• Title/Summary/Keyword: Gravimetric analysis method

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Mass Balance Method for Purity Assessment of Organic Reference Materials: for Thermolabile Materials with LC-UV Method

  • Lee, Joonhee;Kim, Byungjoo
    • Bulletin of the Korean Chemical Society
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    • v.35 no.11
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    • pp.3275-3279
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    • 2014
  • A mass balance method for purity assessment of thermolabile organic reference materials was established by combining several techniques, including liquid chromatography with UV/VIS detector (LC-UV), Karl-Fischer (K-F) Coulometry, and thermal gravimetric analysis (TGA). This method was applied to three fluoroquinolones like enrofloxacin, norfloxacin and ciprofloxacin. LC-UV was used to analyze structurally related organic impurities based on UV/VIS absorbance spectra obtained in combination with LC separation. For all three organic reference materials, the UV/VIS spectra of the separated impurities were similar to that of the major component of the corresponding materials. This indicates that the impurities are structurally related to the respective reference material sharing common chromophores. Impurities could be quantified by comparing their absorbances at the wavelength of maximum absorbance (${\lambda}_{max}$). The water contents of the reference materials were measured by K-F Coulometry by an oven-drying method. The total inorganic impurities contents were assayed from ash residues in TGA analysis with using air as a reagent gas. The final purities estimated from results of those analytical techniques were assigned as ($99.91{\pm}0.06$), ($97.09{\pm}0.17$) and ($91.85{\pm}0.17$)% (kg/kg) for enrofloxacin, norfloxacin and ciprofloxacin, respectively. The assigned final purities would be applied to the reference materials which will be used as calibrators for the certification of those compounds in matrix CRMs as starting points for the traceability of their certified values to SI units.

Crystal Structures and Thermal Properties of Two Binuclear Cd(II) Supramolecular Complexes Based on Quinolinecarboxylate Ligand

  • Hao, Hu-Jun;Yin, Xian-Hong;Lin, Cui-Wu;Wei, Shui-Qiang
    • Bulletin of the Korean Chemical Society
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    • v.32 no.9
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    • pp.3255-3260
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    • 2011
  • Two novel binuclear metal-organic coordination complexes $[Cd_2(L)_2(bpy)_2(H_2O)_2]{\cdot}6H_2O$ (1), $[Cd_2(L)_2(phen)_2-(H_2O)_2]{\cdot}2H_2O$ (2) (where L = 2-methylquinoline-3,4-dicarboxylate dianion, bpy = 2,2'-bipyridine, phen = 1,10-phenanthroline) have been synthesized under hydrothermal conditions and characterized by single crystal Xray diffraction, spectral method (IR), elemental analysis and thermal gravimetric analysis (TGA). Both 1 and 2 consist of two Cd(II) atoms bridged by two monoatomic bridging carboxylate groups from two L ligands, and the second carboxylate group of each L is monodentately coordinated to Cd(II), creating a sevenmembered chelating ring. The coordination at each metal nucleus is completed by a water molecule and a chelating bidentate molecule. The 3D structures of the complexes are stabilized by ${\pi}-{\pi}$ stacking interactions and hydrogen-bonds.

Solid Phase Extraction of Celecoxib from Drug Matrix and Biological Fluids by Grafted Poly β-cyclodextrine/allyl Amine Magnetic Nano-particles

  • Kamari, Sahar;Panahi, Homayon Ahmad;Baimani, Nasim;Moniri, Elham
    • Korean Chemical Engineering Research
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    • v.55 no.3
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    • pp.287-295
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    • 2017
  • Using nanotechnology, magnetic nanoparticles of iron oxide were produced via co-precipitation method and followed modification with organic compounds. In the next step, functionalized monomer was provided via coupling ${\beta}$-cyclodextrine and allylamine onto modified magnetic nanoparticles. These nanoparticles were used to establish the adsorption rate of celecoxib. Magnetic nanoparticles are modified by (3-mercaptopropyl)trimethoxysilane. Nano-adsorbent was characterized by analytical and spectroscopic methods, such as Fourier transform infrared spectroscopy, elemental analysis, thermo-gravimetric analysis, and transmission electron microscopy (TEM). Laboratory parameters, such as the kinetics of adsorption isotherms, pH, reaction temperature and capacity were optimized. Finally, by using this nano-adsorbent in the optimized condition, extraction of celecoxib from biological samples as urine, drug matrix and blood plasma was carried out by high performance liquid chromatography with sensitivity and high accuracy.

Synthesis, Characterization and in vitro Antibacterial Studies on Mixed Ligand Complexes of Iron(III) Based on 1,10-phenanthroline

  • Tigineh, Getinet Tamiru;Sitotaw, Getu;Workie, Amogne;Abebe, Atakilt
    • Journal of the Korean Chemical Society
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    • v.65 no.3
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    • pp.203-208
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    • 2021
  • As part of our attempt to discover novel active compounds against multi-drug resistant pathogens, we hereby report two new complexes of iron(III) with formulae: [Fe(L1)2(H2O)2]Cl3 and [Fe(L1)2(L2)(H2O)]Cl2 where L1 = 1,10-phenanthroline (C12H8N2) and L2 = guanide (C5H4N5O-). The synthesized complexes were characterized using spectroscopic analysis (ESI-MS, ICP-OES, FT-IR, and UV-Vis), cyclic voltammetry, CHN analysis, gravimetric chloride determination, melting point determination, and conductance measurement. Octahedral geometries are assigned to both complexes. In vitro antibacterial activity was tested on two Gram-positive (Staphylococcus aureus, Streptococcus epidermidis) and two Gram-negative (Escherichia coli and Klebsiella pneumoniae) bacteria using the disc diffusion method. The complexes demonstrated appreciable activity against these pathogens. Interestingly, the [Fe(L1)2(L2)(H2O)]Cl2 complex manifested a higher degree of inhibition against the drug-resistant Gram-negative bacteria than the commercially available drug, namely erythromycin.

Studies on X-Ray Fluorescence Analysis of Sulfide Ores by Solution Technique (I). Analysis of Sulfur (용액법을 이용한 황화광석의 X-선 형광분석에 관한 연구 (제1보). 황의 분석)

  • Young-Sang Kim;Kee-Chae Park
    • Journal of the Korean Chemical Society
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    • v.26 no.4
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    • pp.229-234
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    • 1982
  • Using solution technique, sulfur in the sulfide ore was indirectly determined by X-ray fluorescence spectrometry. The sample was dissolved with the mixed solution of B$r_2$ and HN$O_3$, and Si$O_2$, a major constituent, was repelled from the solution by HF treatment several times, B$a^{2+}$ solution was added to the solution to precipitate the S$O^4_{2-}$ ion as BaS$O_4$. Measuring the fluorescent X-ray intensity of excess Ba2+ ion in the filtrate, the content of sulfur in the original ore was back-calculated. Comparing the results by this method with the gravimetric method, the mean difference was ${\pm}1.7%$ in the range of 20 to 40% of sulfur content and the method was tolerably reproducible.

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Analysis of Dietary Fiber Content of Some Vegetables, Mushrooms, Fruits and Seaweeds (채소류, 버섯류, 과일류 및 해조류 식품의 식이섬유 함량)

  • 황선희
    • Journal of Nutrition and Health
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    • v.29 no.1
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    • pp.89-96
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    • 1996
  • This study was conducted to analyze dietary fiber content of 113 common Korean foods. Content of total dietary fiber(TDF) in vegetables, mushrooms, fruite, and seaweeds was determined by enzymatic-gravimetric method developed by Prosky et al. and adopted by AOAC. The average TDF content of the foods analyzed was 3.62$\pm$2.09% for green vegetables, 5.90$\pm$7.61% for light vegetables, 14.27$\pm$18.11% for mushrooms, 3.02$\pm$4.48% for fruits, and 11.39$\pm$12.68% for seaweeds. The foods containing the highest TDF values in the food groups were boiled radish leaves(10.84%) in green vegetables, dried braken(38.36%) in light vegetables, dried juda's ear(18.18%) in mushrooms except dried manna lichen(52.87%), dried persimon(17.73%) in fruits and dried sea mustard(37.77%) in seaweeds. Dried Seaweeds such as sea mustard (37.77%), sea tangle(29.30%), and laver(31.36%) were good sources of dietary fiber. When we consider the health and therapeutic benefits of dietary fiber, it is recommended to continue to consume traditional Korean diet which are mainly composed of vegetables rather than animal foods and to increase consumption of dried mushrooms and seaweeds which contain high content of TDF.

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Investigation on nanoadhesive bonding of plasma modified titanium for aerospace application

  • Ahmed, Sabbir;Chakrabarty, Debabrata;Mukherjee, Subroto;Joseph, Alphonsa;Jhala, Ghanshyam;Bhowmik, Shantanu
    • Advances in aircraft and spacecraft science
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    • v.1 no.1
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    • pp.1-14
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    • 2014
  • Physico-chemical changes of the plasma modified titanium alloy [Ti-6Al-4V] surface were studied with respect to their crystallographic changes by X-Ray Diffraction (XRD) and Scanning Electron Microscope (SEM).The plasma-treatment of surface was carried out to enhance adhesion of high performance nano reinforced epoxy adhesive, a phenomenon that was manifested in subsequent experimental results. The enhancement of adhesion as a consequence of improved spreading and wetting on metal surface was studied by contact angle (sessile drop method) and surface energy determination, which shows a distinct increase in polar component of surface energy. The synergism in bond strength was established by analyzing the lap-shear strength of titanium laminate. The extent of enhancement in thermal stability of the dispersed nanosilica particles reinforced epoxy adhesive was studied by Thermo Gravimetric Analysis (TGA), which shows an increase in onset of degradation and high amount of residuals at the high temperature range under study. The fractured surfaces of the joint were examined by Scanning electron microscope (SEM).

Synthesis and Characterization of Reduced Graphene Oxide/Gelatin Composite Films (환원된 산화그래핀/젤라틴 복합필름의 합성과 분석)

  • Chen, Guangxin;Qiao, Congde;Xu, Jing;Yao, Jinshui
    • Polymer(Korea)
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    • v.38 no.4
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    • pp.484-490
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    • 2014
  • Reduced graphene oxide (RGO) was fabricated using gelatin as a reductant, and it could be stably dispersed in gelatin solution without aggregation. A series of RGO/gelatin composite films with various RGO contents were prepared by a solution-casting method. The structure and thermal properties of the RGO/gelatin composite films were characterized by UV-vis spectroscopy, Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), differential scanning calorimeter (DSC) and thermal gravimetric analysis (TGA). The addition of RGO enhances the degree of crosslinking of gelatin films and decreases the swelling ability of the gelatin films in water, indicating that RGO/gelatin composite films have a better wet stability than gelatin films. The glass transition temperature ($T_g$) of gelatin films is also increased with the incorporation of RGO. The presence of RGO slightly increases the degradation temperature of gelatin films due to the very low content of RGO in the composite films. Since gelatin is a natural and nontoxic biomacromolecule, the RGO/gelatin composite films are expected to have potential applications in the biomedical field.

Synergistic Effects of Mo-V Based Mixed Oxide Catalysts for Acrolein Oxidation(I) (아크로레인 산화용 Mo-V 계 혼합산화물 촉매의 상승효과(I))

  • Na, Suk-Eun;Kim, Kyung-Hoon;Chung, Jong-Shik;Park, Dae-Won
    • Applied Chemistry for Engineering
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    • v.3 no.4
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    • pp.717-721
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    • 1992
  • Mechanical mixtures of vanadium molybdate and copper molybdate catalysts prepared by coprecipitation method, and those of $MoO_3$ and $V_2O_5$ were used to study the synergistic effects between each metal oxide for the selective oxidation of acrolein. The catalytic activity results revealed that the conversion of acrolein and yield of acrylic acid were increased with the mixture catalysts and it could be explained by a remote control mechanism. Thermal gravimetric analysis confirmed the evolution of lattice oxygen in the mixture catalysts.

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Synthesis of transparent conductive film containing solution -deposited poly (3, 4-ethylenedioxythiophene) (PEDOT) and water soluble multi-walled carbon nanotubes

  • Tung, Tran Thanh;Kim, Won-Jung;Kim, Tae-Young;Lee, Bong-Seok;Suh, Kwang-S.
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2008.06a
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    • pp.205-206
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    • 2008
  • The transparent conductive film was prepared by bar coating method of poly (3, 4-ethylenedioxythiophene) (PEDOT) and poly (sodium 4-stylenesulfonate) grafted multi-walled carbon nanotubes (MWNT-PSS) nanocomposites solution on the polyethylene terephthalate (PET) film. In this case, multi-wall carbon nanotubes was treated by chemical methods to obtain water soluble MWNT-PSS and then blending with PEDOT. The non-covalent bonding of polymer to the MWNT surface was confirmed by Fourier transform infrared (FT-IR), thermal gravimetric analysis (TGA) and Transmission electro microscope (TEM) investigation also showed a polymer-wrapped MWNT structure. Furthermore, the electrical, transmission properties of the transparent conductive film were investigated and compared with control samples are raw PEDOT films.

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