• Title/Summary/Keyword: TG-DTG

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Thermal Decomposition of Barium Titanyl Oxalate Tetrahydrate (티타닐 옥살산 바륨 사 수화물의 분해 반응)

  • Lee, Sang-Beom
    • The Journal of Natural Sciences
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    • v.1
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    • pp.47-59
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    • 1987
  • The thermal decomposition mechanism of BaTiO($$C_2$$O_4$)_2$ $4H_2$O has been investigated employing TG, DTG, and DTA techniques. The intermediate compounds and the gaseous products of decomposition were examined by IR spectrometer and X-ray analyser. The decomposition proceeds through five steps. The first step which is the dehydration of the tetrahydrate is followed by the decomposition of oxalate groups. During the second decomposition, half a mole of carbon monoxide is evolved. The oxalate groups are completely destroyed in the range $260~460^{\circ}C$, resulting in the formation of a carbonate which retains free carbon dioxide in the matrix . the final decomposition of the carbonate takes place between $650~750^{\circ}C$ and yields $BaTiO_3$.

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Metal Complexes of Enrofloxacin Part I: Preparation, Spectroscopic, Thermal Analyses Studies and Antimicrobial Evaluation

  • El-Shwiniy, Walaa H.;El-Attar, Mohamed S.;Sadeek, Sadeek A.
    • Journal of the Korean Chemical Society
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    • v.57 no.1
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    • pp.52-62
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    • 2013
  • The interaction of titanium (IV), yttrium (III), zirconium (IV), palladium (II) and cerium (IV) with deprotonated enrofloxacin leads to the formation of the neutral or cationic mononuclear complexes. The isolated solid complexes have been characterized with physicochemical and spectroscopic techniques and thermogravimeteric analyses. The spectroscopic data indicate that the enrofloxacin ligand is on the deprotonated mode acting as bidentate ligand coordinated to the metal ions through the ketone oxygen and a carboxylato oxygen and the metal ions completed the coordination number with water molecules. The thermal decomposition mechanisms proposed for enrofloxacin and their metal complexes were discussed. The activation energies, $E^*$, enthalpies, ${\Delta}H^*$, entropies, ${\Delta}S^*$ and Gibbs free energies, ${\Delta}G^*$, of the thermal decomposition reactions have been derived from thermogravimetric (TG) and differential thermogravimetric (DTG) curves, using Coats-Redfern (CR) and Horowitz-Metzeger (HM) methods. The antimicrobial activity has been evaluated against six different microorganisms.

Photoreactivity and Thermogravimetry of Copper(II) Complexes of N-Salicylideneaniline and Its Derivatives

  • Osman, Ahmed H.;Aly, Aref A.M.;El-Mottaleb, Mohamed Abd;Gouda, Gamal A.H.
    • Bulletin of the Korean Chemical Society
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    • v.25 no.1
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    • pp.45-50
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    • 2004
  • $Cu^{II}$-complexes of N-salicylideneaniline and its derivatives were not light sensitive in most solvents such as acetonitrile. A photo-decomposition occurred upon irradiation in halocarbon solvents such as $CHCl_3$. It has been suggested that such photoreactivity is attributed to the reactivity of charge-transfer to solvent (CTTS) excited state attained upon irradiation. A mechanism has been proposed to account for the results obtained. The complexes have been thermally analysed in nitrogen and static air using thermogravimetry (TG) and derivative thermogravimetry (DTG). The thermal degradation of the complexes proceeds in two or three stages. The kinetic parameters obtained from the Coats-Redfern and Horowitz-Metzger equations show the kinetic compensation effect.

Characterization of Poly(methyl methacrylate)-tin (IV) Chloride Blend by TG-DTG-DTA, IR and Pyrolysis-GC-MS Techniques

  • Arshad, Muhammad;Masud, Khalid;Arif, Muhammad;Rehman, Saeed-Ur;Saeed, Aamer;Zaidi, Jamshed Hussain
    • Bulletin of the Korean Chemical Society
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    • v.32 no.9
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    • pp.3295-3305
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    • 2011
  • Thermal behavior of poly (methyl methacrylate) was analyzed in the presence of tin (IV) chloride. Five different proportions - polymer to additive - were selected for casting films from common solvent. TG, DTG and DTA were employed to monitor thermal degradation of the systems. IR and py-GC-MS helped identify the decomposition products. The blends start degrading at a temperature lower than that of the neat polymer and higher than that of the pure additive. Complex formation between tin of additive and carbonyl oxygen (pendent groups of MMA units) was noticed in the films soon after the mixing of the components in the blends. The samples were also heated at three different temperatures to determine the composition of residues left after the expulsion of volatiles. The polymer, blends and additive exhibited a one step, two-step and three-step degradation, respectively. $T_0$ is highest for the polymer, lowest for the additive and is either $60^{\circ}C$ or $70^{\circ}C$ for the blends. The amount of residue increases down the series [moving from blend-1 (minimum additive concentration) to blend-5 (maximum additive concentration)]. For blend-1, it is 7% of the original mass whereas it is 16% for blend-5. $T_{max}$ also goes up as the concentration of additive in the blends is elevated. The complexation appears to be the cause of observed stabilization. Some new products of degradation were noted apart from those reported earlier. These included methanol, isobutyric acid, acid chloride, etc. Molecular-level mixing of the constituents and "positioning effect" of the additive may have brought about the formation of new compounds. Routes are proposed for the appearance of these substances. Horizontal burning tests were also conducted on polymer and blends and the results are discussed. Activation energies and reaction orders were calculated. Activation energy is highest for the polymer, i.e., 138.9 Kcal/mol while the range for blends is from 51 to 39 Kcal/mol. Stability zones are highlighted for the blends. The interaction between the blended parts seems to be chemical in nature.

Preparation of Cobalt-Substituted Iron Oxide Powder from Organometallic Precursors (Ⅱ) (유기금속 전구체로부터 코발트 치환 산화철 분말 제조 (Ⅱ))

  • Kim, Jeong Su;Gang, Han Cheol;Hong, Yang Gi
    • Journal of the Korean Chemical Society
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    • v.38 no.2
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    • pp.92-100
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    • 1994
  • Ultrafine cobalt-substituted iron oxide particles were prepared by the thermal decomposition and oxidation of the new organometallic precursor, $Co_xFe_{1-x}(N_2H_3COO)_2(N_2H_4)_2$ (x = 0, 0.01, 0.02, 0.03, 0.05, 0.10, 1.00). The organometallic precursors were synthesized by the reaction of Co(II) and Fe(II) ion in a mole ratio of x : 1-x with hydrazinocarboxylic acid, and characterized by quantitative analysis, elemental analysis and infrared spectroscopy. The mechanistic study on the thermal decomposition of the organometallic precursors was performed by TG-DTG and DSC. The cobalt-substituted iron oxide particles were obtained by the heat treatment of the precursors at $350^{\circ}C$ and $450^{\circ}C$ for six hours in air. The prepared iron oxide was found to have two phases such as ${\gamma}-Fe_2O_3$ and a mixture of ${\gamma}-Fe_2O_3\;and\;{\alpha}-Fe_2O_3$ at $350^{\circ}C$ and $450^{\circ}C$ respectively. The particle shape was equiaxial and the particle size was less than 0.05 ${\mu}m.$ The coercivity and squareness of the cobalt substituted iron oxide particles increased with increasing cobalt content. Both coercivity and squareness showed higher values at $450^{\circ}C.$

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Synthesis, Spectral and Thermal Studies of Lanthanide(III) Complexes of Phenylbutazone (Phenylbutazone의 란탄(III) 착물에 대한 합성, 스펙트럼 및 열적 연구)

  • Anoop, M.R.;Binil, P.S.;Jisha, K.R.;Suma, S.;Sudarsanakumar, M.R.
    • Journal of the Korean Chemical Society
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    • v.55 no.4
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    • pp.612-619
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    • 2011
  • Lanthanide(III) complexes of 1,2-diphenyl-4-butyl-3,5-pyrazolidinedione(phenylbutazone, PB) have been synthesized and characterized by elemental analyses, molar conductance measurements, IR, UV-Vis. and NMR spectra. The spectral data reveal that the PB acts as a bidentate and mono-ionic ligand coordinating through both the carbonyl oxygens of the pyrazolidinedione ring. The molar conductance data suggest that the complexes are non-electrolytes. The thermal behaviour of the complexes was studied by TG and DTG in air atmosphere and the results provide information about dehydration, thermal stability and thermal decomposition. The final products are found to be the corresponding metal oxides. The thermodynamic parameters and kinetic parameters were evaluated for the dehydration and decomposition stages. The negative entropy values of the decomposition stages indicate that the activated complexes have a more ordered structure than the reactants and that the reactions are slower than normal. Based on these studies, the complexes have been formulated as $[Ln(PB)_3]{\cdot}5H_2O$(Ln=La and Ce) and $[Ln(PB)_3(H_2O)_2]{\cdot}2H_2O$(Ln=Pr, Nd and Sm).

A Study on the Characteristics of Coffee Ground(CG)-RDF by Using Different Drying Method (건조법에 따른 커피박 고형연료의 특성 고찰 연구)

  • Kim, Sang-bin;Ha, Jin-wook
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.20 no.2
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    • pp.451-457
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    • 2019
  • In this study, the characteristics of coffee grounds were reviewed by making them from solid fuel through heat-drying and oil-drying method. The differences in the higher calorific power by each dried sample were compared. And industrial analysis using the thermogravimetric analyzer was considered for applicability to organic waste and oily samples. Before and after drying, the surface of the specimen was observed with SEM equipment and the ingredients were measured through the EDS equipment. As a result, no other hazardous substances, such as heavy metals, were measured. Next, The differences between thermal decomposition and combustion reactions were considered through the TG and DTG curves. As a result, it is that the oil-dried coffee grounds is longer to burn than the heat-dried coffee grounds. Finally, the combustion gases emitted through the thermogravimetric analyzer were collected and the carbon monoxide and carbon dioxide performed qualitative and quantitative analysis using GC over time.

Tensile Properties and Thermal Stability of Cellulose Nanofibril/Clay Nanocomposites

  • Park, Byung-Dae;Singh, Adya P.;Um, In Chul
    • Current Research on Agriculture and Life Sciences
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    • v.31 no.1
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    • pp.18-24
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    • 2013
  • This work attempted to fabricate organic/inorganic nanocomposite by combining organic cellulose nanofibrils (CNFs), isolated by 2,2,6,6-tetramethylpiperidine-1-oxy radical (TEMPO)-mediated oxidation of native cellulose with inorganic nanoclay. The morphology and dimension of CNFs, and tensile properties and thermal stability of CNF/clay nanocomposites were characterized by transmission electron microscope (TEM), tensile test, and thermogravimetry (TG), respectively. TEM observation showed that CNFs were fibrillated structure with a diameter of about $4.86{\pm}1.341nm$. Tensile strength and modulus of the hybrid nanocomposite decreased as the clay content of the nanocomposite increased, indicating a poor dispersion of CNFs or inefficient stress transfer between the CNFs and clay. The elongation at break increased at 1% clay level and then continuously decreased as the clay content increased, suggesting increased brittleness. Analysis of TG and derivative thermogravimetry (DTG) curves of the nanocomposites identified two thermal degradation peak temperatures ($T_{p1}$ and $T_{p2}$), which suggested thermal decomposition of the nanocomposites to be a two steps-process. We think that $T_{p1}$ values from $219.6^{\circ}C$ to $235^{\circ}C$ resulted from the sodium carboxylate groups in the CNFs, and that $T_{p2}$ values from $267^{\circ}C$ to $273.5^{\circ}C$ were mainly responsible for the thermal decomposition of crystalline cellulose in the nanocomposite. An increase in the clay level of the CNF/clay nanocomposite predominately affected $T_{p2}$ values, which continuously increased as the clay content increased. These results indicate that the addition of clay improved thermal stability of the CNF/clay nanocomposite but at the expense of nanocomposite's tensile properties.

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Preparation, Characterization and First Application of Aerosil Silica Supported Acidic Ionic Liquid as a Reusable Heterogeneous Catalyst for the Synthesis of 2,3-Dihydroquinazolin-4(1H)-ones

  • Yassaghi, Ghazaleh;Davoodnia, Abolghasem;Allameh, Sadegh;Zare-Bidaki, Atefeh;Tavakoli-Hoseini, Niloofar
    • Bulletin of the Korean Chemical Society
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    • v.33 no.8
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    • pp.2724-2730
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    • 2012
  • A new heterogeneous acidic catalyst was successfully prepared by impregnation of silica (Aerosil 300) by an acidic ionic liquid, named 1-(4-sulfonic acid)butylpyridinium hydrogen sulfate [$PYC_4SO_3H$][$HSO_4$], and characterized using FT-IR spectroscopy, the $N_2$ adsorption/desorption analysis (BET), thermal analysis (TG/DTG), and X-ray diffraction (XRD) techniques. The amount of loaded acidic ionic liquid on Aerosil 300 support was determined by acid-base titration. This new solid acidic supported heterogeneous catalyst exhibits excellent activity in the synthesis of 2-aryl-2,3-dihydroquinazolin-4(1H)-ones by cyclocondensation reaction of 2-aminobenzamide with aromatic aldehydes under solvent-free conditions and the desired products were obtained in very short reaction times with high yields. This catalyst has the advantages of an easy catalyst separation from the reaction medium and lower problems of corrosion. Recycling of the catalyst and avoidance of using harmful organic solvent are other advantages of this simple procedure.

Synthesis, Spectral, Characterization, DFT and Biological Studies of New 3-[(3-Chlorophenyl)-hydrazono]-pentane-2,4-dione Metal Complexes

  • Sadeek, Sadeek A.;Zordok, Wael A.;El-Farargy, Ahmed F.;El-Desoky, Sameh I.
    • Journal of the Korean Chemical Society
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    • v.58 no.2
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    • pp.169-178
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    • 2014
  • A new series of metal complexes of V(IV), Pd(II), Pt(IV), Ce(IV) and U(VI) with 3-[(3-chlorophenyl)-hydrazono]-pentane-2,4-dione (Cphpd) were synthesized and characterized by elemental analysis, molar conductivity, magnetic moment measurements, UV-vis, FT-IR and $^1H$ NMR as well as TG-DTG techniques. The data indicated that the Cphpd acts as a bidentate ligand through the hydrazono nitrogen and one keto oxygen. The kinetic parameters have been evaluated by using Coats Redfern (CR) and Horowitz-Metzeger (HM) methods. The thermodynamic data reflected the thermal stability for all complexes. The calculated bond length and the bond stretching force constant, F(U=O), values for $UO_2$ bond are $0.775{\AA}$ and $286.95Nm^{-1}$. The bond lengths, bond angles, dipole moment and the lowest energy model structure of the complexes have been determined with DFT calculations. The antimicrobial activity of the synthesized ligand and its complexes were screened.