• Title/Summary/Keyword: Dioxime

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Synthesis of a New α-Dioxime Derivative and Its Application for Selective Homogeneous Liquid-Liquid Extraction of Cu(II) into a Microdroplet Followed by Direct GFAAS Determination

  • Ghiasvand, A. R.;Shadabi, S.;Kakanejadifard, A.;Khajehkoolaki, A.
    • Bulletin of the Korean Chemical Society
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    • v.26 no.5
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    • pp.781-785
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    • 2005
  • A fast and reliable method for the selective separation and preconcentration of $Cu^{2+}$ ions using homogeneous liquid-liquid extraction was developed. A new $\alpha$-dioxime derivative (2H-1,4-benzothioazine-2,3(4H)dionedioxime, Dioxime I) was synthesized and investigated as a suitable selective complexing ligand for $Cu^{2+}$ ions. Zonyl FSA (FSA) was applied as a phase-separator agent under the slightly acidic pH conditions. Under the optimal experimental conditions ([FSA] = 3.2% w/v, [THF] = 19.5% v/v, [Dioxime I] = 1.9 ${\times}\;10^{-3}$ M, and pH = 4.7), 10 ${\mu}g\;of\;Cu^{2+}$ in 5.2 mL aqueous phase could be extracted quantitatively into 80 $\mu$L of the sedimented phase. The maximum concentration factor was 65-fold. The limit of detection of the proposed method was 0.005 ng $mL^{-1}$. The reproducibility of the proposed method, on the 10 replicate measurements, was 1.3%. The influence of the pH, type and volume of the water-miscible organic solvent, concentration of FSA, concentration of the complexing ligand and the effect of different diverse ions on the extraction and determination of $Cu^{2+}$ ions were investigated. The proposed method was applied to the extraction and determination of $Cu^{2+}$ ion in different synthetic and natural water samples.

Spectrophotometric Determination of Copper(II) Using Diamine-Dioxime Derivative

  • Thipyapong, Khajadpai;Suksai, Chomchai
    • Bulletin of the Korean Chemical Society
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    • v.24 no.12
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    • pp.1767-1770
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    • 2003
  • A simple, rapid and sensitive spectrophotometric method is herewith proposed for the determination of copper(II) by using diamine-dioxime ligand, meso-3,6,6,9-tetramethyl-4,8-diazaundecane-2,10-dione dioxime or meso-HexaMethyl Propylene Amine Oxime (meso-HMPAO). This method is based on the formation of a stable 1 : 1 red-pink complex between copper(II) and meso-HMPAO in aqueous solution. Absorption measurements were carried at 497 nm, with a molar absorptivity value of 338 L $mol^{-1}\;cm^{-1}$. Beer's law was obeyed over the concentration range of 0.5-370 ${\mu}$g $mL^{-1}$ with a Sandell's sensitivity value of 0.18 ${\mu}$g $cm^{-2}$. The proposed method has been successfully applied for determination of copper(II) in foodstuffs and pharmaceutical samples. The results obtained from this method are comparable with those obtained AAS.

Preparation of Organic-inorganic Hybrid PES Membranes using Fe(II) Clathrochelate (Fe(II) clathrochelate을 이용한 유.무기 PES 복합막의 제조)

  • Jung, Bo Ram;Son, Yeji;Lee, Yong Taek;Kim, Nowon
    • Membrane Journal
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    • v.23 no.1
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    • pp.80-91
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    • 2013
  • Metal-templated condensation of cyclohexanedione dioxime and phenylboronic acid in the presence of Fe(II) sulfate heptahydrate proceeds cleanly in methanol to furnish the Fe(II) clathrochelate. An organic/inorganic hybrid membranes composed of Fe(II) clathrochelate and polyethersulfone was prepared by using phase inversion method. For membrane preparation, the Fe(II) clathrochelate was highly soluble (3~5 g/L) in DMF, NMP, and DMAc, which meets the requirements for the solubility of metal complexes in polar aprotic solvent used in membrane preparation. It was stable even in the presence of strong acids, such as trifluorosactic acid (pKa = 0.3). It was characterized by UV-vis spectroscopy, and their stability in solution phase studied in the presence of (i) strong acids or (ii) competing chelates. Organic/inorganic hybrid membranes were prepared with polyethersulfone, polyvinylpyrrolidone, p-toluenesulfonic acid, Fe(II) clathrochelate and DMF by using nonsolvent induced phase inversion method. The addition of Fe(II) clathrochelate leads increase of surface pore density, mean pore size and flux. We can obtain highly asymmetric membranes by addition of Fe(II) clathrochelate.

Study on Morphology Control of Polymeric Membrane with Clathrochelate Metal Complex (Clathrochelate계 금속 착물을 이용한 고분자 멤브레인 구조 제어)

  • Kim, Nowon;Jung, Boram
    • Membrane Journal
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    • v.24 no.6
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    • pp.472-483
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    • 2014
  • This study is preparation of microporous membranes by using macrocyclic metal ion complexes and extended cage complexes. It is a more favorable way to existing methods because polymer and metal ion-ligand complex system provides a fine control over the phase transition behavior. Chemical functionalization of the polar surface can be obtained. Metal-templated condensation of cyclohexanedione dioxime, hydroxyphenylboronic acid in the presence of metal salts proceeds cleanly in methanol to furnish the metal clathrochelate complexes. Organic/inorganic hybrid membranes were prepared with polyethersulfone (PES), polyvinylpyrrolidone (PVP), ethyleneglycol butyl ether (BE), metal clathrochelate s and DMF by using nonsolvent induced phase inversion method. The structure of membranes was characterized with scanning electron microscopy (SEM) and microflow permporometer. The addition of Fe(II) clathrochelate complex with p-hydroxyphenyl group leads to changes of membrane morphology such as narrow mean pore size distribution, increase of surface pore density and decrease of the largest pore size.