41 research outputs found

    Titanium(IV)-EDTA complex - Kinetics of thermal decomposition by non-isothermal procedures

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    This work aims the evaluation of the kinetic triplets corresponding to the two successive steps of thermal decomposition of Ti(IV)-ethylenediaminetetraacetate complex. Applying the isoconversional Wall-Flynn-Ozawa method on the DSC curves, average activation energy: E=172.4 +/- 9.7 and 205.3 +/- 12.8 kJ mol(-1), and pre-exponential factor: logA = 16.38 +/- 0.84 and 18.96 +/- 1.21 min(-1) at 95% confidence interval could be obtained, regarding the partial formation of anhydride and subsequent thermal decomposition of uncoordinated carboxylate groups, respectively.From E and logA values, Dollimore and Malek methods could be applied suggesting PT (Prout-Tompkins) and R3 (contracting volume) as the kinetic model to the partial formation of anhydride and thermal decomposition of the carboxylate groups, respectively

    Application of Nonisothermal Cure Kinetics to the Interaction of Poly(ethylene terephthalate) with Alkyd Resin Varnish

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    Samples of varnish (V), poly(ethylene terephthalate) from recycled soft drink bottles (PET-R), and varnish/poly(ethylene terephthalate) from recycled soft drink bottles mixtures (VPET-Rs) were evaluated with differential scanning calorimetry (DSC) to verify their physicochemical properties and thermal behavior. Films from V and VPET-R were visually similar. The maximum amount of PET-R that we could add to V without significantly altering its filming properties, such adherence and color in glass sheets, was 2%. The cure process (80-203 degrees C) was identified through the DSC curves. The kinetic parameters, activation energy (E), and Arrhenius parameter (A) for the samples containing 0.5-2% PET-R were calculated with the Flynn-Wall-Ozawa isoconversional method. With greater amounts of PET-R added, there was a small change in E for the curing process. A kinetic compensation effect, represented by the equation ln A = -10.5 + 0.29E, was observed for all of the samples. The most suitable kinetic model to describe this curing process was the autocatalytic Sestak-Berggren model, which is applied to heterogeneous systems governed by nucleation and growth. (C) 2010 Wiley Periodicals, Inc. J Appl Polym Sci 119: 1316-1321, 2011Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq

    Evaluation of organic molecules originated during composting process

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    The composting process using sugarcane bagasse, animal manure, and urea as source of organic matter, microorganism, and nitrogen, respectively, were evaluated regarding the thermal behavior considering the maturation period: 0 (raw), 15, 22, 30, and 60 days. Thermogravimetric and differential thermal analysis curves were obtained in a synthetic air atmosphere and heating rate of 10 A degrees C min(-1) in the range of 30-600 A degrees C. The raw compost showed 80% organic matter, which was reduced up to 58% to 60 days compost. Two main mass losses were verified, corresponding to characteristics exothermic peak in differential thermal analysis curves depending on the maturation period. The variation in organic composition was evaluated by Fourier transform infrared spectroscopy verifying the structures (lignin, cellulose, and hemicelluloses) changes with composting process, and the gas chromatography-mass spectrometry was used to identify substance soluble in hexane.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq

    Thermal behaviour and analytical study of the production of TiSnOx from the mixed 8-hydroxyquinolinates

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    Solubility and pH precipitation studies were carried out to obtain the binuclear complex {[TiO(C9H6NO)2][Sn(C9H6NO) 2]} involving 8-hydroxyquinoline as chelating agent. The compound, the individual mononuclear complexes and their physical mixture were evaluated by means of techniques such as TG, DTA, elemental analysis, X-ray diffraction, IR spectroscopy. The properties of the original compounds and also the thermoanalytical conditions exerted a great influence on the degree of crystallinity and on the crystalline phase of the mixed oxide obtained as final product of the thermal decomposition

    SrTiO3 preparation through coprecipitation methods

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    Precursor powders to obtain SrTiO3 were prepared by using 8-hydroxyquinoline precipitant agent. The residues from the thermal decomposition, followed by TG/DTG/DTA, were characterized by XRD and it could be verified that the mixed oxides could be obtained varying the thermal decomposition conditions like atmosphere and heating rate. However, the morphology and crystallinity of these residues is highly affected by such variations. (C) 2000 Elsevier B.V. B.V. All rights reserved

    Tin(II)-EDTA complex: kinetic of thermal decomposition by non-isothermal procedures

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    Tin on the oxide form, alone or doped with others metals, has been extensively used as gas sensor, thus, this work reports on the preparation and kinetic parameters regarding the thermal decomposition of Sn(II)-ethylenediaminetetraacetate as precursor to SnO2. Thus, the acquaintance with the kinetic model regarding the thermal decomposition of the tin complex may leave the door open to foresee, whether it is possible to get thin film of SnO2 using Sn(II)-EDTA as precursor besides the influence of dopants added.The Sn(II)-EDTA soluble complex was prepared in aqueous medium by adding of tin(II) chloride acid solution to equimolar amount of ammonium salt from EDTA under N-2 atmosphere and temperature of 50degreesC arising the pH similar to 4. The compound was crystallized in ethanol at low-temperature and filtered to eliminate the chloride ions, obtaining the heptacoordinated chelate with the composition H2SnH2O(CH2N(CH2COO)(2))(2).0.5H(2)O.Results from TG, DTG and DSC curves under inert and oxidizing atmospheres indicate the presence of water coordinated to the metal and that the ethylenediamine fraction is thermally more stable than carboxylate groups. The final residue from thermal decomposition was the SnO2 characterized by X-ray as a tetragonal rutile phase.Applying the isoconversional Wall-Flynn-Ozawa method on the DSC curves, average activation energy: E-a = 183.7 +/- 12.7 and 218.9 +/- 2.1 kJ mol(-1), and pre-exponential factor: log A = 18.85 +/- 0.27 and 19.10 +/- 0.27 min(-1), at 95% confidence level, could be obtained, regarding the loss of coordinated water and thermal decomposition of the carboxylate groups, respectively. The E-a and logA also could be obtained applying isoconventional Wall-Flynn method on the TG curves.From E-a and log A values, Dollimore and Malek procedures could be applied suggesting R3 (contracting volume) and SB (two-parameter model) as the kinetic model to the loss of coordinated water (177-244degreesC) and thermal decomposition of the carboxylate groups (283-315degreesC), respectively. Simulated and experimental normalized DTG and DSC curves besides analysis of residuals check these kinetic models. (C) 2003 Elsevier B.V. All rights reserved

    Kinetic studies of urban solid residues and leachate from sanitary landfill

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    Urban solid residues are constituted of food remaining, grass leaves, fruit peelings, paper, cardboard, rubber, plastic, etc. The organic fraction formed represents about 50% during the decomposition yields biogas and leachate, which are sources of pollution. Residue samples were collected from the landfill in different and cells from several ages and the corresponding leachate, both after treatments, were submitted to thermal analysis. Kinetic parameters were determined using Flynn-Wall-Ozawa method. The linear relation between the two kinetic parameters (ln A and E) was verified for organic residue urban`s samples, but not for leachate`s sample. The occurred difference can be attributed to the constituents present in leachate

    Kinetic of thermal decomposition of residues from different kinds of composting

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    Non-isothermal kinetic parameters regarding to the thermal decomposition of the ligninocellulosic fraction present in compost from urban solid residues (USR) obtained through stack covered (SC) with composted material, comes from the usine in composing of Araraquara city, São Paulo state, Brazil, and from stack containing academic restaurant organic solid residues (SAR). The samples were periodically revolved round 132 days of composting.Results from TG, DTG and DSC curves obtained on inert atmosphere indicated that the lignocellulosic fraction present, despite the slow degradation during the composting process, is thermally less stable than other substances originated during that process. The lignocellulosic fraction decomposition, between 200 and 400degreesC, were kinetically evaluated through non-isothermal methods of analysis.By using the Flynn-Wall and Ozawa isoconversional method, the medium activation energy, E-a, and pre-exponential factor, IgA, were 283.0+/-4.6, 257.6+/-1.3 U mol(-1) and 25.4+/-0.8, 23.2+/-0.2 min(-1),to the SC and SAR, respectively, at 95% confidence level.From E-a, and IgA values and DSC curves, Malek procedure could be applied, Suggesting that the SB (Sestik-Berggren) kinetic model is suitable for the first thermal decomposition step

    Comportamento térmico do 8-quinolinol e seus nitro-derivados Thermal behavior of the 8-quinolinol and their nitro-derivatives

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    <abstract language="eng">The compounds 5-nitro-8-quinolinol and 5,7-dinitro-8-quinolinol were obtained by nitration of the chelant 8-quinolinol. The compounds were characterized through EA, MNR, XRD, IR, TG, DTA and DSC. It was verified through thermal analysis that the compounds show consecutive processes of sublimation, fusion and vaporization. During the vaporization process, partial thermal decomposition was observed, with formation of carbonaceous residues. Considering a slower heating rate, the sublimation is the prevalent process to the nitro-derivatives while the vaporization is the main process to 8-quinolinol. The thermal stability follows the decreasing order from 5,7-dinitro-8-quinolinol to 5-nitro-8-quinolinol to 8-quinolinol

    Thermal behavior of lignin and cellulose from waste composting process

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    The lignin and cellulose were extracted from reference material (leaves and twigs) and food of compost at different times composting: zero (raw), 30, and 120 days. According to thermogravimetric analysis and its derivative and differential scanning calorimetry curves for these samples, were verified during composting process there were considerable changes in its thermal profiles, as well as, characteristics lignin in cellulose samples and cellulose in lignin samples. These features were found by fourier transformed infrared spectroscopy. © 2012 Akadémiai Kiadó, Budapest, Hungary
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