• Title/Summary/Keyword: IR Spectrophotometry

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Interaction Studies of a Novel, Water-Soluble and Anti-Cancer Palladim(II) Complex with Calf Thymus DNA

  • Mansouri-Torshizi, H.;Saeidifar, M.;Divsalar, A.;Saboury, A.A.;Shahraki, S.
    • Bulletin of the Korean Chemical Society
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    • v.31 no.2
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    • pp.435-441
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    • 2010
  • We report the preparation and characterization of a new and water soluble complex of palladium(II) with 1,10- phenanthroline and butyldithiocarbamate ligands. This compound has been studied through spectroscopic techniques, $^1H$ NMR, IR, electronic spectra and elemental analysis and conductivity measurements. The complex shows 50% cytotoxic concentration ($Ic_{50}$) value against chronic myelogenous leukemia cell line, K562, much lower than that of cisplatin. Thus the mode of binding of this complex to calf thymus DNA have been extensively investigated by isothermal titration UV-visible spectrophotometry, fluorescence, gel filteration and other methods. UV-visible studies show that the complex exhibits cooperative binding with DNA and remarkably denatures the DNA at extremely low concentration ($~13\;{\mu}M$). Fluorescence studies indicate that the complex intercalate into DNA. Gel filtration studies suggest that the binding of Pd(II) complex with DNA is strong enough that it does not readily break. In these interaction studies, several thermodynamic and binding parameters are also determined which may reflect the mechanism of action of this type of compound with DNA.

Free-Radical Copolymerization of Glycidyl Methacrylate with Phthalimidoethyl Acrylate : Synthesis and Determination of Monomer Reactivity Ratios (GMA와 프탈이미드아크릴레이트의 공중합체 합성과 반응성비)

  • Oh, Seung-Min;Oh, Dae-Hee
    • Journal of the Korean Applied Science and Technology
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    • v.30 no.2
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    • pp.297-304
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    • 2013
  • Free-radical copolymerization of glycidyl methacrylate(GMA) and N-phthalimidoethyl acrylate(NPEA) were carried out at $60^{\circ}C$ in dimethylformamide(DMF) solution in the presence of benzoylperoxide(BPO) at low conversion. The polymers were characterized by IR and $^1H$-NMR. The compositions of the copolymer was analyzed by ultra violet(UV/Vis) spectrophotometry. The reactivity ratios of the monomer was determined by the application of Fineman-Ross(FR) and Kelen-T$\ddot{u}$d$\ddot{o}$s(KT) methods. The monomer reactivity ratios of the system and Alfrey-Price's resonance effect(Q) and polar effect(e) value for NIEA were determined as follow. The reactivity ratios of the monomer obtained from FR and KT are found to be $r_1$=0.87, $r_2$=0.98 and $r_1$=0.88, $r_2$=0.99 respectively. The Q and e values of poly(GMA-co-NPEM) calculated from $r_1$ and $r_2$ was Q= 1.31, e=0.75 respectively.

Synthesis and Characterization of 2, 6-Di-(4'-Methyl Phenyl) Pyrylium Fluoroborate and Perchlorate in Single Step Salts Using 4'-Methyl Acetophenone

  • Wie, Jin-Hyeong;Hong, Young-Min;Kim, Hyun-Ook;Kim, Kyung-Hoon;Cho, Sung-Il
    • Journal of Sensor Science and Technology
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    • v.21 no.1
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    • pp.13-20
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    • 2012
  • Due to its high conductivity, pyrylium has been frequently used in electron transfer reactions or in the synthesis of various organic materials. It has also been used as a sensor material. Traditionally, the compounds have been synthesized using various methods; mostly in a multiple steps. In this study, two pyrylium salts, 2, 6-di-(4'-methylphenyl) pyrylium fluoroborate and perchlorate were synthesized. The synthesis of these products was confirmed by 1H-NMR, LC/TOF-MS and FT-IR analyses while their photo-properties were analyzed using UV/VIS spectrophotometry. In addition, the electron transfer capacities of the salts were analyzed with a conductivity meter, it was found that their electron conductivities were high. When the synthesized compounds were dissolved in acetone, a green fluorescent material was observed to form. The fluorescent material can be used as a sensitizer in the electrical industry.

Removal of benzene from aqueous solution by TMA-Zeolite complex (TMA-Zeolite Comphx 에 의한 수용액(水溶液)중 Benzene 제거(除去))

  • Lee, Chan-Il;Lee, Dong-Hoon;Choi, Jyung
    • Korean Journal of Environmental Agriculture
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    • v.17 no.1
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    • pp.43-47
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    • 1998
  • This study was performed to remove the dissolved benzene in water by using TMA-Zeolite complex which was formed by the adsorption of TMA(Tetramethyl ammonium), a kind of ration surfactant on a natural zeolite produced in Korea. The dorminant clay minerals of the natural zeolite was identified by X-ray diffractometry and Infrared spectrophotometry to be mordenite and clinoptilolite. The CEC of the zeolite used was 95.9 cmol/kg. TMA was adsorbed on natural zeolite very quickly, and the amount of TMA adsorption on zeolite was known to be equivalent to about 8% of the CEC of natrual zeolite. The amount of benzene adsorption on TMA-zeolite complex was much more than natural zeolite, indicating that the dissolved benzene in water could be removed effectively by TMA-zeolite comple.

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Tetradiazo(o-carboxy)phenylcalix[4]arene for Determination of Pb2+ Ion

  • Tan, Le Van;Quang, Duong Tuan;Lee, Min-Hee;Kim, Tae-Hyun;Kim, Ha-Suck;Kim, Jong-Seung
    • Bulletin of the Korean Chemical Society
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    • v.28 no.5
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    • pp.791-794
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    • 2007
  • A new azocalix[4]arene, 5,14,17,23-tetra[(2-benzoic acid)(azo)phenyl] calix[4]arene (2), has been prepared by hydrolysis of its ester derivative and characterized by 1H NMR, IR, UV-Vis spectroscopy and elemental analysis. Based on UV spectral changes, we found that 2 exhibits Pb2+ ion selectivity. In basic media, Pb2+ forms a 1:1 complex with the ligand. Beer's law is obeyed in the range of 2.0 × 10?6 ? 2.4 × 10?5 mol L?1 of Pb2+. The molar absorptivity (ε ) of 2-Pb2+ complex is 1.89 × 104 L mol?1 cm?1 at 440 nm, and the detection limit is 1.6 × 10?6 mol L?1.

Studies on the carotenoids in the viscera of abalone (Haliotis discus hannai) (전복(Haliotis discus hannai) 내장(內臟)의 Carotenoid에 관(關)한 연구(硏究))

  • Ahn, Seung-Yo
    • Applied Biological Chemistry
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    • v.17 no.4
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    • pp.257-274
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    • 1974
  • The studies on the carotenoids in the viscera of abalone (Haliotis discus hannai) have been-carried out. The pigments were extracted with acetone-methanol mixture (4 : 1) from the viscera of abalones which were caught around the coastal water of Korea from March to August. The individual carotenoid in the extracts was separated and purified by the silica gel TLC, $Mg(OH)_2$ impregnated paper chromatography and $Mg_2(OH)_2CO_3$ TLC. The isolated eleven carotenoids were investigated and identified by epoxide test, partition test, reduction with sodium borohydride, alkaline hydrolysis, co-chromatography and comparative test with reference carotenoids and electronic and IR absorption spectrophotometry. ${\alpha}$-Carotene, ${\beta}$-carotene. lutein, zeaxanthin, siponaxanthin, siponein, fucoxanthin, loroxan-thin-like and fucoxanthinol-like have been identified among the eleven carotenoids isolated. It has been found that fucoxanthin, on alkaline treatment, was transformed to the product of which chromophore was the same one as fucochrome and semifucoxanthol. Among the identified nein carotenoids siphonaxanthin, siponein, fucoxanthin, loroxanthin-like and fucoxanthinol-like have not been reported previously to be contained in the shellfish.

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The Investigation of a Novel Indicator System for Trace Determination and Speciation of Selenium in Natural Water Samples by Kinetic Spectrophotometric Detection

  • Gurkan, Ramazan;Ulusoy, Halil Ibrahim
    • Bulletin of the Korean Chemical Society
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    • v.31 no.7
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    • pp.1907-1914
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    • 2010
  • A novel catalytic kinetic method is proposed for the determination of Se(IV), Se(VI) and total inorganic selenium in water based on the catalytic effect of Se(IV) on the reduction of bromate by p-nitrophenylhydrazine at pH 3.0. The generated bromine, $Br_2$ or $Cl_2$ plus $Br_2$ in 0.1 M NaCl (or NaBr) environment efficiently decolorized Calmagite and the reaction was monitored spectrophotometrically at 523 nm as a function of time. In this indicator reaction, bromide acted as an activator for the catalysis of selenium (IV) and a reducing agent for selenium (VI) at pH 3.0, which allowed the determination of total selenium. The fixed time method was adopted for the determination and speciation of inorganic selenium. Under the optimum conditions, the calibration graph are linear in the range 1 - 35 ${\mu}gL^{-1}$ of Se(IV) for the fixed time method at $25^{\circ}C$. The detection limit based on statistical $3S_{blank}$/m-criterion was 0.215 ${\mu}gL^{-1}$ for the fixed time method (7 min). All of the variables that affect the sensitivity at 523 nm were investigated, and the optimum conditions were established. The interference effect of various cations and anions on the Se (IV) determination was also studied. The selectivity of the selenium determination was greatly improved with the use of the strongly cation exchange resin such as Amberlite IR120 plus. The proposed kinetic method was validated statistically and through recovery studies in natural water samples. The RSDs for ten replicate measurements of 5, 15 and 25 ${\mu}gL^{-1}$ of Se(IV) and Se(VI) was changed between 2.1 - 4.85%. Analyses of a certified standard reference material (NIST SRM 1643e) for selenium using the fixed-time method showed that the proposed kinetic method has good accuracy. Se(IV), Se(VI) and total inorganic selenium in environmental water samples have been successfully determined by this method after selective reduction of Se(VI) to Se(IV).

Studies on the Constituents of Spiraea Koreana Nakai (참조팝나무의 成分 Alkaloid 에 關한 硏究)

  • Jin, Kab-Dukc
    • Journal of the Korean Chemical Society
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    • v.11 no.3
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    • pp.111-116
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    • 1967
  • A new alkaloid named Spirajine(m.p. 182~$184^{\circ}C$ $[{\alpha}]d^{19}+3.4^{\circ}$ in $CHCl_3$, $C_{23}H_{33}NO_3$, colorless prism) was isolated from the leaves of Spiraea Koreana Nakai (Spiraeceae) (Korean name "Chamjopab namu") which grows in the mountaineous area of Korea, by process of Scheme I (yields 0.13%). Another two unidentified alkaloids (not yet crystallized) were separated by the method of thin layer chromatography. (The Rf values of the two unidentified alkaloids were 0.66, 0.77, respectively and Spirajine 0.72) Spirajine were subjected to the structural investigation with the use of ultra violet and infra red spectrophotometry, and opical rotatory dispersion. The alkaloid contains two ketonic carbonyl groups, tertiary hydroxyl group, methyl groups, N-methyl group and both cyclohexane ring and cyclopentane ring.

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Synthesis of TiO2-Fe2O3 Nanocomposite Powders for Magnetic Photocatalyst (자성광촉매용 TiO2-Fe2O3 나노복합분말의 합성)

  • Lee Chang-Woo;Kim Soon-Gil;Yun Sung-Hee;Lee Jai-Sung;Choa Yong-Ho
    • Korean Journal of Materials Research
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    • v.15 no.8
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    • pp.508-513
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    • 2005
  • [ $TiO_2-Fe_2O_3$ ] nanocomposite powders for magnetic photocatalyst were synthesized by sol-gel process, in which $TiO_2$ photocatalytic layer was formed on the surface of $\gamma-Fe_2O_3$ magnetic core. Transmission electron microscopy (TEM) observation and X-ray diffractometry (XRD) analysis revealed that$\gamma-Fe_2O_3$ nanoparticles, $10\~20nm$ in diameter, were coated by $TiO_2$ shell of 5nm in thickness and $TiO_2$ was anatase phase. Also hydroxyl group (-OH) used to decompose organic compounds was detected by Fourier transformation infrared spectrometry(FT-IR) analysis. UV-Visible spectrophotometry results showed that light absorption occurred in the wavelength range of $400\~700 nm$, and the band gap energy $(E_g)$ of powder was 1.8 eV. Finally it was found that the coercivity $(H({ci})$ and saturation magnetization $(M_s)$ of the powder were 79 Oe and 14.8 emu/g, respectively as experimental vibrating sample magnetometer (VSM) measurements.

A Study on the Synthesis and Physical Properties of N-acyloxyethyl carboxybetaine Type Amphoteric Surfactants (N-acyloxyethylcarboxybetaine 형 양성계면활성제의 합성과 물성에 관한 연구)

  • Kim, Yong-In;Soh, Hie-Jeun;Oh, Yang-Hwan;Kim, Byung-Kie
    • Journal of the Korean Applied Science and Technology
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    • v.6 no.1
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    • pp.31-40
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    • 1989
  • Five novel amphoteric surfactants of N-acyloxyethylcarboxybetaine series were synthesized via Schotten-Baumman reaction between five acid chlorides containing 10, 12, 14, 16 and 18 carbon atoms in their N-alkyl groups and dimethylaminoethanol to give the intermediate products, 2-dimethylaminoethylalkanoates(2). Quaternization of these products(2) was permitted to from 2-(acyloxyethyldimethylammonic)- acetates(3), whose structures were identified by elemental analysis, IR spectrophotometry and $^1Hnmr$ spectrometry. The yield of the final products was shown in the range of 77-80% based on the intermediate products. The surface tension of the aqueous solution of (3) was measured, and the critical micelle concentrations (cmc) were shown in the range of $2.1\;{\times}\;10^{-3}\;-\;3.3\;{\times}\;10^{-4}mol/l$, and the surface tension at cmc was 28-36 dyne/cm. Cmc was lowered gradually by the increment of the length of N-alkyl ester containing group. The isoelectric point was shown in the range of 4.44-5.20. It showed a tendency to lean toward the acidic site and its range was broadened as increase of the hydrophobic group length. A linear relationship between log cmc and the number of carbon atoms(N) in the hydrophobic alkyl chain was shown in the relative equation of log cmc=-1.75-0.1N, and the contribution rate of N on the standard free energy change in micellization, ${\bigtriangleup}({\bigtriangleup}G^{\circ}m)/{\bigtriangleup}N$, was calculated as -0.23 RT.