• Title/Summary/Keyword: elemental analysis

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Formation of Cadmium(II) Nitrate Complexes with Macrocycles

  • Ho-Doo Kim;Hak-Jin Jung;Oh-Jin Jung
    • Bulletin of the Korean Chemical Society
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    • v.14 no.5
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    • pp.561-567
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    • 1993
  • The twelve macrocycle (L) complexes of cadmium(II) nitrate have been synthesized: $CdL(NO_3)_2$. All the complexes have been indentified by elemental analysis, electric conductivity measurements, IR and NMR spectroscopic techniques. The molar electric conductivities of the complexes in water and acetonitrile solvent were in the range of 236.8-296.1 $cm^2{\cdot}mol^{-1}{\cdot}ohm^{-1}$ at 25$^{\circ}$C. The characteristic peaks of macrocycles affected from Cd(II) were shifted to lower frequencies as compared with uncomplexed macrocycles. A complex with 1,4,8,11-tetrakis(methylacetato)-1,4,8,11-tetraaza cyclodecane (L4) exhibited two characteristic bands such as strong stretching (1646 $cm^{-1})$, and weaker symmetric stretching band (1384 $cm^{-1})$. NMR studies indicated that all nitrogen donor atoms of macrocycles have greater affinity to cadmium(II) metal ion than do the oxygen atoms. The $^{13}$C-resonance lines of methylene groups neighboring the donor atom such as N and S were shifted to a direction of high magnetic field and the order of chemical shifts were $L_1 < L_2 < L_3 < L_6 < L_4$. Also the chemical shifts values were larger than those of methylene groups bridgeheaded in side-armed groups. This result seems due to not only the strong interaction of Cd(Ⅱ) with nitrogen donors according to the HSAB theory, but weak interaction of Cd(Ⅱ) and COO- ions or sulfur which is enhanced by the flexible methylene spacing group in side-armed groups. Thus, each additional gem-methyl pairs of L_3, L_4\;and\; L_6$ macrocycles relative to $L_1, L_2,\;and\;L_5$ leads to an large enhancement in Cd(II) affinity. ^{13}C$-NMR spectrum of the complex with $L_{12}$ (1,5,9,13-tetracyclothiacyclohexadecane-3,11-diol) reveals the presence of two sets of three resonance lines, and intensities of the each resonance line have the ratio of 1 : 2 : 2. This molecular conformation is predicted as structure of tetragonal complex to be formed by coordinating two sulfur atoms and the other two sulfur atoms which is affected by OH-groups.

Characterization of Core/Shell PMMA/CdS Nanoparticles Synthesized by Surfactant-free Emulsion Polymerization (무유화 유화중합에 의해 합성된 Core/shell 형태 PMMA/CdS 나노입자의 특성분석)

  • Yoon, Hyojung;Rhym, Young-Mok;Shim, Sang Eun
    • Journal of Adhesion and Interface
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    • v.13 no.4
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    • pp.188-192
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    • 2012
  • Herein, CdS-coated PMMA nanoparticles were prepared by in-situ surfactant-free emulsion copolymerization and subsequent CdS coating process. As-prepared CdS/PMMA hybrid particles had 201.7 nm in diameter. The amount of CdS nanocrystals in the hybrid particles was 10.37 wt% determined by TGA and elemental analysis. The size of CdS crystals was 3.55 nm preferentially grown in (111) plane. UV-vis spectrum of PMMA/CdS nanoparticles showed the significant blue-shift in optical illumination. The reason was found because the synthesized CdS nanocrystals on PMMA particles had a different band gap energy of 2.70 eV which was significantly higher than that of known-value of bulk CdS (2.41 eV) due to a quantum confinement effect.

Expression and Purification of Transmembrane Protein MerE from Mercury-Resistant Bacillus cereus

  • Amin, Aatif;Sarwar, Arslan;Saleem, Mushtaq A.;Latif, Zakia;Opella, Stanley J.
    • Journal of Microbiology and Biotechnology
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    • v.29 no.2
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    • pp.274-282
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    • 2019
  • Mercury-resistant ($Hg^R$) bacteria were isolated from heavy metal polluted wastewater and soil collected near to tanneries of district Kasur, Pakistan. Bacterial isolates AZ-1, AZ-2 and AZ-3 showed resistance up to $40{\mu}g/ml$ against mercuric chloride ($HgCl_2$). 16S rDNA ribotyping and phylogenetic analysis were performed for the characterization of selected isolates as Bacillus sp. AZ-1 (KT270477), Bacillus cereus AZ-2 (KT270478) and Bacillus cereus AZ-3 (KT270479). Phylogenetic relationship on the basis of merA nucleotide sequence confirmed 51-100% homology with the corresponding region of the merA gene of already reported mercury-resistant Gram-positive bacteria. The merE gene involved in the transportation of elemental mercury ($Hg^0$) via cell membrane was cloned for the first time into pHLV vector and transformed in overexpressed C43(DE3) E. coli cells. The recombinant plasmid (pHLMerE) was expressed and the native MerE protein was obtained after thrombin cleavage by size exclusion chromatography (SEC). The purification of fusion/recombinant and native protein MerE by Ni-NTA column, dialysis and fast protein liquid chromatography (FPLC/SEC) involved unfolding/refolding techniques. A small-scale reservoir of wastewater containing $30{\mu}g/ml$ of $HgCl_2$ was designed to check the detoxification ability of selected strains. It resulted in 83% detoxification of mercury by B. cereus AZ-2 and B. cereus AZ-3, and 76% detoxification by Bacillus sp. AZ-1 respectively (p < 0.05).

Surface Modification of Nano Silica Prepared by Sol-gel Process and Subsequent Application towards Gas-barrier Films (졸-겔 공정으로 제조한 나노 실리카의 표면개질 및 가스차단성 필름으로의 응용)

  • Jang, Hyo Jun;Chang, Mi Jung;Nam, Kwang Hyun;Chung, Dae-won
    • Applied Chemistry for Engineering
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    • v.30 no.1
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    • pp.68-73
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    • 2019
  • We prepared hydrophobic silica particles by a sol-gel process from tetraethyl orthosilicate (TEOS), followed by coupling the reaction with octyltrimethoxysilane (OTMS) or hexadecyltrimethoxysilane (HDTMS) under various reaction conditions. We confirmed the extent of silica surface modification with organic compounds by SEM-EDS, thermogravimetry and elemental analysis. The silica particles obtained after the hydrolysis reaction of TEOS in ethanol at $50^{\circ}C$ for 24 h and the coupling reaction with OTMS for 2 h at the same temperature displayed the optimum performance in terms of the dispersity in an organic solvent and the surface roughness of films composited with epoxy resins. The oxygen permeability of the composite film with modified-silica was 12% lower than that of using the film without modified-silica.

An organofunctionalized MgO∙SiO2 hybrid support and its performance in the immobilization of lipase from Candida rugosa

  • Kolodziejczak-Radzimska, Agnieszka;Zdarta, Jakub;Ciesielczyk, Filip;Jesionowski, Teofil
    • Korean Journal of Chemical Engineering
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    • v.35 no.11
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    • pp.2220-2231
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    • 2018
  • Lipase from Candida rugosa was immobilized on $MgO{\cdot}SiO_2$ hybrid grafted with amine, thiol, cyano, phenyl, epoxy and carbonyl groups. The products were analyzed using Fourier transform infrared spectroscopy, nuclear magnetic resonance, low-temperature $N_2$ sorption and elemental analysis. Additionally, the degree of coverage of the oxide material surface with different functional groups and the number of surface functional groups were estimated. The Bradford method was used to determine the quantity of immobilized enzyme. The largest quantity of enzyme (25-28 mg/g) was immobilized on the hybrid functionalized with amine and carbonyl groups. On the basis of hydrolysis reaction of p-nitrophenyl palmitate to p-nitrophenol, it was determined how the catalytic activity of the obtained biocatalysts is affected by pH, temperature, storage time, and repeated reaction cycles. The best results for catalytic activity were obtained for the lipase immobilized on $MgO{\cdot}SiO_2$ hybrids with amine and carbonyl groups. The biocatalytic system demonstrated activity above 40% in the pH range 4-10 and in the temperature range $30-70^{\circ}C$. Lipase immobilized on the $MgO{\cdot}SiO_2$ systems with amine and epoxy groups retains, respectively, around 80% and 60% of its initial activity after 30 days of storage, and approximately 60-70% after 10 reaction cycles.

A Study on Growth of Intermetallic Compounds Layer of Photovoltaic Module Interconnected by Multi-wires under Damp-heat Conditions (고온고습시험에 의한 멀티 와이어 PV 모듈의 금속 간 화합물 층의 성장에 관한 연구)

  • Moon, Ji Yeon;Cho, Seong Hyeon;Son, Hyoung Jin;Jun, Da Yeong;Kim, Sung Hyun
    • Current Photovoltaic Research
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    • v.8 no.4
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    • pp.124-128
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    • 2020
  • Output power of photovoltaic (PV) modules installed outdoors decreases every year due to environmental conditions such as temperature, humidity, and ultraviolet irradiations. In order to promote the installation of PV modules, the reliability must be guaranteed. One of the important factors affecting reliability is intermetallic compounds (IMC) layer formed in ribbon solder joint. For this reason, various studies on soldering properties between the ribbon and cell have been performed to solve the reliability deterioration caused by excessive growth of the IMC layer. However, the IMC layer of the PV module interconnected by multi-wires has been studied less than using the ribbon. It is necessary to study soldering characteristics of the multi-wire module for improvement of its reliability. In this study, we analyzed the growth of IMC layer of the PV module with multi-wire and the degradation of output power through damp-heat test. The fabricated modules were exposed to damp-heat conditions (85 ºC and 85 % relative humidity) for 1000 hours and the output powers of the modules before and after the damp-heat test were measured. Then, the process of dissolving ethylene vinyl acetate (EVA) as an encapsulant of the modules was performed to observe the IMC layer. The growth of IMC layer was evaluated using OM and FE-SEM for cross-sectional analysis and EDS for elemental mapping. Based on these results, we investigated the correlation between the IMC layer and output power of modules.

Engineering characteristics of dune sand-fine marble waste mixtures

  • Qureshi, Mohsin U.;Mahmood, Zafar;Farooq, Qazi U.;Qureshi, Qadir B.I.L.;Al-Handasi, Hajar;Chang, Ilhan
    • Geomechanics and Engineering
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    • v.28 no.6
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    • pp.547-557
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    • 2022
  • Dune sands are poorly graded collapsible soils lacking fines. This experimental study explored the technical feasibility of sustainable invigoration of fine waste materials to improve the geotechnical properties of dune sand. The fine waste considered in this study is fine marble waste. The fine waste powder was mixed with dune sand at different contents (5, 10,15, 20, 25, 50%), where the gradation, void ratio, compaction, and shear strength characteristics were assessed for each fine marble waste -dune sand blend. The geotechnical properties of the dune sand-fine marble waste mix delineated in this study reveal the enhancement in compaction and gradation characteristics of dune sand. According to the results, the binary mixture of dune sand with 20% of fine marble waste gives the highest maximum dry density and results in shear strength improvement. In addition, a numerical study is conducted for the practical application of the binary mix in the field and tested for an isolated shallow foundation. The elemental analysis of the fine marble waste confirms that the material is non-contaminated and can be employed for engineering applications. Furthermore, the numerical study elucidated that the shallow surface replacement of the site with the dune sand mixed with 20% fine marble waste gives optimal performance in terms of stress generation and settlement behavior of an isolated footing. For a sustainable mechanical performance of the fine marble waste mixed sand, an optimum dose of 20% fine marble waste is recommended, and some correlations are proposed. Thus, for improving dune sand's geotechnical characteristics, the addition of fine marble waste to the dune sand is an environment-friendly solution.

Investigation on Microstructure and Flowability of Gas Atomized Heat-resistant KHR45A Alloy Powders for Additive Manufacturing

  • Geonwoo Baek;Mohsen Saboktakin Rizi;Yeeun Lee;SungJae Jo;Joo-Hyun Choi;Soon-Jik Hong
    • Journal of Powder Materials
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    • v.30 no.1
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    • pp.13-21
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    • 2023
  • In additive manufacturing, the flowability of feedstock particles determines the quality of the parts that are affected by different parameters, including the chemistry and morphology of the powders and particle size distribution. In this study, the microstructures and flowabilities of gas-atomized heat-resistant alloys for additive manufacturing applications are investigated. A KHR45A alloy powder with a composition of Fe-30Cr-40Mn-1.8Nb (wt.%) is fabricated using gas atomization process. The microstructure and effect of powder chemistry and morphology on the flow behavior are investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and revolution powder analysis. The results reveal the formation of spherical particles composed of single-phase FCC dendritic structures after gas atomization. SEM observations show variations in the microstructures of the powder particles with different size distributions. Elemental distribution maps, line scans, and high-resolution XPS results indicate the presence of a Si-rich oxide accompanied by Fe, Cr, and Nb metal oxides in the outer layer of the powders. The flowability behavior is found to be induced by the particle size distribution, which can be attributed to the interparticle interactions and friction of particles with different sizes.

Effect of irrigants on the color stability, solubility, and surface characteristics of calcium-silicate based cements

  • Selen Kucukkaya Eren;Sevinc Askerbeyli Ors;Hacer Aksel;Senay Canay ;Duygu Karasan
    • Restorative Dentistry and Endodontics
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    • v.47 no.1
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    • pp.10.1-10.11
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    • 2022
  • Objectives: This study aimed to investigate the color stability, solubility, and surface characteristics of 3 calcium silicate-based cements (CSCs) after immersion in different solutions. Materials and Methods: ProRoot white mineral trioxide aggregate (MTA), Biodentine, and Endosequence Root Repair Material (ERRM) were placed in cylindrical molds and stored at 37℃ for 24 hours. Each specimen was immersed in distilled water, 5% sodium hypochlorite (NaOCl), 2% chlorhexidine, or 0.1% octenidine hydrochloride (OCT) for 24 hours. Color changes were measured with a spectrophotometer. Solubility was determined using an analytical balance with 10-5 g accuracy. The surface characteristics were analyzed using scanning electron microscopy and energy-dispersive spectroscopy. Data were analyzed using 2-way analysis of variance, the Tukey test, and the paired t-test. Results: MTA exhibited significant discoloration in contact with NaOCl (p < 0.05). White precipitation occurred on the surfaces of Biodentine and ERRM after contact with the solutions, and none of the materials presented dark brown discoloration. All materials showed significant solubility after immersion in the solutions (p < 0.05), irrespective of the solution type (p > 0.05). The surface topography and elemental composition of the samples showed different patterns of crystal formation and precipitation depending on the solution type. Conclusions: All materials presented some amount of solubility and showed crystal precipitation after contact with the solutions. Biodentine and ERRM are suitable alternatives to ProRoot MTA as they do not exhibit discoloration. The use of OCT can be considered safe for CSCs.

Adsorption of heavy metal ions onto a surface treated with granular activated carbon and activated carbon fibers (표면 처리에 따른 입상활성탄 및 활성탄소섬유의 중금속 흡착)

  • Kang, Kwang Cheol;Kwon, Soo Han;Kim, Seung Soo;Choi, Jong Won;Chun, Kwan Sik
    • Analytical Science and Technology
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    • v.19 no.4
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    • pp.285-289
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    • 2006
  • In this study, the effect of an acidic treatment on granular activated carbon (GAC) and activated carbon fibers (ACF) was investigated for a $Pb^{2+}$ and $Ni^{2+}$ ion adsorption. 1.0 M nitric acid solution was used as the acid solution for the surface treatment. Surface properties of the GAC and ACF were characterized by the pH, elemental analysis and pHpzc (pH of the point of zero charge). Their specific surface area and the pore structure were also evaluated by the nitrogen adsorption data at 77K. As a result, the acidic treatment led to an increase of the oxygen-containing functional groups. Furthermore, the adsorption capacity of the acid-treated GAC and ACF was improved in the order of acidic-ACF > untreated-ACF > acidic-GAC > untreated-GAC, though the decrease in specific surface area induced by a pore blocking of the functional groups was observed.