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

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Solid Chemical Material Site Analysis Research of Event Site (사건현장의 고체상 화학물질 현장분석 연구)

  • Kim, Sungbum;Noh, Hyeran;Lee, Jinseon;Kim, Jungmin;Cho, Munsik;Park, Choonhwa;Chun, Kwangsoo;Ahn, Seungyoung;Seok, Gwangseol
    • Journal of the Society of Disaster Information
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    • v.8 no.3
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    • pp.304-309
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    • 2012
  • National Institute of Environmental Research has Portable FT-IR(Fourier Transform Infrared Spectroscopy, A2 Technologies, U.S.A.) and Portable XRD(X-ray Diffraction, Olympus Innov-X co., U.S.A.) for the analysis of the solid sample rapidly on the spot where chemical terror accident took place and the portable equipments are operating now. However, we need a series of the analysis procedures for an efficient application of the equipments and getting the rapid analytical value about the investigation and sampling on the spot. And the accuracy of the portable equipments' analytical value is high but the application of them in an emergency is low because we are lack of the procedures about field-centered analysis and the usage. Therefore we would like to organize the result of this research about field analysis and the procedures of the solid portable equipments. And we also would like to apply it to the field of chemical terror accident.

Synthesis of High Purity Alumina by Controlled Precipitation Method from Clay Minerals (I) Preparation of Aluminum Sulfate Hydrate and Alumina from Clay Minerals (점토 광물로부터 제어 침전법에 의한 고순도 알루미나의 합성 (I) 점토 광물로부터 수화 황산 알루미늄 및 알루미나의 제조)

  • No, Tae-Hwan;Lee, Heon-Su;Son, Myeong-Mo;Park, Hui-Chan
    • Korean Journal of Materials Research
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    • v.2 no.1
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    • pp.3-11
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    • 1992
  • Aluminum sulfate hydrate was prepared using sulfuric acid from Ha-dong kaolin. The effects of calcination-temperature and calcination-time of kaolin, reaction-temperature and reaction-time, and sulfuric acid concentration on the formation of aluminum sulfate hydrate were investigated. The precipitation condition of aluminum sulfate hydrate from sulfuric acid solution was determined. Also, the products heat-treated at different temperatures have been investigated by X-ray diffraction, thermogravimetry, differential thermal analysis, Fourier transform infrared spectrophotometer, scanning electron microscopy, particle size distribution analysis and chemical analysis. In the optimum condition, the conversion of aluminum oxide in kaolin to aluminum sulfate hydrate was 60%. From the results of XRD, TG-DTA, and FT-IR, it is suggested that the aluminum sulfate hydrate is thermally decomposed as follows ; $Al_2(SO_4)_3{\cdot}18H_2O{\rightarrow}Al_2(SO_4)_3{\cdot}6H_2O{\rightarrow}Al_2(SO_4){\rightarrow}\;amorphous\;alumina{\rightarrow}{\gamma}-alumina{\rightarrow}{\delta}-alumina{\rightarrow}{\theta}-alumina{\rightarrow}{\alpha}-alumina$. The purity of alumina powder prepared by calcining aluminum sulfate hydrate at $1200^{\circ}C$ was 99.99 percent.

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Effect of PC(Polycarboxylate) Type Superplasticizer on the Hydration Reaction of Cement Paste (PC(Polycarboxylate)계 고유동화제가 시멘트 수화 반응에 미치는 영향)

  • Chae, Eun-Jin;Shin, Jin-Yong;Suh, Jeong-Kwon;Lee, Jung-Min;Park, Jin-Won
    • Journal of the Korea Concrete Institute
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    • v.18 no.4 s.94
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    • pp.569-576
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    • 2006
  • PC-type copolymers were synthesized using MPEG(polyethylene glycol methyl ether methacrylate, Mn=2080) to different mole ratios of mono-carboxylic acid(AA : acylic acid). The mole ratios of AA were 2, 3, 4 and PC-type terpolymers were synthesized using mono-, dicarboxylic acid(ITA : itaconic acid MAL : maleic acid) with the same graft chain. To investigate effects of PC-type co-, ter-polymers on the hydration of cement experiments involving FT-IR, XRD, DSC, SEM have been analysed with cement paste specimens to 1, 3, 28 day. The hydration reaction rate of cement paste was slightly delayed at 1 day, due to increase in molar ratio of [AA]/[MPEG], it was recovered in the days after and the copolymer was more active than the terpolymer, because of low carboxylic acid content PC-type copolymers applied 2AA-type were fastest copolymer on hydration reaction of cement paste to 3 day and the more AA mole ratios increased, the more hydration was retarded.

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.

Sol-gel Synthesis and Properties of Phosphate Ceramics

  • Lee, Burtrand I.;Cao, Zhicheng;Samuels, Willam D.;Exarhos, Gregory J.
    • The Korean Journal of Ceramics
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    • v.6 no.4
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    • pp.390-395
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    • 2000
  • Silicon, titanium, zirconium phosphates were synthesized by starting with appropriate chemical precursors in a solution. The synthetic procedure, chemical and physical structures were examined by FT-IR, liquid and solid state NMR, TGA, SEM, XRD, etc. The phosphates were examined for thermal and electrical properties. Advantages of the synthesis technique and the data on unique structures and thermal properties are reported.

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The Role of DCCA in the Sol-Gel Process Preparing Silica Glass (졸-겔법에 따른 실리카 유리 제조에 있어서 DCCA의 역할에 관한 연구)

  • 박용완;연석주
    • Journal of the Korean Ceramic Society
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    • v.28 no.6
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    • pp.488-494
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    • 1991
  • In this study, the effects of catalyst and DCCA content were investigated in order to determine the optimum conditions of monolithic silica gel formation through sol-gel process. Formamide, oxalic acid, glycerol and dimethylformamide are used as DCCA. To observe the phenomena in drying and heat-treating of gels, we examined structural exchange of gels using FT-IR, TG-DTA and XRD. Monolithic gels were obtained by adding formamide and dimethylformamide as DCCA. According to the heat treatment schedule, silica glass is prepared by heat-treatment up to 1050$^{\circ}C$.

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Preparation of Polycrystalline Mullite Fiber Using the Sol-Gel Technique (졸-겔법에 의한 다결정 물라이트 섬유의 제조)

  • 김경용;김윤호;이수원;정형진;김구대
    • Journal of the Korean Ceramic Society
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    • v.26 no.6
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    • pp.795-801
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    • 1989
  • The polycrystalline mullite fiber was synthesized from various combination of starting materials including metal alkoxides and colloidal sol by the sol-gel process. The best spinnability was observed in the sol which showed shear thinning and hysteresis (i.e., thixotropic flow), indicating that the network structure was broken down as the shear rate increased. The mullite fiber was polycrystalline after firing and characterized by thermal analysis, XRD, FT-IR spectroscopy, rheological measurements, and SEM.

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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.

Preparation of Porous TiO2 Thin Films by Poly(vinyl chloride)-graft-poly(N-vinyl pyrrolidone) and Their Applications to Dye-sensitized Solar Cells

  • Yeon, Seung-Hyeon;Patel, Rajkumar;Koh, Jong-Kwan;Ahn, Sung-Hoon;Kim, Jong-Hak
    • Journal of the Korean Electrochemical Society
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    • v.14 no.2
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    • pp.83-91
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    • 2011
  • Mesoporous titanium dioxide ($TiO_2$) thin films were prepared using poly(vinyl chloride)-graft-poly(N-vinyl pyrrolidone) (PVC-g-PVP) as a templating agent via sol-gel process. Grafting of PVC chains from PVC backbone was done by atom transfer radical polymerization (ATRP) technique. The successful grafting of PVP to synthesize PVC-g-PVP was checked by fourier-transform infrared spectroscopy (FT-IR) and gel permeation chromatography (GPC). The carbonyl group interaction of PVC-g-PVP graft copolymer with $TiO_2$ was confirmed by FT-IR. The porous morphologies of the $TiO_2$ films genereated after calcination at $450^{\circ}C$ was characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The mesoporous $TiO_2$ films with 580 nm in thickness were used as a photoelectrode for solid state dye sensitized solar cell (DSSC) and showed an energy conversion efficiency of 1.05% at 100 $mW/cm^2$.

Synthesis of Polyurethane Nanocomposite Filled Inorganic Particles and Their Properties (무기입자를 충전한 폴리우레탄 나노복합체의 합성 및 물성)

  • Son, Bok-Gi;Hwang, Taek-Sung
    • Polymer(Korea)
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    • v.31 no.5
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    • pp.379-384
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    • 2007
  • The nanocomposites with inorganic nano powder, improved thermal stability, were prepared by urethane polymerization. The structure and surface properties of the nanocomposites were determined by X-ray diffraction and FT-IR, respectively. The thermal stabilities were studied using TGA and DSC. Their morphologies and mechanical properties were observed by SEM and UTM. As a result, the nanocomposites with MMT led to the increase of the silicate layers. The distance between layers of the nanacomposites with MMT was increased by $7.5{\AA}$ and the new peaks at $1038cm^{-1}$ were shown in the presence of the Si-O groups on the silica. The thermal stabilities of the nanocomposites were higher than those of pore polyurethane matrix. The nanocomposites had higher in mechanical properties than the pure polyurethane matrix.