Decomposição térmica de complexos de Zn e Cd com isomaleonitriladitiolato (imnt)

Thermal decomposition of [Bu4N]2[Zn(imnt)2] and [M(NH3)2(imnt)] complexes with M = Zn and Cd, and imnt = (bis 1,1-dicyanoethylene-2,2 dithiolate) in inert atmosphere was investigated by thermogravimetric analysis (TG) and differential scanning calorimetry (DSC). Pyrolysis studies at different temperatures, 300, 400, 500, and 600 ºC, in N2 atmosphere were performed and the products were characterized by X-ray diffraction (XRD), infrared and Raman spectroscopy, and scanning electron microscopy (SEM). The products were identified as sulfide sub-micron particles, along with amorphous carbon. Particle sizes estimated by SEM were ca. 50 nm for the cationic complexes and 500 nm for the neutral complexes.

Decomposição térmica de espumas de poliuretano para fabricação de vitrocerâmica celular de Li2O-ZrO2-SiO2-Al2O3 (LZSA)

Characterization of the thermal decomposition of polyurethane (PUR) foams was performed by Fourier-transformed infrared (FT-IR) spectroscopy and thermogravimetric analysis (TGA). Three main weight loss paths were observed by TGA, the residue being lower than 3 wt.% for 3 different PUR foams analyzed. FT-IR spectra indicated CO2, CO, NH3 and isocyanides as main decomposition products. PUR foams of different cell sizes were immersed in a slurry of the parent glass ceramic of composition Li2O-ZrO2-SiO2-Al 2O3 (LZSA) and submitted to heat treatment. The LZSA cellular glass ceramics obtained after sintering and crystallization resembled the original morphology of the PUR foams.

Estudo da decomposição térmica de propelente sólido compósito de baixa emissão de fumaça

The thermal decomposition of hydroxyl-terminated polybutadiene (HTPB)/ammonium nitrate (AN) based propellants, so called smokeless formulations, and raw materials were investigated by differential scanning calorimetry (DSC) and thermogravimetry (TG). The thermoanalytical profile of different components and of propellant were evaluated and the Arrhenius parameters for the thermal decomposition of the propellant sample were determined by the Ozawa method. The kinetic parameters of the thermal decomposition of propellant samples were determined by DSC measurements. The values obtained for activation energy (Ea) and pre-exponential factor were 163 kJ mol-1 and 1.94x10(6) min-1.

Estudos termoanalíticos de sais de sódio e potássio de ditiocarbamatos em atmosfera oxidante

Thermoanalytical behavior of sodium and potassium salts of pyrrolidinedithiocarbamate (pyr), piperidineditiocarbamate (pip), morpholinedithiocarbamate (mor), hexametileneiminedithiocarbamate (hex), were investigated. In a first step the salts were synthesized and characterized by infrared spectroscopy (FTIR), ¹H and 13C nuclear magnetic resonance (NMR) and elementar analysis. Finally, thermal analytical (TG/DTG and DSC) studies were performed in order to evaluate the thermal stability, as well as the pathways of the thermal decomposition based in the intermediate and final decomposition products.

Estudo cinético da decomposição térmica do pentaeretritol-tetranitrado (PETN)

The pentaerythritol-tetranitrate (PETN) is a nitroether used in explosives and propellant formulations. Due to its suitable properties, PETN is used in booster manufacture. Knowing the thermal decomposition behavior of an energetic material is very important for storage and manipulation, and the purpose of this work is to study the kinetic parameters of the decomposition of PETN, compare the results with literature data and to study the decomposition activation energy differences between two crystalline forms of PETN (tetragonal and needle) by means of differential scanning calorimetry (DSC). Fourier transform infrared spectroscopy (FT-IR) is used to study the two crystalline forms.

Termogravimetria: um novo enfoque para a clássica determinação de cálcio em cascas de ovos

The use of thermoanalytical data in sample preparation is described as a tool to catch the students' attention to some details that can simplify both the analysis and the analytical procedure. In this case, the thermal decomposition of eggshells was first investigated by thermogravimetry (TGA). Although the classical procedures suggest long exposure to high temperatures, the TGA data showed that the decomposition of organic matter takes place immediately when the sample is heated up to 800 °C under air atmosphere. After decomposition, the calcium content was determined by flame atomic emission photometry and compared with the results obtained using classical volumetric titration with EDTA.

Modification of a Brazilian smectite clay with different quaternary ammonium salts

In this work, a smectite clay from the State of Paraiba, Brazil, was treated with six different types of ammonium salts, which is an usual method to enhance the affinity between the clay and polymer for the preparation of nanocomposites. The clays, before and after modification, were characterized by X ray diffraction. The conformation of the salts within the platelets of the clay depended on the number of long alkyl chains of the salt. The thermal stability of the clays was also studied. The ammonium salts thermal decomposition was explained in light of their position within the organoclays.

Análise térmica aplicada à caracterização da sinvastatina em formulações farmacêuticas

Thermogravimetry (TG) and differential scanning calorimetry (DSC) are used in pharmaceutical studies for drugs characterization, purity, formulations compatibility, polymorphism identification, stability evaluation, and thermal decomposition of drugs and pharmaceutical formulations. Simvastatin showed fusion at 138.5 ºC and thermal stability up to 248 ºC. Simvastatin was incompatible with preservative excipient butylhydroxyanisole (BHA) performing a process of crystal amorphization. The drug showed morphological polymorphism, where it has the same unit cell but with different crystal habits according to the recrystallization solvent.

Síntese, caracterização e comportamento térmico de amidossulfonatos de terras raras

Hydrated compounds prepared in aqueous solution by reaction between amidosulfonic acid [H3NSO3] and suspensions of rare earth hydroxycarbonates [Ln2(OH)x(CO3)y.zH2O] were characterized by elemental analysis (% Ln, % N and % H), infrared spectroscopy (FTIR) and thermogravimetry (TG). The compounds presented the stoichiometry Ln(NH2SO3)3.xH2O (where x = 1, 5, 2.0 or 3.0). The IR spectra showed absorptions characteristic of H2O molecules and NH2SO3 groups. Degree of hydration, thermal decomposition steps and formation of stable intermediates of the type [Ln2(SO4)3] and (Ln2O2SO4), besides formation of their oxides, was determined by thermogravimetry.

Síntese, liofilização e caracterização de acetato de 57Fe(III)

Iron(III) acetate was synthesized by the reflux method using iron enriched in the 57Fe isotope and the compound processed by freeze-drying. The as-synthesized and freeze-dried acetates were characterized regarding their structural, thermal, vibrational and hyperfine properties. Similar diffractometric and spectroscopic results were found for both materials and also for an industrial acetate made with natural iron. However, the microstructures differed: the as-synthesized compound showed flake morphology with micrometric dimensions, whereas the freeze-dried showed flake morphology with sub-micrometric dimensions. The activation energies for thermal decomposition, calculated from the exothermic events occurring in differential scanning calorimetry measurements, were 100.9 kJ/mol (as-synthesized) and 114.7 kJ/mol (freeze-dried).

"Serpentes de Faraó": a história de uma brincadeira pirotécnica e sua aplicabilidade no ensino de princípios químicos básicos

Fun methodologies developed with alternative materials for teaching chemical reactions of carbon are interesting activities for discussing concepts of stoichiometry and thermochemistry. The decomposition of organic matter, CO2 production and coal formation can be demonstrated in the experiment "Pharaoh´s snake". This experiment is attractive since the simple combustion of sucrose generates a peculiar structure of coal. This paper proposes a simple methodology for making the sugar tablets used in the experiment and contextualizes the experimental observations with the chemical reaction of carbon which leads to coal and to the thermodynamics involving combustion processes.

Ni(II), Cu(II), AND Zn(II) COMPLEXES DERIVED FROM A NEW SCHIFF BASE 2-((Z)-(3-METHYLPYRIDIN-2- YLEIMINO)METHYL)PHENOL AND SYNTHESIS OF NANO SIZED METAL OXIDE PARTICLES FROM THESE COMPOUNDS

Synthesis, spectral identification, and magnetic properties of three complexes of Ni(II), Cu(II), and Zn(II) are described. All three compounds have the general formula [M(L)2(H2O)2], where L = deprotonated phenol in the Schiff base 2-((z)-(3-methylpyridin-2-yleimino)methyl)phenol. The three complexes were synthesized in a one-step synthesis and characterized by elemental analysis, Fourier transform infrared spectroscopy, electronic spectra, X-ray diffraction (XRD), and room temperature magnetic moments. The Cu(II) and Ni(II) complexes exhibited room temperature magnetic moments of 1.85 B.M. per copper atom and 2.96 B.M. per nickel atom. The X-band electron spin resonance spectra of a Cu(II) sample in dimethylformamide frozen at 77 K (liquid nitrogen temperature) showed a typical ΔMS = ± 1 transition. The complexes ([M(L)2(H2O)2]) were investigated by the cyclic voltammetry technique, which provided information regarding the electrochemical mechanism of redox behavior of the compounds. Thermal decomposition of the complexes at 750 ºC resulted in the formation of metal oxide nanoparticles. XRD analyses indicated that the nanoparticles had a high degree of crystallinity. The average sizes of the nanoparticles were found to be approximately 54.3, 30.1, and 44.4 nm for NiO, CuO, and ZnO, respectively.

Dehydration and volatilization non isothermic kinetic of the solid state aluminium 8-hydroxyquinolinate

Al(C9H6ON)3.2.5H2O was precipitated from the mixture of an aqueous solution of aluminium ion and an acid solution of 8-hydroxyquinoline, by increasing the pH value to 9.5 with ammonia aqueous solution. The TG curves in nitrogen atmosphere present mass losses due to dehydration, partial volatilisation (sublimation plus vaporisation) of the anhydrous compound followed by thermal decomposition with the formation of a mixture of carbonaceous and residues. The relation between sublimation and vaporisation depends on the heating rate used. The non isothermic integral isoconventional methods as linear equations of Ozawa-Flynn-Wall and Kissinger-Akahira-Sunose (KAS) were used to obtain the kinetic parameters from TG and DTA curves, respectively. Despite the fact that both dehydration and volatilisation reactions follow the linearity by using both methods, only for the volatilisation reaction the validity condition, 20<= E/RT<= 50, was verified.

Thermoanalytical study of purine derivatives compounds

Thermal methods of analysis are now used in a very large range of scientific investigations. In this work simultaneous thermogravimetry-differential thermal analysis (TG-DTA), X-Ray powder diffractometry and infrared spectroscopy were used to study the derivative compounds of purine, i. e. aminophylline, theophylline, caffeine and uric acid. The results led to informations about the thermal stability and thermal decomposition of these compounds.

Kinetic evaluation of the dehydration of Yb(III) Lu(III) and Y(III) 4-chlorobenzylidenepyruvate by thermogravimetry (TG)

The dehydration kinetic of Yb, Lu and Y 4-chlorobenzylidenepyruvate was studied by using thermogravimetry and the kinetics parameters obtained by Flynn and Wall method suggest that the dehydration step follows a first order mechanism. The activation energies calculated were 103.6, 96.6 and 97.2 kJ/mol and the lifetime considering the temperature of 31 and 101 º C for the dehydration of these compounds were 23, 26, 31 minutes and 0.6, 1.3 and 1.4 seconds, respectively. The results have similar values and suggest that the water is attached in the same way.