Kinetic model of poly(3-hydroxybutyrate) thermal degradation from experimental non-isothermal data

The non-isothermal data given by TG curves for poly(3-hydroxybutyrate) (PHB) were studied in order to obtain a consistent kinetic model that better represents the PHB thermal decomposition. Thus, data obtained from the dynamic TG curves were suitably managed in order to obtain the Arrhenius kinetic parameter E according to the isoconversional F-W-O method. Once the E parameters is found, a suitable logA and kinetic model (f(alpha)) could be calculated. Hence, the kinetic triplet (E +/- SD, logA +/- SD and f(alpha)) obtained for the thermal decomposition of PHB under non-isothermal conditions was E=152 +/- 4 kJ mol(-1), logA=14.1 +/- 0.2 s(-1) for the kinetic model, and the autocatalytic model function was: f(alpha)=alpha(m)(1-alpha)(n)=alpha(0.42)(1-alpha)(0.56).

Study of the thermal behavior of the transition phase of Co(II)-diclofenac compound by non-isothermal method

The Co(II)-diclofenac complex was evaluated by simultaneous thermogravimetry-differential thermal analysis (TG-DTA) and differential scanning calorimetry (DSC). The DTA curve profile shows one exothermic peak because of the transition phase of the compound between 170 and 180 A degrees C, which was confirmed by X-ray powder diffractometry. The transition phase behavior was studied by DSC curves at several heating rates of a sample mass between 1 and 10 mg in nitrogen atmosphere and in a crucible with and without a lid. Thus, the kinetic parameters were evaluated using an isoconversional non-linear fitting proposed by Capela and Ribeiro. The results show that the activation energy and pre-exponential factor for the transition phase is dependant on the different experimental conditions. Nevertheless, these results indicate that the kinetic compensation effect shows a relationship between them.

Synthesis, characterization and thermal behaviour of solid-state compounds of europium(III) and gadolinium(III) 3-methoxybenzoate

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Synthesis, characterization and thermal behaviour on solid tartrates of some bivalent metal ions

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Effect of the catalyst MCM-41 on the kinetic of the thermal decomposition of poly(ethylene terephthalate)

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Synthesis, characterization and thermal behaviour of solid state compounds of 2-chlorobenzylidenepyruvate with trivalent aluminium, gallium, indium and scandium metals

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Synthesis, characterization and thermal behaviour of solid state compounds of 4-methoxybenzoate with Manganese, Nickel and Copper

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Thermal and spectroscopic investigation on N,N-dimethylbenzylamine based cyclopalladated compounds containing isonicotinamide

Synthesis, spectroscopic characterization and thermal analysis of the [Pd(dmba)(Cl)(iso)] (1), [Pd(dmba)(NCO)(iso)] (2), [Pd(dmba)(N(3))(iso)] (3) and [Pd(dmba)(Br)(iso)] (4) (dmba = N,N'-dimethylbenzylamine; iso = isonicotinamide) compounds are described in this work. The complexes were investigated by infrared spectroscopy (IR), differential thermal analysis (DTA) and thermogravimetry (TG) and the residues of the thermal decomposition were identified as Pd(o) by X-ray powder diffraction. The thermal stability order of the complexes varied as [Pd(dmba)(Cl)(iso)] (1) > [Pd(dmba)(Br)(iso)] (4) > [Pd(dmba)(NCO)(iso)] (2) > [Pd(dmba)(N(3))(iso)] (3).

Synthesis, characterization, and thermal behavior of palladium(II) coordination compounds containing isonicotinamide

Palladium(II) coordination compounds of general formula trans-[PdX(2)(isn)(2)], X = Cl(-) (1), N(3) (-) (2), SCN(-) (3), NCO(-) (4), isn = isonicotinamide; were synthesized and characterized in solid state by elemental analysis, infrared spectroscopy, and simultaneous TG-DTA. TG experiments reveal that the compounds 1-4 undergo thermal decomposition in three or four stages, yielding Pd(0) as final residue, according to calculus and identification by X-ray powder diffraction.

Synthesis, characterization, thermal studies, and DFT calculations on Pd(II) complexes containing N-methylbenzylamine

This work describes the synthesis, characterization, and the thermal behavior investigation of four palladium(II) complexes with general formulae [PdX(2)(mba)(2)], in which mba = N-methylbenzylamine and X = OAc(-) (1), Cl(-) (2), Br(-) (3) or I(-) (4). The complexes were characterized by elemental analysis, infrared vibrational spectroscopy, and (1)H nuclear magnetic resonance. The stoichiometry of the complexes was established by means of elemental analysis and thermogravimetry (TG). TG/DTA curves showed that the thermodecomposition of the four complexes occurred in 3-4 steps, leading to metallic palladium as final residue. The palladium content found in all curves was in agreement with the mass percentages calculated for the complexes. The following thermal stability sequence was found: 3 > 2 > 4 > 1. The geometry optimization of 1, 2, 3, and 4, calculated using the DFT/B3LYP method, yielded a slightly distorted square planar environment around the Pd(II) ion made by two anionic groups and two nitrogen atoms from the mba ligand (N1 and N2), in a trans-relationship.

Synthesis, spectral and thermal studies on dicarboxylate-bridged palladium(II) coordination polymers. Part I

This work describes the synthesis, IR and (13)C CPMAS NMR spectroscopic as well the thermal characterization of the new dicarboxylate complexes [Pd(2)(ox)(2)(4,4'-bipy)]n (1), [Pd(2)(ox)(2)(bpe)](n) (2) and [Pd(2)(ox)(2)(pz)](n) (3) {ox = oxalate, bipy = 4,4'-bipyridine, bpe = 1,2-bis(4-pyridyl)ethane, pz = pyrazine}. TG experiments reveal that compounds 1-3 undergo thermal decomposition in three steps. Metal palladium was the final product of the thermal decompositions, which was identified by X-ray powder diffraction.

Synthesis, characterization, and investigation of the thermal behavior of Cu(II) pyrazolyl complexes

This work reports the synthesis, characterization, and thermal behavior of three complexes of copper (II): [CuCl(2)(HPz)(4)] (1), [CuCl(2)(HdmPz)(4)] (2), and [CuCl(2)(HIPz)(4)] (3) (HPz = pyrazole; HdmPz = 3,5-dimethylpyrazole; HIPz = 4-iodopyrazole). The compounds were characterized by elemental analysis, infrared spectroscopy, and UV-Vis measurements. The thermal study of the compounds showed that the ligands are eliminated in 2-4 stages, yielding CuO as final residue.

Synthesis, spectral and thermal studies on dicarboxylate-bridged palladium(II) coordination polymers. Part II

The synthesis and thermal behavior of the new [Pd(fum)(bipy)] (n) center dot 2nH(2)O (1), [Pd(fum)(bpe)] (n) center dot nH(2)O (2) and [Pd(fum)(pz)] (n) center dot 3nH(2)O (3) {bipy = 4,4'-bipyridine, bpe = 1,2-bis(4-pyridyl)ethene and pz = pyrazine} fumarate complexes are described in this work as well their characterization by IR and (13)C CPMAS NMR spectroscopies. TG curves showed that the compounds released organic ligands and lattice water molecules in the temperature range of 46-491 A degrees C. In all the cases, metallic palladium was identified as the final residue.

Thermal, structural and optical properties of new tungsten lead-pyrophosphate glasses

Crystalline lead-pyrophosphate precursor was prepared in aqueous solution from lead nitrate and phosphoric acid and characterized by X-ray diffraction, thermogravimetry and Raman scattering. This crystalline lead-phosphate was then used to prepare glass samples in the binary system Pb(2)P(2)O(7)-WO(3). Dependence of WO(3) content on thermal, structural and optical properties were investigated by thermal analysis (DSC), Raman spectroscopy, UV-visible and near-infrared absorption and M-Line technique to access refractive index values. Incorporation of WO(3) in the lead-pyrophosphate matrix enhances the glass transition temperature and thermal stability against devitrification, favors formation of P-O-W bonds and WO(6) clusters. In addition, optical properties are strongly modified with a redshift of the optical bandgap with WO(3) incorporation as well as an increase of the refractive index from 1.89 to 2.05 in the visible. (C) 2011 Elsevier B.V. All rights reserved.

Thermal decomposition and stability in a series of heterobimetallic carbonyl compounds of the type [Fe(CO)4(HgX)2] (X=Cl, Br, I)

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)