• Title/Summary/Keyword: elemental analysis

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A Two-Dimensional Terrace-Like N-heterocyclic-Pb(II) Coordination Compound: Structure and Photoluminescence Property

  • Ma, Kui-Rong;Zhu, Yu-Lan;Zhang, Yu;Li, Rong-Qing;Cao, Li
    • Bulletin of the Korean Chemical Society
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    • v.32 no.3
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    • pp.894-898
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    • 2011
  • The first example of lead compound from $Pb(NO_3)_2$ and $H_3L$ N-heterocyclic ligand $(H_3L\;=\;(HO_2C)_2(C_3N_2)(C_3H_7)CH_2(C_6H_4)(C_6H_3)CO_2H)$, $[Pb_4(L')_4]{\cdot}5H_2O$ 1 (L' = OOC$(C_3H_7)(C_3N_2)CH_2(C_6H_4)(C_6H_3)COO)$, has been obtained under hydrothermal condition by decarboxylation, and characterized by elemental analysis, IR, TGDTA, and single-crystal X-ray diffraction. Compound 1 possesses a rare two-dimensional upper-lower offset terrace-like layer structure. In 1, crystallographic distinct Pb(II) ion adopts five-coordination geometry, and two lattice water molecules occupy the voids between 2-D layers. Results of solid state fluorescence measurement indicate that the emission band 458 nm may be assigned to $\pi^*-n$ and $\pi^*-\pi$ electronic transitions within the aromatic systems of the ligand L', however, the emission bands centred at 555 nm, 600 nm and 719 nm may be derived from phosphorescent emission ($\lambda_{excitation}$ = 390 nm).

Synthesis, Characterization and Property Studies on a Dinuclear Copper(II) Complex with Dipyridine Derivate and Acetylacetone

  • Zhao, Pu Su;Guo, Zhi Yan;Sui, Jing;Wang, Jing;Jian, Fang Fang
    • Bulletin of the Korean Chemical Society
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    • v.32 no.1
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    • pp.49-52
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    • 2011
  • A dinuclear copper(II) complex of [$Cu_2(aceace)_4$(dipyph)] [aceace = acetylacetone, dipyph = 1,4-di(4-pyridylethene-2-yl-)benzene] has been synthesized and characterized by elemental analysis, IR and X-ray single crystal diffraction. It crystallizes in the monoclinic system, space group P21/c, with lattice parameters a = 7.9584(16) $\AA$, b = 18.594(4) $\AA$, c = 15.063(4) $\AA$ $\beta=120.97(2)^o$ and $M_r$ = 807.85 ($C_{40}H_{44}Cu_2N_2O_8$), Z = 2. Each of the $Cu^{2+}$ ion adopts a square pyramid geometry and coordinates with four oxygen atoms from two aceace ligands and one nitrogen atom from dipyph bidentate ligand. Magnetic measurement shows that the Weiss constant and Curie constant for the title compound are -0.22 K and 0.1154 emu K/mol, respectively. Thermal stability data indicate that the title complex undergoes two steps decomposition and the residue is $Cu_2O_4$. In the potential range of -1.5 ~ 0.8 V, the title complex represents an irreversible electrochemical process.

Preparation and Polymerization of Alkenylsilanes (Alkenylsilane의 제조와 고분자화반응)

  • Kim, Chung Kyun;Choi, Soon Kyu;Park, Eun Mi;Jung, In Kyung
    • Journal of the Korean Chemical Society
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    • v.41 no.2
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    • pp.88-97
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    • 1997
  • The silyltriflates$(Ph_{3-n}SiH(OTf)_n)$have been produced by the reaction of triphenylsilane and triflic acid$(CF_3SO_3H)$at low temperature. These highly reactive compounds are a valuable reagent for the synthesis of numerous new functional substituted silane derivatives. The reaction of silyltriflates with alkenyl- and alkynylmagnesium bromide as well as organolithium compounds gave new silanes$Ph_2SiHR(R=\;C(CPh,\;CH=CH_2,\;CH_2CH=CH_2,\; (CH_2)_2CH=CH_2,\;(CH_2)_3CH=CH_2)$in high yields. The hydrosilation of prepared alkenyl- and alkynylsilanesPh_2SiHR$in the presence of a platinum catalyst(Pt/C) at high temperature$(200{\circ}C)$gave carbosilane polymers$((Ph_2SiCH=CPh)_n$and$(Ph_2Si(CH_2)m)n;\;m=2∼4, n{\ge}10)$along with five- and six-membered silaalkane ring compounds derived from intramolecular hydrosilation reactions. All of the prepared compounds are confirmed by NMR, UV, IR and mass spectroscopy as well as elemental analysis.

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Metal-Nitrosyl Complexes(II) : Synthesis and Characterization of Dinitrosyltungsten(O) Complexes (금속-니트로실 착물 (제 2 보) : 디니트로실 텅스텐(O) 착물의 합성과 특성)

  • Sang-Oh Oh;Seong-Jong Mo
    • Journal of the Korean Chemical Society
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    • v.36 no.6
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    • pp.906-913
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    • 1992
  • The polymeric compound [{$W(NO)_2Cl_2$}$_n$] were prepared by reductive nitrosylation of $WNaNO_2$ and acidified $WFeSO_4$ with $WWCl_6$ at room temperature. The reactions of [{$W(NO)_2Cl_2$}$_n$] with unidentate and bidentate ligands afforded neutral monomeric [$W(NO)_2Cl_2L_2$(or L-L)] in a relative high yields (70$\sim$90%). 3,5-lutidine, ${\gamma}$-cyanopyridine, 1,2-phenylenediamine, 1,10-phenanthroline, sym-diphenylethylenediamine, 9,10-phenanthrenequinone, 1,3-bis(diphenylphosphino)propane, 1,1'-bis(diphenylphosphino)ferrocene and 8-hydroxyquinoline were used as coordinating ligands. These dinitrosyltungsten complexes were characterized by elemental analysis, $^1H$-NMR, infrared, and UV-visible spectroscopy are reported. The spectral data indicated that geometric structures of the products were cis-dinitrosyl-trans-dichloro-cis-$L_2$ of $C_{2v}$ symmetry.

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Synthesis, Crystal Structure and Quantum Chemistry of a Novel Schiff Base N-(2,4-Dinitro-phenyl)-N'-(1-phenyl-ethylidene)-hydrazine

  • Ji, Ning-Ning;Shi, Zhi-Qiang;Zhao, Ren-Gao;Zheng, Ze-Bao;Li, Zhi-Feng
    • Bulletin of the Korean Chemical Society
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    • v.31 no.4
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    • pp.881-886
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    • 2010
  • A novel Schiff base N-(2,4-dinitro-phenyl)-N'-(1-phenyl-ethylidene)-hydrazine has been synthesized and structurally characterized by X-ray single crystal diffraction, elemental analysis, IR spectra and UV-vis spectrum. The crystal belongs to monoclinic with space group P21/n. The molecules are connected via intermolecular O-$H{\cdots}O$ hydrogen bonds into 1D infinite chains. The crystal structure is consolidated by the intramolecular N-$H{\cdots}O$ hydrogen bonds. weak intermolecular C-$H{\cdots}O$ hydrogen bonds link the molecules into intriguing 3D framework. Furthermore, Density functional theory (DFT) calculations of the structure, stabilities, orbital energies, composition characteristics of some frontier molecular orbitals and Mulliken charge distributions of the title compound were performed by means of Gaussian 03W package and taking B3LYP/6-31G(d) basis set. The time-dependent DFT calculations have been employed to calculate the electronic spectrum of the title compound, and the UV-vis spectra has been discussed on this basis. The results show that DFT method at B3LYP/6-31G(d) level can well reproduce the structure of the title compound.

Temperature Dependence of Activation and Inhibition of Mushroom Tyrosinase by Ethyl Xanthate

  • Alijanianzadeh, M.;Saboury, A.A.
    • Bulletin of the Korean Chemical Society
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    • v.28 no.5
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    • pp.758-762
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    • 2007
  • A new alkyldithiocarbonate (xanthate), as sodium salts, C2H5OCS2Na, was synthesized by the reaction between CS2 with ethyl alcohol in the presence of NaOH. The new xanthate was characterized by 1H NMR, IR and elemental analysis. Then, the new synthesized compound was examined for functional study of cresolase activity of Mushroom Tyrosinase (MT) from a commercial source of Agricus bisporus in 10 mM phosphate buffer pH 6.8, at three temperatures of 10, 20 and 33℃ using UV spectrophotemetry. 4-[(4-methylphenyl)- azo]-phenol (MePAPh) was used as a synthetic substrate for the enzyme for cresolase reaction. The results show that ethyl xanthate can activate or inhibit the cresolase activity of mushroom tyrosinase depending to the concentration of ethyl xanthate. It was concluded that the enzyme has two distinct sites for ethyl xanthate. The first one is a high-affinity activation site and the other is a low-affinity inhibition site. Activation of the enzyme in the low concentration of ethyl xanthate arises from increasing the affinity of binding for the substrate as well as increasing the enzyme catalytic constant. The affinity of ligand binding in the activation site is decreased by increasing of the temperature, which is the opposite result for the inhibition site. Hence, the nature of the interaction of ethyl xanthate is different in two distinct sites. The binding process for cresolase inhibition is only entropy driven, meanwhile the binding process for cresolase activation is not only entropy driven but also enthalpy driven means that hydrophobic interaction is more important in the inhibition site.

Synthesis, DNA Photocleavage and Singlet Oxygen Measurement of Cationic Bisporphyrins

  • Wang, Kai;Jin, Qi;Zhang, Xiulan;Song, Shuai-Hua
    • Journal of the Korean Chemical Society
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    • v.57 no.2
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    • pp.246-251
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    • 2013
  • With -$OCH_2CO$- as a linker, a non ${\beta}$-substituted cationic bisporphyrin (4a) and a ${\beta}$-substituted cationic bisporphyrin (4b) were prepared through methylation of the intermediate which was obtained from ${\beta}$-amino-5,10,15,20-tetra (4-cyanophenyl) porphyrin or 5-hydroxylphenyl-10,15,20-tris(4-cyanophenyl) reacting with 5-hydroxy-10,15,20-trispyridinylporphyrin. Their structures were confirmed by $^1H$ NMR, IR, UV-vis, MS and elemental analysis. DNA photocleavage ability and the singlet oxygen ability of those cationic bisporphyrins were investigated. DNA photocleavage activity of ${\beta}$-substituted cationic bisporphyrin was significantly weaker than that of $H_2TMPyP$, but similar to that of non ${\beta}$-substituted cationic bisporphyrin. While 4a and 4b showed substantial photocleavage activities toward DNA, with 68% and 66% observed at 10 ${\mu}M$. The assessment of indirectly measured $^1O_2$ production rates against $H_2TMPyP$ were described and the relative singlet oxygen production yields were: free cationic bisporphyrins > $H_2TMPyP$. The results showed the cationic bisporphyrins with ${\beta}$-substitution and non ${\beta}$-substitution could be developed as potential photodynamic agents.

Characterization of Fe-ACF/$TiO_2$ composite Photocatalysts Effect Via Degradation of MB Solution (Fe-ACF/$TiO_2$ 복합체의 특성과 MB용액의 분해에서 포토-펜톤 효과)

  • Zhang, Kan;Meng, Ze-Da;Ko, Weon-Bae;Oh, Won-Chun
    • Elastomers and Composites
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    • v.44 no.3
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    • pp.290-298
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    • 2009
  • In this paper, the Fe-activated carbon fiber (ACF)/$TiO_2$ composite catalysts were prepared by a sol-gel method. The synthesized photocatalysts were used for the photo degradation of Methylene blue solution under UV light. From Brunauer-Emmett-Teller measurements (BET) data, it was shown the blocking of the micropores on the surface of ACF by treatment of Fe and Ti compound. As shown in SEM images, the ferric compounds and titanium dioxides were fixed onto the ACF surfaces. The result of X-ray powder diffraction showed that the crystal phase contained a mixing anatase and rutile structure and the 'FeO+$TiO_2$' from the composites. The EDX spectra for the elemental analysis showed the presence of C, O, and Ti with Fe peaks. Degradation activity of MB could be attributed to +OH radicals derived from electron/hole pair's reactions due to photolysis of $TiO_2$ and photo-Fenton effect of Fe.

Polyoxyethylene Tocopheryl Ethers; A Series of Novel Surfactants from Tocopherol for Functional Cosmetics (토코페롤에서 유도된 기능성 화장품용의 새로운 계면 활성제)

  • 김영대;김창규
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.18 no.1
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    • pp.1-41
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    • 1992
  • A new and unique class of nonionic surfactants was synthesized by reacting biological a-tocopherol with ethylene oxide for functional cosmetics. The structures were confirmed by Hl-UMR, FT-lR, TLC and elemental analysis. POV and conjugated diene value study for EPO showed POE(n)TE had antioxidative effect similar to tocopheryl acetate Protective effect on cell membrane in photohemolysis of POE(5)TE, POE(10)TE and POE(18)TE were slightly lower than tocopherol but higher than nonoxynol-12, and POE(10)TE had UV absorption power comparable with tocopherol and homosalate. Biological activity of the hydrophobic group of the new surfactants make them unique and different from those of conventional nonionic surfactants Systematic safety evaluations of POE(n)TEs on the skin and eye proved that they are as safe as tocopherol. The results of physicochemical study showed POE(10)TE had the lowest CMC value, POE(18)TE had the maximum surface tension reduction and the highest foam volume and POE(n)TEs had various HLB values by the degree of ethoxylation. The test resul Is of technological and practical applications of these surfactants for cosmetics showed some POE(n)TEs were superior to conventional surfactants. POE(5)TE in W/O emulsions, POE(10)TE and POE(12)TE in O/W emulsions, POE(12)TE in dispersions, POE(18)TE in solubilizations and POE(50)TE in gelations were shown to be excellent which was considered due to the structural characteristic and formation of liquid crystals of POE(n)TEs. By the development and applications of these excel lent multi-functional surfactants, innovative functional cosmetics were successfully formulated.

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Densified Fuels from Poplars (포플러로부터 고밀화연료의 제조)

  • 한규성;최돈하
    • Journal of Korea Foresty Energy
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    • v.21 no.3
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    • pp.59-65
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    • 2002
  • Recently, densified fuels from biomass are widely used North America and Europe as a regenerable and clean bioenergy. Compaction of sawdust of poplars(Populus tomentiglandulosa and Populus davidiana) with starch glue for densified fuel were studied. Calorific and elemental analysis were carried out to assess these species as fuel. Hot-press process was used and compaction was performed under temperatures from 120 to $160^{\circ}C$ and at pressure of 50kgf/$cm^2$ for prescribed time. Densified fuels were evaluated by its specific gravities, compressive strengths and fines. In the case of with-glue system, when the press temperature is $160^{\circ}C$ and press time is above 7.5 minutes, densified fuels with fines less than 5% can be produced. On the contrary, in the case of without-glue system, densified fuels with fines less than 5% can be produced by controlling the press conditions and the moisture content of sawdust.

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