• Title/Summary/Keyword: XRD and FT-IR

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Chemical Characteristics of Timbers from the Yeongheungdo Shipwreck (영흥도선의 화학적 특성)

  • Cha, Mi Young
    • Journal of Conservation Science
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    • v.33 no.1
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    • pp.35-42
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    • 2017
  • The Yeongheungdo shipwreck was excavated in the sea of Seomeopbeol, Ongjin-gun, Incheon, Korea. Chemical characterization of timbers from the shipwreck occurred via maximum moisture content, chemical composition, FT-IR, solid state $^{13}C$ NMR, and XRD analyses. As maximum moisture content of the outer part of the timbers averaged 623%, a phenomenon in that lignin increased relatively, according to the decrease in cellulose, and the ash content increased, which is typical of waterlogged archaeological wood was shown. The results from the FT-IR and solid state $^{13}C$ NMR analyses showed that the cellulose band of the outer part had disappeared or had remarkably decreased. In addition, the bands assigned to lignin dramatically increased. However, regarding the inner part of the timbers, hemicellulose and some crystalline cellulose and amorphous cellulose bands decreased. Therefore, a large difference exists between the degradation levels of the outer and inner parts of the timbers of the Yeongheungdo shipwreck.

Removal of Cu(II) with the Recycled Hydroxylapatite from Animal Bones (동물뼈로부터 재활용된 hydroxylapatite를 이용한 Cu(II) 제거)

  • Kim, Mu-Nui;Kim, Won-Gee;Lee, Seung-Mok;Yang, Jae-Kyu
    • Journal of Korean Society of Environmental Engineers
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    • v.31 no.9
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    • pp.735-742
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    • 2009
  • The bone of spinal animals has a hydroxylapatite ($Ca_{10}(PO_4)_6(OH)_2$, HAp) structure which is well known as an excellent inorganic ion exchanger for various heavy metal ions in solutions. In this study, the reusability of cow-bone, pig-bone and fish-bone as a potential material for the removal of heavy metals in solutions was evaluated from the removal of Cu(II) ion in batch tests. The surface properties of three bones, calcined at different temperatures, were measured with SEM, XRD, FT-IR analyses. From the SEM analysis, a clear development of heterogeneity as well as pores having small diameter was observed as the calcination temperature increased. The results of X-ray diffraction analysis showed well developed crystallinity on the surface of calcined bones obtained at higher temperatures, suggesting a transform of amorphous type to crystalline type. Fourier transform infrared (FT-IR) analysis showed disappearance of water molecule on the surface of HAp and organic functional groups of the HAp with increasing the calcination temperatures. Cu(II) removal in the control test was below 15%. By the way, additional 40% increase of Cu(II) removal was observed in the presence of calcined bones. For three bones, Cu(II) removal was decreased as the calcined temperature increased. Cu(II) removal was increased as the solution pH increased due to a favorable condition for the cation exchange as well as precipitation.

Characteristics of soybean urease induced CaCO3 precipitation

  • Zhu, Liping;Lang, Chaopeng;Li, Bingyan;Wen, Kejun;Li, Mingdong
    • Geomechanics and Engineering
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    • v.31 no.3
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    • pp.281-289
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    • 2022
  • Bio-CaCO3 is a blowout environment-friendly materials for soil improvement and sealing of rock fissures. To evaluate the chemical characteristics, shape, size and productivity of soybean urease induced CaCO3 precipitates (SUICP), experimental studies were conducted via EDS, XRD, FT-IR, TGA, BET, and SEM. Also, the conversion rate of SUICP reaction at different time were determined and analyzed. The Bio-CaCO3 product obtained by SUICP is comprehensively judged as calcite based on the results of EDS, XRD and FT-IR. The SUICP calcite precipitates are detected as spherical or ellipsoidal particles 3-6 ㎛ in diameter with nanoscale pores on their surface, and this morphology is novel. The median secondary particle size d50 is 39-88 ㎛, indicating the agglomeration of the primary calcite particles. The Bio-calcite decomposes at 650-780℃, representing a medium thermal stability. The conversion rate of SUICP reaction can reach 80% in 24h, which is much more efficient than microbially induced CaCO3 precipitation. These results reveal the knowledges of SUICP, and further direct its engineering applications. Moreover, we show an economic channel to obtain porous spherical calcite.

Bifunctional Fe-SBA-15-SO3H Mesoporous Catalysts with Different Si/Fe Molar Ratios: Synthesis, Characterization and Catalytic Activity

  • Erdem, Sezer;Erdem, Beyhan;Oksuzoglu, Ramis Mustafa;Citak, Alime
    • Bulletin of the Korean Chemical Society
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    • v.34 no.5
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    • pp.1481-1486
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    • 2013
  • Bifunctional Fe-SBA-15-$SO_3H$ mesoporous materials with different Si/Fe molar ratios (3, 5, and 7) have been synthesized via a simple direct hydrothermal method and characterized by XRD, $N_2$-adsorption/desorption, TG/DTG and FT-IR techniques, and used as solid acid catalysts in the esterification of lactic acid with methanol. XRD and $N_2$ sorption characterizations show successful iron doping within the mesoporous channels of SBA-15-$SO_3H$. The FT-IR and TG/DTG characterizations also reveal the presence of iron. With the incorporation of Fe ions into the SBA-15-$SO_3H$, the acid sites substantially increased because of the self-separated acidity of the hydrolysis of $Fe^{3+}$ solutions. However, in the Si/Fe = 3 molar ratio, the catalytic conversion decreased which is caused by the reduced cooperation effect between the acid pairs due to the weakened hydrogen bonds and collapse of the pore structure. This further suggests that the mesoporous structure decreases with the decrease in Si/Fe ratio.

Electrochemical Non-Enzymatic Glucose Sensor based on Hexagonal Boron Nitride with Metal-Organic Framework Composite

  • Ranganethan, Suresh;Lee, Sang-Mae;Lee, Jaewon;Chang, Seung-Cheol
    • Journal of Sensor Science and Technology
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    • v.26 no.6
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    • pp.379-385
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    • 2017
  • In this study, an amperometric non-enzymatic glucose sensor was developed on the surface of a glassy carbon electrode by simply drop-casting the synthesized homogeneous suspension of hexagonal boron nitride (h-BN) nanosheets with a copper metal-organic framework (Cu-MOF) composite. Comprehensive analytical methods, including field-emission scanning electron microscopy (FE-SEM), Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), cyclic voltammetry, electrochemical impedance spectroscopy, and amperometry, were used to investigate the surface and electrochemical characteristics of the h-BN-Cu-MOF composite. The FE-SEM, FT-IR, and XRD results showed that the h-BN-Cu-MOF composite was formed successfully and exhibited a good porous structure. The electrochemical results showed a sensor sensitivity of $18.1{\mu}A{\mu}M^{-1}cm^{-2}$ with a dynamic linearity range of $10-900{\mu}M$ glucose and a detection limit of $5.5{\mu}M$ glucose with a rapid turnaround time (less than 2 min). Additionally, the developed sensor exhibited satisfactory anti-interference ability against dopamine, ascorbic acid, uric acid, urea, and nitrate, and thus, can be applied to the design and development of non-enzymatic glucose sensors.

Synthesis of potassium titanate by wet process (습식법에 의한 티탄산칼륨 섬유의 합성)

  • 강대갑;송종택
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.5 no.3
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    • pp.278-283
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    • 1995
  • The potassium titanate fibres were synthesized with wet process by the addition of KOH solution to the TiOz gel produced by the reaction between element titanium particles and $H_2O_2$ solution at $50^{\circ}C$. And then they were characterized by XRD, SEM and FT - IR. It was found that potassium titanate fibres were mainly affected by KOH/TiOz mole ratio, synthesis time and aging time in this wet process employed. For $KOH/TiO_2 = 1/1$, synthesizing time 24 hrs, aging time 24 hrs and calcination temperature of TEX>$900^{\circ}C$ for 1 hr, their products were mainly found to be potassium tetratitanate which had thin and long fibres in the range of 10 ~ 20 mm. As the synthesizing time increased and the amount of KOH decreased, potassium tetratitanate was converted into potassium hexatitanate. Also, the length of their fibres became short.

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Synthesis and Properties of Liquid Crystalline Copolymers with Ether-ether-ester Linkage in Main Chain (주사슬에 ether-ether-ester 결합을 갖는 액정공중합체의 합성 및 성질)

  • Bang, Moon-Soo
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.11 no.4
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    • pp.1367-1372
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    • 2010
  • Copoly(ether-ether-ester)s having flexible side chain were synthesized by polycondensation. Intrinsic viscosities of polymers were between 0.42 and 0.78dl/g in tetrachloroethane. The polymer structures were investigated by $^1H$-NMR and FT-IR, and thermal and liquid crystalline properties of polymers were measured by DSC, TGA, POM and XRD. As results of investigations, synthetic copolymers exhibited lower melting temperature than homopolymers. When the biphenylene units contents in copolymer were more than 60 mol %, nematic mesophase was observed, and the mesophase of synthetic polymers was dependent upon biphenylene content.

Synthesis of Organic Silicon Compounds from Siliceous Mudstone (규질이암으로부터 실리콘 유기화합물 합성)

  • Kim, Byoung-Gyu;Jang, Hee-Dong;Kim, Jong-Seok
    • Journal of the Mineralogical Society of Korea
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    • v.20 no.3
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    • pp.155-163
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    • 2007
  • A novel route to the synthesis of tetramethoxysilane and other silicon alkoxides is described using siliceous mudstone as the raw material. The reaction of amorphous silica with triethanol-amine is enhanced by using an alkali metal hydroxide catalyst to form a range of triethanol-amnine-substituted silatrane species. These can undergo alkoxide exchange in acidic alcohols to form alkoxysilatranes, tetraalkoxysilanes, hexaalkoxydisiloxanes and higher siloxanes. Products were identified by FT-IR spectroscopy, XRD, SEM, 1H and 13C NMR spectroscopy, or gas chromatography.

Solid State $^{27}Al$, $^{29}Si$ MAS NMR Spectroscopic Studies on Crystallization of ZSM-5 Synthesized at Low Temperature and Atomospheric Pressure (저온상압에서 합성된 Na,TPA-ZSM-5의 결정화에 관한 Solid State $^{27}Al$$^{29}Si$ MAS NMR 분광학적 고찰)

  • Yun, Young Ja;Ha, Jae Mok
    • Journal of the Korean Chemical Society
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    • v.40 no.10
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    • pp.656-662
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    • 1996
  • Using low temperature and atmospheric pressure method, we synthesized Na, TPA-ZSM-5 with Si/Al ratio of about 100. We employed 27Al and 29Si MAS NMR spectroscopy and FT-IR to investigate the crystallization process as a function of time. The chemical shift depends on the initial composition of reactants and changes during the course of synthesis different from those reported by others earlier. However, the chemical shift of our final product showed in the range of typical ZSM-5. And the defect site was removed by the calcine. From XRD and SEM data, the formation of ZSM-5 was also confirmed.

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Oxidative Dehydrogenation of n-Butane over Cr Catalysts Supported on Alumina and SBA-15 (Cr이 담지 된 알루미나, SBA-15 촉매에서 n-부탄의 산화적 탈수소화 반응)

  • Shin, Jin Hyun;Shin, Jin Ho;Cho, Deug Hee;Ko, Moon Kyu
    • Korean Chemical Engineering Research
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    • v.51 no.3
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    • pp.364-369
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    • 2013
  • Oxidative dehydrogenation of n-butane over mesoporous Cr catalysts were studied. Catalysts were prepared by Cr impregnated method over Ti or Zr dispersed mesoporous support such as SBA-15, ${\gamma}$-alumina and characterized by XRD, SEM, TEM, FT-IR UV-Vis and ICP-AES. The effect of high surface area was not noticed appreciably in terms of conversion, but for Cr catalysts with Ti and Zr-incorporated on SBA-15 and ${\gamma}$-alumina. showed high selectivity of trans-2-butene.