• Title/Summary/Keyword: Electron diffraction data

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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.

Effectiveness of Ni-based and Fe-based cladding alloys in delaying hydrogen generation for small modular reactors with increased accident tolerance

  • Alan Matias Avelar;Fabio de Camargo;Vanessa Sanches Pereira da Silva;Claudia Giovedi;Alfredo Abe;Marcelo Breda Mourao
    • Nuclear Engineering and Technology
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    • v.55 no.1
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    • pp.156-168
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    • 2023
  • This study investigates the high temperature oxidation behaviour of a Ni-20Cr-1.2Si (wt.%) alloy in steam from 1200 ℃ to 1350 ℃ by Thermogravimetric Analysis (TGA), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDS) and X-ray Diffraction (XRD). The results demonstrate that exposed Ni-based alloy developed a thin oxide scale, consisted mainly of Cr2O3. The oxidation kinetics obtained from the experimental results was applied to evaluate the hydrogen generation considering a simplified reactor core model with different cladding alloys following an unmitigated Loss-Of-Coolant Accident (LOCA) scenario in a hypothetical Small Modular Reactor (SMR). Overall, experimental data and simulations results show that both Fe-based and Ni-based alloys may enhance cladding survivability, delaying its melting, as well as reducing hydrogen generation under accident conditions compared to Zr-based alloys. However, a substantial neutron absorption occurs when Ni-based alloys are used as cladding for current uranium-dioxide fuel systems, even when compared to Fe-based alloys.

The Analysis of Structure and Electron Energy State of Potassium-Graphite Fiber Intercalation Compounds (칼륨-흑연 섬유층간화합물의 구조와 전자 에너지 상태의 분석)

  • Oh, Won-Chun;Kim, Myung-Kun;Ko, Young-Shin
    • Analytical Science and Technology
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    • v.6 no.5
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    • pp.479-487
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    • 1993
  • Potassium-Graphite Fiber Intercalation Compounds(K-GFIC) have been prepared from well oriented pitch-based Graphite fiber by the transformed two-bulbs method with variation of reaction temperatures of graphite($T_g$ : $450^{\circ}C$, $400^{\circ}C$, $350^{\circ}C$, $300^{\circ}C$, $250^{\circ}C$). The stage transition process of K-GFICs was studied by X-ray diffraction methods, and we have observed peaks with d-values of (001) diffraction of $5.40{\AA}$ and $8.78({\pm}0.01){\AA}$, which are charecteristic for the stage 1 and stage 2, respectively. The stage stability and energy states of K-GFICs were studied by UV/VIS spectrophotometer. As a results, We found that the minimum values of reflactance of K-GFICs with pure stage was moved to higher energy pristine Graphite fiber's. But because of mixtured stage, we could not observe minimum reflectance in the visible region at high reaction temperatures($400^{\circ}C$, $450^{\circ}C$). From X-ray diffraction and UV/VIS sepctrophotometry data, we can suggest that K-GFICs with lower stage has many charge carriers existed between C atoms of graphite Layers. And then, these results also provides information on the electrical and other physical properties of K-GFICs.

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Crystallographical Characteristics of Solar Salts Produced from Jeonnam Area by X-Ray Diffraction Technique (X선 회절법에 의한 전남지역 천일염의 결정학적 특성)

  • Jeong, Byung-Jo;Kim, Yong;Kim, Chang-Dae;Hyun, Seung-Cheol;Ham, Gyung-Sik
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.38 no.9
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    • pp.1284-1288
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    • 2009
  • Identification of various inorganic compound crystals contained in solar salts, which are produced from 12 areas of Jeonnam, was firstly made by the X-ray diffraction (XRD) technique. The analysis of the XRD spectra was carried out on the basis of Joint Committee on Powder Diffraction Standards (JCPDS) data and the results of Energy Dispersive X-ray Spectrometer (EDX) measurements. In particular, the analysis of the XRD spectra supported that each solar salt contains $Na_2S$ (Shinan Jeungdo and Sinui), $KMgCl_3$ (Shinan Bigeum), $Ca(ClO_3)_2$ (Shinan Docho), $CaAl_4O_7$ (Haenam Songji), $CaSiO_3$ and $CaCl_2$ (Goheung) as inorganic compound crystals, which have not been reported for the solar salts. Also, the XRD results indicated that the solar salts maintain a cubic NaCl crystal structure without any change of lattice parameters etc. However, it was shown in the Field Emission Scanning Electron Microscope (FE-SEM) images that an external form of the solar salts has a lamination layer shape of a cubic structure, which is different from a simple cubic form for the purified salts and the reagent NaCl.

A Study on Geology of Clay Mineral Deposits of Pohang-Ulsan Area and their Physico-Chemical Properties (포항-울산간의 점토자원의 지질과 그 물리화학적 특성에 관한 연구)

  • Kim, Ok Joon;Lee, Ha Young;Kim, Suh Woon;Kim, Soo Jin
    • Economic and Environmental Geology
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    • v.4 no.4
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    • pp.167-215
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    • 1971
  • I. Purpose and Importance of the Study The purpose of the present study is to clarify to geological, mineralogical, and physico-chemical properties of the clay minerals deposits imbedded in the Tertiary sediments in the areas between. Pohang and Ulsan along southeastern coastal region of Korea. These clays are being mined and utilized for filter and insecticide after activation or simple pulverizing, nontheless activated clays are short coming as chemical industry in Korea has been rapidly grown in recent years. In spite of such increase in clay demand, no goological investigation on clay deposits nor physico-chemical properties of the clays have been carried out up to date. Consequently activated clays produced in Korea is not only of low grade but also of shortage in supply, so that Korea has to import activated clays of better grade. The importance of the present study lies, therefore, on that guiding principle could be laid down by knowing stratigraphical horizons, of clay deposits and fundamental data of improving grade of activated clays might be derived from the results of physico-chemical examinations. II. Contents and Scope of the study The contents of the study are pinpointed down in the following two subjects: 1) General geological investigation of Tertiary formations distributed in the areas between Pohang and UIsan, and detail geological study of the bentonitic clay deposits imbedded in them. 2) To clarifty physico-chemical characteristics of the clays by means of chemical analysis, X-ray diffraction and electron microscope. The scope of the study involves the following there points: i) Regional geological investigation-This investigation has been carried out in order to find out the distribution of Tertiary sediments and exact location of clay mineral deposits in the areas between Pohang and UIsan. ii) Detail geological investigation-This has been concentrated in and around the clay deposits which. had been found out by the regional investigation. iii) Laboratory researchs include i) age determination and correlation of Tertiary sediments by paleontological study, and ii) Chemical analysis, X-ray diffraction, and electron microscopic studies on clays, samples taken from various clay deposits. III. Research Results and Suggestions 1) The geology of the area investigated is composed mainly of Janggi and Beomgokri groups of Miocene age in ascending order rested on the upper Silla system, Balkuksa granite and volcanic rocks of upper Cretaceous age as base. 2) Janggi group is composed in ascending order of Janggi conglomerate, Nultaeri rhyolitic tuff, Keumkwangdong shale, two beds of lignite-bearing formations which consist of alternation of conglomerate, sandstone and mudstone, and andesitic, rhyolitic, and basaltic tuff beds. 3) Beomgokri group is mainly composed of andesitic to rhyolitic tuff interlayered by conglomerate and tuffaceous sandstone. In the areas around boundary between North-and South Kyeongsang-do is distributed Haseori farmation which is composed of conglomerate, sandstone, mudstone and andesitic to rhyolitic tuff, and which is correlated to Eoilri formation of Janggi group. 4) Clay deposits of the area are interbedded in Eoilri, Haseori, Nultaeri tuff, Keumkwangdong shale, upper and lower horizon of the lower lignite-bearing seam, and Keumori rhyolitic tuff formations of Janggi group; and are genetically classi.fied into four categories, that is, i) those derived from volcanic ash beds(Haseori and Daeanri deposits), ii) those of secondary residual type from rhyolitic tuff beds(Seokupri deposits), iii) Clay beds above and beneath the lignite seams, (Janggi and Keumkwangdong deposits), and iv) those derived from rhyolitic tuff beds(Sangjeong and Tonghae deposits). 5) Mineral constituents of clay deposits are, according to X-ray diffraction, montmorillonite accompanied in different degree by cristobalite, plagioclase, quartz, stilbite, and halloysite in rare occasion. The clays are grouped according to mineral composition into four types; i) those consist mostly of montmorillonite, ii) those composed of montmorillonite and cristobalite, iii) those composed of montmorillonite and plagioclase, and iv) those composed of montmorillonite, plagioclase and quartz. 6) Clays interbedded in Haseori formation and vicinity of lignite seams belong to the first type, are of good quality and derived either from volcanic ash bed, or primary clay beds near lignite seams. Clays belonged to other types are derived from weathering of rhyolitic tuff formations and their quality varies depending upon original composition and degree of weathering. Few clays in secondary residual type contain small amount of halloysite. 7) Judging from analytical data, content of silica($SiO_2$) varies proportionally with content of cristobalite, and alumina($Al_2O_3$) content does not vary with that of plagioclase, but increases in the sedimentary bedded type of deposits. 8) It is unknown whether or not these days could be upgraded by beneficiation since no grain size of these impurities nor beneficiation test had been studied. 9) Clay beds derived from valcanic ash layers or sedimentary layers at the vicinity of lignite seams are thin in thickness and of small, discontinueous lenticular shape, although they are of good quality; and those derived from rhyolitic tuff formations or residual type from tuff are irregular in both occurrence and quality. It is, therefore, not only very difficult but also meaningless to calculate its reserve, and reserve estimation, even if done, will greatly be deviated from practically minable one. Consequently, way of discovery and exploitation of clay deposits in the area under consideration is to check the geologically favorable areas whenever needed.

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Intergrowth and Interlayering of Muscovite, Chlorite, and Biotite in a Garnet Zone Metamorphic Rock of the Ogcheon Belt, South Korea (옥천대의 석류석데 변성암에서 산출되는 백운모, 녹니석 및 흑운모의 Intergrowth와 Interlayering)

  • Yeong Boo Lee;Jung Hoo Lee;Chang Whan Oh
    • Journal of the Mineralogical Society of Korea
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    • v.15 no.2
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    • pp.122-131
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    • 2002
  • Muscovite, chlorite and biotite in metapelites of the Ogcheon Hetamorphic Belt are studied using electron probe microanalysis (EPMA), backscattered electron images (BEI) of scanning electron microscopy (SEM) and lattice fringe images of transmission electron microscopy (TEM). These minerals are observed to be intergrown under a polarized light microscope and are apparently interlayered below EPMA resolution; EPMA data often indicate mixtures of phyllosilicates such as muscovite/chlorite (M/C), biotite/chlorite (B/C), muscovite/pyrophyllite/chlorite (M/P/C). biotite/pyrophyllite/chlorite (B/P/C) or biotite/muscovite/chlorite (B/M/C). BEI observations show that the three minerals (muscovite, chlorite and biotite) are mixed at various scales in a grain through the garnet zone, and the interlayering of the three minerals are observed from TEM lattice fringe images and selected area electron diffraction patterns. The result of TEM observations reveals that 7-$\AA$ layers (serpentine, precursor of chlorite) are interlayered within 10-$\AA$ layers (muscovite) at 100~200 $\AA$ scale as well as M/C in the chlorite zone. The 7-$\AA$ layers become smaller in size and less frequent in the biotite tone, and 10-$\AA$ layers are interlayered with chlorite (14 $\AA$) at an individual layer scale. The 7-$\AA$ layers are no longer observed in the garnet zone, and 10-$\AA$ layers (biotite) are interlayered with chlorite (B/C) at 50~100 $\AA$ scale. Relatively large scale (1000~2000 $\AA$) of intergrowth is also frequently observed from the garnet zone samples. However, rocks from all three metamorphic zones show interlayering of a few units of 7-, 10- and 14-$\AA$ layers with each other at TEM observations. The result of this study implies that metamorphic minerals such as muscovite, chlorite and biotite form through disequilibrum mineral reactions resulting in inhomogenious phases.

Preparation and Dissolution of Polyvinylpyrrolidone(PVP)-Based Solid Dispersion Systems Containing Solubilizers (가용화 조성물을 함유한 PVP형 고체분산체의 제조 및 특성)

  • Cao, Qing-Ri;Kim, Tae-Wan;Choi, Choon-Young;Kwon, Kyoung-Ae;Lee, Beom-Jin
    • Journal of Pharmaceutical Investigation
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    • v.33 no.1
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    • pp.7-14
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    • 2003
  • The PVP-based solid dispersion systems (SDs) containing lovastatin (LOS) and solubilizers (sodium lauryl sulfate, tween 80 and oleic acid) were prepared to enhance dissolution rate of practically water insoluble LOS using solvent evaporation method. Two different organic cosolvents either acetone/ethanol or acetonitrile/ethanol were used for the preparation of SDs. The LOS contents were highly decreased when acetone/ethanol cosolvents were used. The decrease of LOS contents was not caused by acetonitrile or acetone, based on HPLC data. The surface morphology as investigated by scanning electron microscope (SEM) and angle of repose as an index of flowability of SDs were highly dependent on the type and amount of solubilizers used. Based on differential scanning calorimetry (DSC) and X-ray powder diffraction data, the SDs made crystalline LOS into amorphous structure or partially eutectic mixtures. The simultaneous use of the solubilizers in SDs was also useful to increase dissolution rate of LOS in gastric or intestinal fluid. The SDs containing solubilizers reached 76% and 60% in gastric and intestinal fluid, respectively but the commercial tablet gave only less than 4%. These solubilizers in SDs could be also applicable for enhancing dissolution and bioavailability of poorly water-soluble drugs.

Study on thermal behavior of Ammonium Hexafluofide Titanate for Synthesis of TiO2 Powders (TiO2 분말 합성을 위한 Ammonium Hexafluofide Titanate의 열적 거동 연구)

  • Lee, Duk-Hee;Park, Jae-Ryang;Lee, Chan-Gi;Park, Kyung-Soo;Kim, Hyeon-Mo
    • Journal of Powder Materials
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    • v.23 no.5
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    • pp.353-357
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    • 2016
  • In this study, $TiO_2$ powders are synthesized from ammonium hexafluoride titanate (AHFT, $(NH_4)_2TiF_6$) as a precursor by heat treatment. First, we evaluate the physical properties of AHFT using X-ray diffraction (XRD), particle size analysis (PSA), thermogravimetric analysis (TGA), and field-emission scanning electron microscopy (FE-SEM). Then, to prepare the $TiO_2$ powders, is heat-treated at $300-1300^{\circ}C$ for 1 h. The ratio of anatase to rutile phase in $TiO_2$ is estimated by XRD. The anatase phase forms at $500^{\circ}C$ and phase transformation to the rutile phase occurs at $1200^{\circ}C$. Increase in the particle size is observed upon increasing the reaction temperature, and the phase ratio of the rutile phase is determined from a comparison with the calculated XRD data. Thus, we show that anatase and rutile $TiO_2$ powders could be synthesized using AHFT as a raw material, and the obtained data are utilized for developing a new process for producing high-quality $TiO_2$ powder.

Surface Transition by Solvent Washing Effects and Biological Properties of Metal Treated Activated Carbons

  • Oh, Won-Chun
    • Bulletin of the Korean Chemical Society
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    • v.25 no.5
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    • pp.639-646
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    • 2004
  • Metal treated activated carbons are prepared using various metals. Adsorption behaviors, morphologies, as well as antibacterial effects of metal treated samples are compared before and after solvent washing. Adsorption isotherms are used to characterize the porous structure of metal treated activated carbons before and after the solvent washing with acetone or ethyl alcohol. From these data, it is noticed that the changes in physicochemical properties of metal treated activated carbons depend on the solvents employed. Similar results are observed from BET data obtained from nitrogen adsorption isotherms. From scanning electron microscopy (SEM) studies, the changes in shape and size of metal particles are observed after the samples are washed with solvents. These changes result in different blocking effects, which, in turn, affect the adsorption behavior of metal treated activated carbons. X-ray diffraction (XRD) patterns of the samples treated with different metals are different each other. High intense sharp peaks attributed to metals are observed from silver treated samples, while the peaks are not observed from copper treated samples. To compare thermodynamic behavior of metal treated activated carbons washed with different type of solvents, differential scanning calorimetric (DSC) analysis is carried out. The analysis shows similar endothermic curves for all of the samples. Finally, antibacterial effects of metal treated activated carbon against Escherichia coli are discussed. Comparing the effects among the metals employed, highest effects are obtained from Cd, while lowest effects are obtained from Cu. Antibacterial activity becomes higher with the increase of the amount of metals treated, Optimum concentrations of metals to treat activated carbons, obtained from a shake flask test, are known to be 0.4, 0.1, and 0.6 moles for Ag, Cd, and Cu, respectively.

Growth and Characterization of Conducting ZnO Thin Films by Atomic Layer Deposition

  • Min, Yo-Sep;An, Cheng-Jin;Kim, Seong-Keun;Song, Jae-Won;Hwang, Cheol-Seong
    • Bulletin of the Korean Chemical Society
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    • v.31 no.9
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    • pp.2503-2508
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    • 2010
  • ZnO thin films were grown on Si or $SiO_2$/Si substrates, at growth temperatures ranging from 150 to $400^{\circ}C$, by atomic layer deposition (ALD) using diethylzinc and water. Despite the large band gap of 3.3 eV, the ALD ZnO films show high n-type conductivity, i.e. low resistivity in the order of $10^{-3}\;{\Omega}cm$. In order to understand the high conductivity of ALD ZnO films, the films were characterized with X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy, elastic recoil detection, Rutherford backscattering, Photoluminescence, and Raman spectroscopy. In addition, the various analytical data of the ZnO films were compared with those of ZnO single crystal. According to our analytical data, metallic zinc plays an important role for the high conductivity in ALD ZnO films. Therefore when the metallic zinc was additionally oxidized with ozone by a modified ALD sequence, the resistivity of ZnO films could be adjusted in a range of $3.8{\times}10^{-3}\;{\sim}\;19.0\;{\Omega}cm$ depending on the exposure time of ozone.