• Title/Summary/Keyword: elemental analysis

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Coordination of an Amino Alcohol Schiff Base Ligand Toward Cd(II)

  • Mardani, Zahra;Hakimi, Mohammad;Moeini, Keyvan;Mohr, Fabian
    • Journal of the Korean Chemical Society
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    • v.63 no.1
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    • pp.29-36
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    • 2019
  • A potentially tetradentate Schiff base ligand, 2-((2-((pyridin-2-ylmethylene)amino)ethyl)amino)ethan-1-ol (PMAE), and its cadmium(II) complex, [$Cd(PMAE)I_2$] (1), were prepared and characterized by elemental analysis, FT-IR, Raman, $^1H$ and $^{13}C$ NMR spectroscopies and single-crystal X-ray diffraction. In the crystal structure of 1, the cadmium atom has a slightly distorted square-pyramidal geometry and a $CdN_3I_2$ environment in which the PMAE acts as an $N_3$-donor. In the crystal packing of the complex, the alcohol and amine groups of the coordinated ligands participate in hydrogen bonding with iodide ions and form $R^2{_2}(14)$ and $R^2{_2}(8)$ hydrogen bond motifs, respectively. In addition to the hydrogen bonds, the crystal network is stabilized by ${\pi}-{\pi}$ stacking interactions between pyridine rings. The thermodynamic stability of the isolated ligand and its cadmium complex along with their charge distribution patterns were studied by DFT and NBO analysis.

Synthesis and Electrochemical Studies of Ni(Ⅱ) Complexes with Tetradentate Schiff Base Ligands

  • 정병구;임채평;국성근;조기형;최용국
    • Bulletin of the Korean Chemical Society
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    • v.17 no.2
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    • pp.173-179
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    • 1996
  • A series of tetradentate Schiff base ligands; [1,2-bis(naphthylideneimino)ethane, 1,3-bis(naphthylideneimino)propane, 1,4-bis(naphthylideneimino)butane, and 1,5-bis(naphthylideneimino)pentane] and their Ni(Ⅱ) complexes have been synthesized. The properties of these ligands and their Ni(Ⅱ) complexes have been characterized by elemental analysis, IR, NMR, UV-vis spectra, molar conductance, and thermogravimetric analysis. The mole ratio of Schiff base to Ni(Ⅱ) metal was found to be 1:1. The electrochemical redox process of the ligands and their Ni(Ⅱ) complexes in DMF and DMSO solution containing 0.1 M tetraethyl ammonium perchlorate (TEAP) as a supporting electrolyte have been investigated by cyclic voltammetry, chronoamperometry, differential pulse voltammetry, and controlled potential coulometry at glassy carbon electrode. The redox process of the ligands was highly irreversible, whereas redox process of Ni(Ⅱ) complexes were observed as one electron transfer process in quasi-reversible and diffusion-controlled reaction. The electrochemical redox potentials of the Ni(Ⅱ) complexes were affected by the chelate ring size of ligands. The diffusion coefficients of Ni(Ⅱ) complexes containing 0.1 M TEAP in DMSO solution were determined to be 5.7-6.9 × 10-6 cm2/sec. Also the exchange rate constants were determined to be 1.8-9.5 × 10-2 cm2/sec. These values were affected by the chelate ring size of ligands.

Antimicrobial and Water Repellency Effect of Functional PET Fibers with ODDMAC(octadecyldimethyl(3-triethoxy silylpropyl) ammonium chloride) (ODDMAC를 이용한 항균성 및 발수성 동시 발현이 가능한 기능성 PET 섬유)

  • Yang, Heejin;Jeon, Hyeji;Lee, Sang Oh;Lee, Jaewoong
    • Textile Coloration and Finishing
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    • v.32 no.4
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    • pp.265-273
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    • 2020
  • In this study, octadecyldimethyl(3-triethoxy silylpropyl)ammonium chloride (ODDMAC) incorporated with Polyethylene terephthalate (PET) fabrics with different environmental conditions such as various temperature and time intervals. First, ODDMAC (15 weight %) was dissolved in ethanol. Then PET fabrics immersed in the ODDMAC solution at 25 ℃ for 10 minutes and dried at 80 ℃ for 5 minutes. The dried PET/PDDMAC fabrics carried out for curing process out at 110 ℃ ~ 190 ℃. The treated PET/ODDMAC has examined the surface and side coating properties through SEM analysis and elemental analysis. PET/ODDMAC fabric washed with water up to 50 times and studied the durability of the materials. It was confirmed that the treated PET fabric also exhibited good water repellency. In addition, the antimicrobial activity against the gram-positive bacteria Staphylococcus aureus and gram-negative bacteria Escherichia coli were studied by the disc diffusion method on the treated fabric.

Estimation of Alkali Overdosing in a Lime Neutralization Process for Acid Mine Drainage

  • Cheong, Young-Wook;Cho, Dong-Wan;Lee, Jin-Soo;Hur, Won
    • Applied Chemistry for Engineering
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    • v.33 no.1
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    • pp.109-112
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    • 2022
  • Lime has been used for the neutralization of acidic waste because it is cheap and available in large quantities. The resulting sludge often contains a considerable amount of unreacted lime due to alkali overdosing, even during automatic neutralization processes, which mainly arises from the poor solubility of lime. The sludge cake from lime neutralization of Ilkwang Mine also contained high percentages of calcium and magnesium. The elemental content of the sludge cake was compared with those obtained from a simulation of the lime neutralization facility installed at Ilkwang Mine. A Goldsim® model estimated the degree of lime overdosing to be 19.1% based on the fractions of ferrous oxide. The analysis suggests that resolubilization of aluminum hydroxide could occur in the settling basin, in which pH exceeded 10 due to the continued dissolution of the overdosed lime. The present study demonstrated that chemical analysis of sludge combined with process simulation could provide a reasonable estimate of mass balance and chemistry in a neutralization facility for acid mine drainage.

Synthesis, spectral, thermal, structural study and theoretical treatment of new complexes of mannich base with Ni(II) and study of cytotoxicity effect on (Hepa-2) cell line and antimicrobial activity

  • Omar H. Al-Obaidi
    • Analytical Science and Technology
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    • v.36 no.2
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    • pp.70-79
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    • 2023
  • The synthesis of the Mannich base as a ligand (L) N-(morpholino (phenyl) methyl) acetamide is the subject of this study. Elemental analyses, FT-IR spectra, UV-vis, 1H-NMR, and magnetic measurements were used to confirm the synthesis of the [Ni(L)2]Cl2 complex, thermal analysis (TG/DTG), atomic absorption, and scanning, and structurally explained as electron microscopy (SEM), and X-ray powder diffraction (XRD) methods. The melting point of the complex and its molar conductivity were also measured. The suggested geometries of the complexes formed have a tetrahedral structure, according to the data acquired using various techniques. Theoretical approaches to the complex formation have been investigated. For molecular mechanics and semi-empirical calculations, the HYPERCHEM6 program had been used. The effect of the novel Ni(II) complex on the cancer cell Hepa-2 (human hepatocellular ademocarcinoma), that is the human laryngeal cancer, was studied. It has been found that these ligand and complex have potent effects on the cancer cell. The antibacterial activity of the free ligand and its complex was evaluated against two kinds of human pathogenic bacteria. The first category is Gram-positive (Staphylococcus aureas, epiderimids), whereas the second group is Gram-negative (Psedamonas aeruginosa, Escherichia coli) (from the diffusion method). Finally, it was discovered that various chemicals had varied growth-inhibiting effects on bacteria.

Cationized Lignin Loaded Alginate Beads for Efficient Cr(VI) Removal

  • Jungkyu KIM;YunJin KIM;Seungoh JUNG;Heecheol YUN;Hwanmyeong YEO;In-Gyu CHOI;Hyo Won KWAK
    • Journal of the Korean Wood Science and Technology
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    • v.51 no.5
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    • pp.321-333
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    • 2023
  • In this study, lignin, a lignocellulosic biomass, was chemically modified to produce polyethyleneimine-grafted lignin (PKL) with maximum hexavalent chromium [Cr(VI)] adsorption capacity. Changes in the physicochemical properties due to the cationization of lignin were confirmed through elemental analysis, Fourier transform infrared spectroscopy, and moisture stability evaluation. Alginate (Alg) beads containing PKL (Alg/PKL) were prepared by incorporating cationic lignin into the Alg matrix to apply the prepared PKL in a batch-type water treatment process. The optimal Alg/lignin mixing ratio was selected to increase the Cr(VI) adsorption capacity and minimize lignin elution from the aqueous system. The selected Alg/PKL beads exhibited an excellent Cr(VI) removal capacity of 478.98 mg/g. Isothermal adsorption and thermodynamic analysis revealed that the Cr(VI) removal behavior of the Alg/PKL beads was similar to that of heterogeneous chemical adsorption. In addition, the bulk adsorbent material in the form of beads exhibited adsorption behavior in three stages: surface adsorption, diffusion, and equilibrium.

Preparation and Characterization of Fe-Ni Nanocatalyst for AEM Electrolysis via Spontaneous Reduction Reaction in Dry Process (건식 공정에서 자발적 환원 반응에 의한 AEM 수전해용 Fe-Ni 나노 촉매 제조 및 특성)

  • JAEYOUNG LEE;HONGKI LEE
    • Journal of Hydrogen and New Energy
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    • v.35 no.2
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    • pp.185-194
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    • 2024
  • Fe-Ni nanocatalysts loaded on carbon black were prepared via spontaneous reduction reaction of iron (II) acetylacetonate and nickel (II) acetylacetonate in dry process. Their morphology and elemental analysis were characterized by scanning electron microscopy, transmission electron microscopy (TEM), and energy dispersive X-ray analyzer. The loading weight of the nanocatalysts was measured by thermogravimetric analyze and the surface area was measured by BET analysis. TEM observation showed that Fe and Ni nanoparticles was well dispersed on the carbon black and their average particle size was 4.82 nm. The loading weight of Fe-Ni nanocatalysts on the carbon black was 6.83-7.32 wt%, and the value increased with increasing iron (II) acetylacetonate content. As the Fe-Ni loading weight increased, the specific surface area decreased significantly by more than 50%, because Fe-Ni nanoparticles block the micropores of carbon black. I-V characteristics showed that water electrolysis performance increased with increasing Ni nanocatalyst content.

A comparative study of 3D printing and sol-gel polymer production techniques: A case study on usage of ABS polymer for radiation shielding

  • Hasan Ogul;Batuhan Gultekin;Fatih Bulut;Hakan Us
    • Nuclear Engineering and Technology
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    • v.56 no.6
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    • pp.1943-1949
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    • 2024
  • This study focuses on the comparative analysis of ABS polymer samples produced using two distinct manufacturing techniques: 3D printing and the sol-gel methods. In the first approach, ABS polymer was augmented with rare earth oxides, Er2O3 and Gd2O3, in nano powder form and fabricated into test specimens using 3D printing technology. In the second approach, identical samples were prepared via the sol-gel technique involving mold-based fabrication. Elemental content analysis revealed no significant differences between the samples produced by the two methods. The study proceeds to evaluate the gamma-ray shielding, neutron shielding, temperature resistance, and SEM/EDS pictures of ABS samples generated through both techniques. 3D printing method exhibited more favorable results in terms of structure morphology and thermal stability while there is no significant difference for radiation shielding. The results provide insights into the performance and suitability of each production method for radiation shielding applications. This research not only contributes to enhancing radiation shielding technology but also informs the selection of the most appropriate fabrication method for specific applications in nuclear technologies and diagnostic energy range in medical purposes.

Synthesis, characterization, and biological significance of mixed ligand Schiff base and alizarin dye-metal complexes

  • Laith Jumaah Al-Gburi;Taghreed H. Al-Noor
    • Analytical Science and Technology
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    • v.37 no.4
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    • pp.239-250
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    • 2024
  • This study reports the synthesis of a bi-dentate Schiff base ligand (L), 7-(2-((2-formylbenzylidene) amino)-2-phenylacetamido)-3-methyl-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid, prepared from phthalaldehyde and cephalexin antibiotic. The synthesized Schiff base ligand (L) and the secondary ligand alizarin (Az) are used to prepare the new complexes [M(Az)2(L)] and [Cr(Az)2(L)]Cl, where M = Mn(II), Co(II), Ni(II), Cu(II), and Zn(II). The mode of bonding of the Schiff base has been characterized by UV-Visible, FT-IR, Mass, 1H-, and 13C-NMR spectroscopic techniques, and micro elemental analysis (CHNS). The complexes were characterized using UV-Vis, FT-IR, molar conductance, magnetic moment, and thermal analysis (TG/DTG). The molar conductance data revealed that the complexes are non-electrolytes except for [Cr(L)(Az)2]Cl, which is an electrolytic type 1:1. The Schiff base and its complexes have been tested for their biological activity against two strains of bacteria and one fungus. When screened against gram-positive and gram-negative pathogens, the Az and L ligands and their complexes showed potential antimicrobial activity.

Studies on the Michael Addition Reaction between Secondary Amino Groups on the Silica Surface with Poly(ethylene glycol) Diacrylates (실리카 나노입자 표면에 결합된 2차 아미노기와 Poly(ethylene glycol) Diacrylate의 마이클 부가반응에 대한 연구)

  • Jeon, Ha Na;Ha, KiRyong
    • Polymer(Korea)
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    • v.36 no.6
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    • pp.822-830
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    • 2012
  • We used dipodal type bis[3-(trimethoxysilyl)propyl]amine (BTMA) silane coupling agent to modify silica nanoparticles to introduce secondary amino groups on the silica surface. These N-H groups were reacted with three different molecular weights (M.W. = 258, 575, and 700) of poly(ethylene glycol) diacrylates to introduce different attached layer thicknesses on the silica surface by Michael addition reaction. After Michael addition reaction, we used several analytical techniques such as fourier transform infrared spectroscopy (FTIR), elemental analysis (EA) and solid state $^{13}C$ cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy to characterize introduced structures. We found almost complete Michael addition reaction of both two acrylate groups of PDGDA with N-H groups of BTMA modified silica to form ${\beta}$-amino acid esters. Between equimolar ratio of pure BTMA and pure PEGDA reaction, only one acrylate group of two acrylate groups of PEGDA reacted with N-H groups of pure BTMA to form ${\beta}$-amino acid ester and the other remaining acrylate group can be used to form a polymer later.