(H)(PPh_3)_2(CH_3COCH_3)] PF_6$ (1) and $[Ir(NC_9H_6CO)(H)(PPh_3)_2(CH_3COCH_3)] PF_6$ (2), respectively. The compound $[Ir(cod)(PPh_3)_2] PF_6$ also reacts with $Ph_2PC_6H_4-o-CHO$ in the acetone / $H_2O$ mixture to give $[Ir(Ph_2PC_6H_4-o-CO)(H)(PPh_3)_2(CH_3COCH_3)] PF_6$ (3). Compounds 1, 2, and 3 were characterized by infrared, $^1H$ NMR, $^{31}P$ NMR spectra and conductivity measurement. The $^1H$ NMR spectra of 1, 2, and 3 support the presence of a terminal hydride that is cis to the phosphine. The IR band of 3 at 2185 $cm^{-1}$, which is assigned to $\nu$(Ir-H), and the hydride cleavage reaction of 3 with $CCl_4$, provide evidence for the Ir-H bond.

H2S Gas Sensing Properties of CuO Nanotubes

  • Kang, Wooseung;Park, Sunghoon
    • Applied Science and Convergence Technology
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    • v.23 no.6
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    • pp.392-397
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    • 2014
  • CuO nanotubes are synthesized using $TeO_2$ nanorod templates for application to $H_2S$ gas sensors. $TeO_2$ nanorod templates were synthesized by using the VS method through thermal evaporation. Scanning electron microscopy, transmission electron microscopy and X-ray diffraction showed that the synthesized nanotubes were monoclinic-structured polycrystalline CuO with diameter and wall thickness of approximately 100~300 nm and 5~10 nm, respectively. The CuO nanotube sensor showed responses of 136~325% for the $H_2S$ concentration of 0.1~5 ppm at room temperature. These response values are approximately twice as high as that of the CuO nanowire sensor for the same concentrations of $H_2S$ gas. Along with the investigation of the performance of the sensors, the mechanisms of $H_2S$ gas sensing of the CuO nanotubes are also discussed in this study.

Synthesis and Photo Luminescent Characteristics of SrAl2O4:Eu2+,Dy3+ Phosphor using Polymer Matrix (폴리머 매트릭스를 전구체로 사용한 SrAl2O4:Eu2+,Dy3+ 축광성 형광체의 합성 및 형광 특성)

  • Kim, Soo-Jong;Kwon, Hyuk-Sil
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.20 no.8
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    • pp.671-679
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    • 2007
  • [ $SrAl_2O_4:Eu^{2+},\;Dy^{3+}$ ] phosphor was synthesized using the impregnation method, and its photoluminescence and long-afterglow properties were investigated, A mixture of $Sr(NO_3)_2,\;Al(NO_3)_2\;9H_2O,\;EuCl_3\;6H_2O,\;DyCl_3\;6H_2O,\;NdCl_3\;6H_2O$ salts were dissolved in distilled water and impregnating into the polymer precursor. After drying, the impregnated mixture was heat treated at $900-1400^{\circ}C$ for 2h in a $N_2-H_2$ reduction atmosphere. The microstructure and crystal structure of the $SrAl_2O_4:Eu^{2+},\;Dy^{3+}$ powders were examined by scanning electron microscopy and X-ray diffraction, respectively. The photoluminescence spectra showed an excitation band along over wide wavelength of 250-450nm, and a broaden emission with a maxima peak at 360nm. In addition, the spectra also showed a good long after glow that decayed over a 1000sec period after 10 min excitation illumination.

Effects of Intraperitoneally Administered Lipoic Acid, Vitamin E, and Linalool on the Level of Total Lipid and Fatty Acids in Guinea Pig Brain with Oxidative Stress Induced by H2O2

  • Celik, Sait;Ozkaya, Ahmet
    • BMB Reports
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    • v.35 no.6
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    • pp.547-552
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    • 2002
  • The aim of our study was to investigate the protective effects of intraperitoneally-administrated vitamin E, dl-alpha lipoic acid, and linalool on the level of total lipid and fatty acid in guinea pig brains with oxidative stress that was induced by $H_2O_2$. The total brain lipid content in the $H_2O_2$ group decreased when compared to the $H_2O_2$ + vitamin E (p<0.05), $H_2O_2$ + linalool (p<0.05), ALA (p<0.05), control (p<0.01), linalool (p<0.01), and vitamin E (p<0.01) groups. While the proportion of total saturated fatty acid (${\Sigma}SFA$) in the $H_2O_2$ group significantly increased (p<0.005) when compared to the vitamin E group, it only slightly increased (p<0.01) when compared to the control and $H_2O_2$ + vitamin E groups. The ratio of the total unsaturated fatty acid (${\Sigma}USFA$) in the $H_2O_2$ groups was lower (p<0.05) than the control, vitamin E, and $H_2O_2$ + vitamin E groups. The level of the total polyunsaturated fatty acid (${\Sigma}PUEA$) in the $H_2O_2$ group decreased in when compared to the control, vitamin E, and $H_2O_2$ + vitamin E groups. While the proportion of the total w3 (omega 3), w6 (omega 6), and PUFA were found to be lowest in the $H_2O_2$ group, they were slightly increased (p<0.05) in the lipoic acid group when compared to the control and $H_2O_2$ + lipoic acid groups. However, the level of ${\Sigma}SFA$ in the $H_2O_2$ group was highest; the level of ${\Sigma}USFA$ in same group was lowest. As the proportion of ${\Sigma}USFA$ and ${\Sigma}PUFA$ were found to be highest in the linalool group, they were decreased in the $H_2O_2$ group when compared to the control group. Our results show that linalool has antioxidant properties, much the same as vitamin E and lipoic acid, to prevent lipid peroxidation. Additionally, vitamin E, lipoic acid, and linalool could lead to therapeutic approaches for limiting damage from oxidation reaction in unsaturated fatty acids, as well as for complementing existing therapy for the treatment of complications of oxidative damage.

Thermal Behavior of the Layered Structure in Metal-dodecanesulfonate intercalation compounds, [M($H_2O$)$_6$](C$_12$H$_25$SO$_3$)$_2$.x$H_2O$ (M=Co, Cu) (도데칸술폰이 삽입된 금속 화합물, [M($H_2O$)$_6$(C$_12$H$_25$SO$_3$)$_2$.x$H_2O$ (M=Co, Cu)의 층상 구조의 열적 성질)

  • 허영덕;박성훈;전태현
    • Journal of the Korean institute of surface engineering
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    • v.33 no.1
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    • pp.25-33
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    • 2000
  • The synthesis and characterization of intercalated compound of dodecanesulfornate into hydrated metal, [M($H_2$O)\ulcorner](C\ulcornerH\ulcorner$SO_3$)$_2$.$xH_2$O (M=Co, Cu) was presented. The compounds shows a layered structure which was determined by powder X-ray diffraction. Thermal behavior of the layered structure was investigated using thermal analysis, and FT-IR spectroscopy by varying the temperature. The increase in layer spacing of the products by increasing the temperature is also checked by X-ray diffraction. We can suggest three kinds of layered structure by varying the temperature, which is accompanied by changing the intercalated dodecanesulfonate from the monolayer to the bilayer structure or changing the tilt angle.

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Cationic Iridium(I) Complex of Ethyl Cinnamate and Hydrogenation of Unsaturated Esters with Iridium(I)-Perchlorato Complex

  • Yang, Kyung-Joon;Chin, Chong-Shik
    • Bulletin of the Korean Chemical Society
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    • v.7 no.6
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    • pp.466-468
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    • 1986
  • Reaction of $Ir(ClO_4)(CO)(PPh_3)_2$ with trans-$C_6H_5CH$ = $CHCO_2C_2H_5$ produces a new cationic iridium(I) complex, [Ir (trans-$C_6H_5CH$ = $CHCO_2C_2H_5)(CO)(PPh_3)_2]ClO_4$ where trans-$C_6H_5CH$ = $CHCO_2C_2H_5$ seems to be coordinated through the carbonyl oxygen rather than through the $\pi$-system of the olefinic group according to the spectral data. It has been found that Ir$(ClO_4)(CO)(PPh_3)_2$ catalyzes the hydrogenation of $CH_2$ = $CHCO_2C_2H_5$, trans-$CH_3CH$ = $CHCO_2C_2H_5$ and trans-$C_6H_5CH$ = $CHCO_2C_2H_5$ to $CH_3CH_2CO_2C_2H_5$, $CH_3CH_2CH_2CO_2C_2H_5$ and $C_6H_5CH_2CH_2CO_2C_2H_5$, respectively at room temperature under the atmospheric pressure of hydrogen. The relative rates of the hydrogenation of the unsaturated esters are mostly understood in terms of steric reasons.

Morphological Changes of $K_2$$Ti_4$$O_9$ fiber for the Immobilization of Nuclear Waste Metal tons (방사능이온의 고정화를 위한 $K_2$$Ti_4$$O_9$ 섬유의 형상변화)

  • 정경택;문제권;서용철;설용건;오원진
    • Proceedings of the Korea Society for Energy Engineering kosee Conference
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    • 1995.11a
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    • pp.71-74
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    • 1995
  • 티타니아계의 흡착제로 최근 주목을 끄는 것은 티탄산칼륨 신소재를 들을 수 있다. 모서리의 chains sharing들과 b축을 따라서 TiO$_{6}$, 즉 8면체의 coner 결합으로 특징 지워지는 티탄산칼륨은 $K_2$O.nTiO$_2$로 표시되는 화합물로 플라스틱의 보강재나 단열재료 용도로 사용되었다. 공업재료로서 중요한 것은 n의 값이 2, 4, 6으로 각각 2티탄산칼륨(K$_2$Ti$_2$O$_{5}$), 4티탄산칼륨(K$_2$Ti$_4$O$_{9}$), 6티탄산칼륨(K$_2$Ti$_{6}$O$_{13}$)으로 불린다. 티탄산칼륨은 기계적 강도가 고강도재료 지르코이나에 해당하고 선팽창계수는 알루미나보다 작아 우수한 내열 및 단열 고강도재료이며 융막재, 이온교환재등으로 쓰인다. 층상구조의 티탄산칼륨을 산처리하여 칼륨을 추출하고 수소이온으로 치환한 결정질 티탄산칼륨 섬유(H$_2$Ti$_4$O$_{9}$.1.2~1.3$H_2O$)는 (H$^{-}$. H$_3$O$^{+}$)Ti$_4$O$_{9}$의 형태를 지니게 된다.

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Examination of Berberine Dye using GC-MS after Selective Degradation Treatments (GC-MS를 이용한 Berberine 염료의 퇴화 거동 연구)

  • Ahn, Cheun-Soon
    • Journal of the Korean Society of Clothing and Textiles
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    • v.33 no.12
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    • pp.2002-2010
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    • 2009
  • The degradation behavior of berberine is examined using GC-MS to select the fingerprint products that can be used to identify berberine dye in badly faded archaeological textiles. A total of $100^{\circ}C$ thermal and $H_2O_2/UV/O_2$ degradation systems were used to degrade berberine chloride 0.1% solution up to 408 hours. The samples were analyzed using the GC-MS. Dihydroberberine, 2-pteridinamine, 6,7-dimethyl-N-[(trimethylsilyl) oxy]-, and 8-methoxy-11-[3-methylbutyl]-11H-indolo[3,2-c]-quinoline, 5-oxide were detected as the major products of thermal degradation and identified as the fingerprint products for berberine dye at the early stage of degradation. Isobenzofuran-1,3-dione,4,5-dimethoxy-, 9H-fluorene,3,6-bis(2-hydroxyethyl)-,1,3-dioxolo[4,5-g]isoquinolin-5(6H)-one,7,8-dihydro-, and 3-tert-butyl-4-hydroxyanisole were detected as the major products generated by the $H_2O_2/UV/O_2$ degradation and identified as the fingerprint products for berberine dye under severe degradation conditions.