• Title/Summary/Keyword: FT-NMR

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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.

Preparation and Characterization of BaTiO3 Powders and Thin films (티탄산바륨 분말과 박막의 제조 및 특성 연구)

  • Jung, Miewon;Son, Hyunjin;Lee, Jiyun;Kim, Hyunjung
    • Analytical Science and Technology
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    • v.17 no.2
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    • pp.173-179
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    • 2004
  • The $BaTiO_3$ powders and thin films were prepared by an alkoxide modified sol-gel process (polymerization-complex route) using ethylene glycol. The stable starting (Ba-Ti)-mixed metal organic sol was made by addition of acetylacetone. The $BaTiO_3$ powders, which had a particle size of 40~77 nm, were crystallized from an amorphous to a tetragonal phase on annealing at 700 and $1100^{\circ}C$ for 1 h. From FT-IR, solid-state $^{13}C$ CP/MAS NMR spectroscopy and X-ray diffractometry, the trace of the Ba-Ti-oxycarbonate phase first appeared at $400^{\circ}C$. Hydrolyzed sol was spin coated on a quartz wafer at 3500 rpm for 60 s and pyrolyzed at $1100^{\circ}C$ for 1 h. After heat treatment, the coated layer became dense and smooth.

A Study on the Synthesis ann Pyrolytic Properties of SiC/Ti Hybrid Ceramic Precursor by Hydrolysis (가수분해에 의한 탄화규소/티타늄 혼성 세라믹 전구체 합성과 열분해 특성에 관한 연구)

  • 황택성;이존태;우희권
    • Polymer(Korea)
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    • v.24 no.3
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    • pp.299-305
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    • 2000
  • In order to increase the thermal stability at high temperatures, new hybrid ceramic percursors were synthesized by chemical modification of polycarbosilane (PCS). The structure of hybrid ceramic percursors were investigated by using FT-IR and $^1$H-NMR spectrometers. The syntheses of hybrid ceramic precursors were confirmed by monitoring the change of the adsorption peaks appearing at 0893, 1092, 609 $cm^{-1}$ / on the FT-IR spectra, and also by the presence of peaks at 3.8, 2.0, 0.6 ppm on the $^1$H-NMR spectra. The conversion of hybrid ceramic percursor was around 74 and 10 wt% higher than that of the pure PCS. After the heat-treatment at 150$0^{\circ}C$, the crystalline peaks for $\beta$-SiC were observed at 2$\theta$=35.7, 42.2, 61.0$^{\circ}$ on the X-ray powder diffractogram. It showed the conversion of hybrid ceramic percursor to crystalline $\beta$-SiC.

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Effects of Reaction pH and Hardener Type on Reactivity, Properties, and Performance of Urea-Formaldehyde (UF) Resin

  • Park, Byung-Dae;Kim, Yoon Soo;So, Won Tek;Lim, Kie Pyo
    • Journal of the Korean Wood Science and Technology
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    • v.30 no.3
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    • pp.1-11
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    • 2002
  • This study was conducted to investigate the effects of reaction pH conditions and hardener types on the reactivity, chemical structure and adhesion performance of UF resins. Three different reaction pH conditions, such as traditional alkaline-acid (7.5 → 4.5), weak acid (4.5), and strong acid (1.0), were used to synthesize UF resins which were cured by adding three different hardeners (ammonium chloride, ammonium citrate, and zinc nitrate) to measure adhesion strength. Fourier transform infrared (FT-IR) and carbon-13 nuclear magnetic resonance (13C-NMR) spectroscopies were employed to study chemical structure of the resin prepared under three different reaction pH conditions. Adhesion strength of the resins cured with three different hardeners was determined with lap shear specimens in tension. The gel time of UF resins decreased with an increasing in the amount of both ammonium chloride and ammonium citrate added in the resins. However, the gel time increased for zinc nitrate. Both FT-IR and 13C-NMR spectroscopies showed that the strong reaction pH condition produce uronic structures in UF resin, while both alkaline-acid and weak acid conditions produce quite similar chemical species in the resins. The maximum adhesion strength was occurred with the resin prepared under strong acid pH condition. However, this study indicated that the weak acid reaction condition provide a balance between increasing resin reactivity and improving adhesion strength of UF resin. The measurement of formaldehyde emission from the panels bonded with the UF resins prepared is planned for future work.

Characterization of Layered Double Hydroxides(Mg-Al-$CO_3$ systems) and Rehydration Reaction of Their Calcined Products in Aqueous Chromate Solution (층상이중수산화물(Mg-Al-$CO_3$ 체계)의 물리 · 화학적 특성규명 및 소성된 시료의 크롬산이온 수용액에서 재수화반응)

  • Rhee, Seog Woo;Kang, Mun-Ja;Moon, Hichung
    • Journal of the Korean Chemical Society
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    • v.39 no.8
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    • pp.627-634
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    • 1995
  • Layered double hydroxides ($Mg-Al-CO_3$ systems, LDH), which are hydrotalcite-like anionic clay minerals, having different $Mg^{2+}\;to\;Al^{3+}$ ratio were synthesized by coprecipitation method. The subsequent products were characterized by the following methods; elemental analysis, X-ray powder diffraction, thermal analysis (DSC and TGA), FT-IR and $^{27}$Al-MAS NMR. X-ray powder patterns showed that the products formed were layered structure materials. Two heat absorption peaks were observed around 20 ∼280$^{\circ}C$ (surface water and interlayer water) and 280∼500$^{\circ}C$ (water from lattice hydroxide and carbon dioxide from interlayer carbonate) in DSC diagrams, and they were quantitatively analyzed by TGA diagrams (in case LDH4 16.2% and 28.6% respectively). FT-IR spectra indicate that the interlayer carbonate ions occupied symmetrical sites between two adjacent layers in a parallel direction. $^{27}$Al-MAS NMR spectra show only single resonance (8.6 ppm) of the octahedrally coordinated aluminum similar magnesium. When LDH4 was calcined at 560$^{\circ}C$ for 3 hours in air, its layered structure was destroyed giving a mixed metal oxide. However it readily became rehydrated in aqueous chromate solution to its original structure.

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Structural and Chemical Characterization of Aquatic Humic Substances in Advanced Water Treatment Processes (고도정수처리 공정에서 수질계 휴믹물질의 구조 및 화학적 특성분석)

  • Kim, Hyun-Chul;Yu, Myong-Jin
    • Journal of Korean Society of Environmental Engineers
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    • v.27 no.3
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    • pp.240-246
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    • 2005
  • Humic substances HS) from process waters at advanced water treatment plant consisted of GAC and Ozone/GAC processes were isolated and extracted by physicochemical fractionation methods to investigate their characteristics. They are characterized for their functionality, chemical composition, spectroscopic characteristics using FT-IR and $^1H$-NMR spectroscopy. Humic fraction gradually decreased from 36.3% to 24.2% from 0.45 to 0.30 mgC/L) through ozonation and carbon adsorption. The humic fraction was isolated into the phenolic and carboxylic groups using A-21 resin, and the concentration of phenolic groups gradually decreased from 38.4% to 23.5% (from 4.9 to $3.2\;{\mu}M/L$ as phenolic-OH) through ozonation and carbon adsorption. In the case of carboxylic groups, the concentration decreased from 61.6% to 43.3% (from 7.8 to $5.8\;{\mu}M/L$ as COOH) through the water treatment processes. On the other hand, concentrations of those roups decreased from 38.4% to 24.0% and 61.6% to 44.9% through carbon adsorption without ozonation, respectively. The structural changes of HS identified from FT-IR and $^1H$-NMR were consistent with the results from the isolation of functional groups in HS.

Synthesis and Characterization of Novel Polythiourethanes (새로운 폴리(티오우레탄)의 합성 및 특성)

  • 김경만;허영태;박인환;이범재
    • Polymer(Korea)
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    • v.27 no.5
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    • pp.470-476
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    • 2003
  • In order to obtain high refractive plastic materials, 1,2 -ethylenedisulfanylbis(2-mercaptomethyl-1-ethanthiol) (ESTT) was newly prepared in good yield by the reaction of 1,2-ethylenedisulfanylbis(2-bromomethyl-1-ethanthiol) (ESTB) with thiourea followed by hydrolysis using an aqueous ammonia solution and characterized by $^1$H-NMR (-SH at 1.7 ppm), $\^$13/C-NMR(-CH$_2$SH at 28.4 ppm) and FT-IR (-SH at 2540 cm$\^$-1/) spectroscopy, etc. Polythiourethanes (PTU) were obtained from the combinations of ESTT with each of 4,4'-methylenebis(phenylisocyanate) (MDI), tolyene 2,4-diisocyanate (TDI), isophorone diisocyanate (IPDI), mxylene diisocyanate (XDI), and 1,6-diisocyanatohexane (HMDI) in the presence of dibutyltin dilaurylate as a catalyst, in a casting mold, and characterized by FT-IR (existence of N=C=O) spectroscopy and elemental analyzer (sulfur content). Accordingly, their thermal, mechanical and optical properties were investigated by using DSC, TGA, hardness tester and refractometer: both the melting point on DSC and crystallinity on X -ray diffraction (XRD) for specimens of PTUs were not observed. PTUs with T$\_$g/s above 110 $^{\circ}C$ showed good hardness (Shore D) in the range of 86 to 89. Thermal stabilities of PTUs obtained by using ESTT and each of diisocyanates containing aromatic rings were especially good. Also, the optical transmittances of amorphous PTUs through UV-visible source in the range of 400 to 600 nm were good. PTUs showed refractive indexes above 1.60, and their refractive indexes gradually increased with increase of sulfur contents.

Effect of Thermal History on the Physical Properties of Nylon66 (열 이력이 나일론66의 물성에 미치는 영향)

  • Lee, Bom Yi;Jo, Chan Woo;Shim, Chang Up;Lim, Su Jung;Kim, Youn Cheol
    • Applied Chemistry for Engineering
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    • v.25 no.1
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    • pp.90-95
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    • 2014
  • Nylon66 extrudates as a function of the extrusion number were prepared by a twin screw extruder. Chemical structures, thermal properties, melt index, crystal structures, mechanical properties such as the tensile strength, elongation at break and impact strength, and rheological property were measured by FT-IR, $^1H$-NMR, melt indexer, DSC, TGA, XRD, universal tensile tester, Izod impact tester, and rheometer. FT-IR and $^1H$-NMR characterizations indicated that the number of extrusions did not affect the chemical structure. The decrease in the molecular weight was checked by the melt index of extrudates. There were no effects of the thermal history on the melting and degradation temperature. The tensile and impact strength and modulus were found to be similar, regardless of the number of extrusions, but the elongation decreased significantly. The complex viscosity of extrudates at low frequencies decreased with the extrusion number. No structural changes after extrusion were confirmed from the fact that there was no change in the slope and shape of G'-G" plot.

Synthesis of New Bicyclic Aziridines Containing Chalcone Analogs and Investigation of Their Photochromic Properties

  • Besharati-Seidani, Tayebeh;Mahmoodi, Nosrat O.
    • Bulletin of the Korean Chemical Society
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    • v.34 no.3
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    • pp.875-883
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    • 2013
  • Ten new derivatives of 1,3-diazabicyclo[3.1.0]hex-3-enes linked via ether linkage to chalcones were synthesized and characterized by UV, FT-IR, $^1H$ NMR and $^{13}C$ NMR spectral techniques. The spectra of all synthesized compounds, confirmed structure-photochromic behavior relationships (SPBR) both in solution or in solid state by irradiation under UV light at 254 nm. In other efforts for first time photochromic behavior of ketoaziridines has been investigated.

Copolymerization of 4′-vinylbenzo-15-crown-5 with Di(ethylene glycol) Ethyl Ether Acrylate

  • Jin, Long Yi;Mah, Soukil
    • Fibers and Polymers
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    • v.3 no.2
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    • pp.49-54
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    • 2002
  • Radical copolymerization behavior of 4'-vinylbenzo-15-crown-5, a vinyl monomer having a pendant 15-membared crown ether unit (VCE) with di(ethylene glycol) ethyl ether acrylate (DEGEEA) was carried out in toluene solution using 2,2-azobisisobutyronitrile (AIBN) as an initiator. The copolymers were characterized by means of FT-IR, $^1{H-NMR}$, and $^{13}{C-NMR}$ . The reactivity ratio of VCE and DEGEEA, determined by Fineman-Ross and Kelen-Tudos method, gave values 0.55 for VCE, and 0.11 for DEGEEA respectively.