Desenvolvimento de um compósito de espuma rígida de poliuretana de mamona e fibras de sisal para isolação térmica

The search for sustainable technologies that can contribute to reduce energy consumption is a great challenge in the field of insulation materials. In this context, composites manufactured from vegetal sources are an alternative technology. The principal objectives of this work are the development and characterization of a composite composed by the rigid polyurethane foam derived from castor oil (commercially available as RESPAN D40) and sisal fibers. The manufacture of the composite was done with expansion controlled inside a closed mold. The sisal fibers where used in the form of needlepunched nonwoven with a mean density of 1150 g/m2 and 1350 g/m2. The composite characterization was performed through the following tests: thermal conductivity, thermal behavior, thermo gravimetric analysis (TG/DTG), mechanical strength in compression and flexural, apparent density, water absorption in percentile, and the samples morphology was analyzed in a MEV. The density and humidity percentage of the sisal fiber were also determined. The thermal conductivity of the composites was higher than the pure polyurethane foam, the addition of nonwoven sisal fibers will become in a higher level of compact foam, reducing empty spaces (cells) of polyurethane, inducing an increase in k value. The apparent density of the composites was higher than pure polyurethane foam. In the results of water absorption tests, was seen a higher absorption percent of the composites, what is related to the presence of sisal fibers which are hygroscopic. From TG/DTG results, with the addition of sisal fibers reduced the strength to thermal degradation of the composites, a higher loss of mass was observed in the temperature band between 200 and 340 °C, related to urethane bonds decomposition and cellulose degradation and its derivatives. About mechanical behavior in compression and flexural, composites presented a better mechanical behavior than the rigid polyurethane foam. An increase in the amount of sisal fibers induces a higher rigidity of the composites. At the thermal behavior tests, the composites were more mechanically and thermally resistant than some materials commonly used for thermal insulation, they present the same or better results. The density of nonwoven sisal fiber had influence over the insulation grade; this means that, an increaser in sisal fiber density helped to retain the heat

Efeitos da radiação uv, temperatura e vapor aquecido nos compósitos poliméricos: monitoramento, instabilidade estrutural e fratura

The application of composite materials and in particular the fiber-reinforced plastics (FRP) has gradually conquered space from the so called conventional materials. However, challenges have arisen when their application occurs in equipment and mechanical structures which will be exposed to harsh environmental conditions, especially when there is the influence of environmental degradation due to temperature, UV radiation and moisture in the mechanical performance of these structures, causing irreversible structural damage such as loss of dimensional stability, interfacial degradation, loss of mass, loss of structural properties and changes in the damage mechanism. In this context, the objective of this thesis is the development of a process for monitoring and modeling structural degradation, and the study of the physical and mechanical properties in FRP when in the presence of adverse environmental conditions (ageing). The mechanism of ageing is characterized by controlled environmental conditions of heated steam and ultraviolet radiation. For the research, it was necessary to develop three polymer composites. The first was a lamina of polyester resin reinforced with a short glass-E fiber mat (representing the layer exposed to ageing), and the other two were laminates, both of seven layers of reinforcement, one being made up only of short fibers of glass-E, and the other a hybrid type reinforced with fibers of glass-E/ fibers of curaua. It should be noted that the two laminates have the lamina of short glass-E fibers as a layer of the ageing process incidence. The specimens were removed from the composites mentioned and submitted to environmental ageing accelerated by an ageing chamber. To study the monitoring and modeling of degradation, the ageing cycles to which the lamina was exposed were: alternating cycles of UV radiation and heated steam, a cycle only of UV radiation and a cycle only of heated steam, for a period defined by norm. The laminates have already undergone only the alternating cycle of UV and heated steam. At the end of the exposure period the specimens were subjected to a structural stability assessment by means of the developed measurement of thickness variation technique (MTVT) and the measurement of mass variation technique (MMVT). Then they were subjected to the mechanical tests of uniaxial tension for the lamina and all the laminates, besides the bending test on three points for the laminates. This study was followed by characterization of the fracture and the surface degradation. Finally, a model was developed for the composites called Ageing Zone Diagram (AZD) for monitoring and predicting the tensile strength after the ageing processes. From the results it was observed that the process of degradation occurs Abstract Raimundo Nonato Barbosa Felipe xiv differently for each composite studied, although all were affected in certain way and that the most aggressive ageing process was that of UV radiation, and that the hybrid laminated fibers of glass-E/curaua composite was most affected in its mechanical properties

Morfologia em alta resolução espacial de estrelas de tipo Mira e R Corenae Borealis

Mira and R Coronae Borealis (R CrB) variable stars are evolved objects surrounded by circumstellar envelopes (CSE) composed of the ejected stellar material. We present a detailed high-spatial resolution morfological study of the CSE of three stars: IRC+10216, the closest and more studied Carbon-Rich Mira; o Ceti, the prototype of the Mira class; and RY Sagitarii (RY Sgr), the brightest R CrB variable of the south hemisphere. JHKL near-infrared adaptive optics images of IRC+10216 with high dynamic range and Vband images with high angular resolution and high depth, collected with the VLT/NACO and VLT/FORS1 instruments, were analyzed. NACO images of o Ceti were also analyzed. Interferometric observations of RY Sgr collected with the VLTI/MIDI instrument allowed us to explore its CSE innermost regions (»20 40 mas). The CSE of IRC+10216 exhibit, in near-infrared, clumps with more complex relative displacements than proposed in previous studies. In V-band, the majority of the non-concentric shells, located in the outer CSE layers, seem to be composed of thinner elongated shells. In a global view, the morphological connection between the shells and the bipolar core of the nebulae, located in the outer layers, together with the clumps, located in the innermost regions, has a difficult interpretation. In the CSE of o Ceti, preliminar results would be indicating the presence of possible clumps. In the innermost regions (.110 UA) of the CSE of RY Sgr, two clouds were detected in different epochs, embedded in a variable gaussian envelope. Based on a rigorous verification, the first cloud was located at »100 R¤ (or »30 AU) from the centre, toward the east-north-east direction (modulo 180o) and the second one was almost at a perpendicular direction, having aproximately 2£ the distance of the first cloud. This study introduces new constraints to the mass-loss history of these kind of variables and to the morphology of their innermost CSE regions

Investigação da estabilidade térmica e das propriedades elétricas do TiO2 em função da dopagem com Ce(SO4)2

The metalic oxides have been studies due to differents applications as materials semiconductor in solar cells, catalysts, full cells and, resistors. Titanium dioxide (TiO2) has a high electric conductivity due to oxygen vacancies. The Ce(SO4)2.2H2O doped samples TiO2 and TiO2 pure was obtained sol-gel process, and characterized by X-ray diffractometry,thermal analysis, and impedance spectroscopy. The X-ray diffraction patterns for TiO2 pure samples shows at 700°C anatase phase is absent, and only the diffraction peaks of rutile phase are observed. However, the cerium doped samples only at 900°C rutile in the phase present with peaks of cerium dioxide (CeO2). The thermal analysis of the TiO2 pure and small concentration cerium doped samples show two steps weight loss corresponding to water of hydration and chemisorbed. To larger concentration cerium doped samples were observed two steps weight loss in the transformation of the doped cerium possible intermediate species and SO3. Finally, two steps weight loss the end products CeO2 and SO3 are formed. Analyse electric properties at different temperatures and concentration cerium doped samples have been investigated by impedance spectroscopy. It was observed that titanium, can be substituted by cerium, changing its electric properties, and increased thermal stability of TiO2 anatase structure

Estudo do comportamento térmico e da luminescência de filmes de quitosana com os íons Eu3+ e Tb3+

Films of chitosan with trivalent lanthanides ions Eu3+ and Tb3+ were respectively prepared in the ratio of 3:1 m/m (chitosan: lanthanide) and 6:1 m/m (chitosan: lanthanide). There were no formations of films in a ratio of 1:1 m/m (chitosan: lanthanides). The films of chitosan with the Tb3+ ion have the same transparent appearance than the pure chitosan films. The film of chitosan with Eu3+ ion has a muddy appearance. These films present good resistance to tear. The appearance of the compounds prepared in ratio 1:1m/m is a white powder. The films and compounds of chitosan were characterized by Elementary Analysis (CHN), Thermal Analysis (TG/DTG) and Spectroscopy of Luminescence. The CHN analysis was made only for compounds prepared in ratio 1:1m/m, suggesting that these compounds possess the formula QUILn.6H2O, where QUI = Chitosan and Ln = Lanthanide. The results of the curves TG/DTG indicated that there are strong interactions between Eu3+ or Tb3+ and chitosan, causing a lesser lost of mass in the films. The luminescence analysis showed that the films of chitosan with the ions Eu3+ and Tb3+ present emissions in the region of the visible one, with bands of the chitosan and of the Eu3+ ion. The luminescence analysis of the compounds of chitosan with the Eu3+ and Tb3+ ions suggest that the chitosan does not transfer into energy to the ions lanthanides, however the chemical neighborhood around of the ion lanthanides breaks the selection rules and, conseqüently the 4f-4f transitions of the lanthanide ions are observed

Reavaliação da eficiência de óleo de coco saponificado e de sua microemulsão como inibidores de corrosão em uma célula eletroquímica

An interesting development in surfactants science and technology is their application as corrosion inhibitors, since they act as protective films over anodic and cathodic surfaces. This work aims to investigate the efficiency of saponified coconut oil (SCO) as corrosion inhibitor and of microemulsified system (SCO + butanol + kerosene oil + distilled water), in saline medium, using an adapted instrumented cell, via techniques involving linear polarization resistance (LPR) and mass loss coupons (MLC). For this, curves of efficiency versus SCO concentration (ranging between 0 and 75 ppm) have been constructed. According to the obtained results, the following efficiency levels were reached with OCS: 98% at a 75 ppm concentration via the LPR method and 95% at 75 ppm via the MLC method. The microemulsified system, for a concentration of 15 ppm of SCO, obtained maximum inhibition of 97% (LPR) and 93% (MLC). These data indicate that it is possible to optimize the use of SCO in similar applications. Previous works have demonstrated that maximal efficiencies below 90% are attained, typically 65% as free molecules and 77% in microemulsified medium, via the LPR method in a different type of cell. Therefore, it can be concluded that the adapted instrumented cell (in those used methods) showed to be an important tool in this kind of study and the SCO was shown effective in the inhibition of the metal

Síntese, caracterização e aplicação de MCM-41 funcionalizado com diisopropilamina no processo de adsorção do dióxido de carbono

Emissions of CO2 in the atmosphere have increased successively by various mechanisms caused by human action, especially as fossil fuel combustion and industrial chemical processes. This leads to the increase in average temperature in the atmosphere, which we call global warming. The search for new technologies to minimize environmental impacts arising from this phenomenon has been investigated. The capture of CO2 is one of the alternatives that can help reduce emis ions of greenhouse gases. The CO2 can be captured through the process of selective adsorption using adsorbents for this purpose. Were synthesized by hydrothermal method, materials of the type MCM-41 and Al-MCM-41 in the molar ratio Si / Al equal to 50. The synthesis of gels were prepared from a source of silicon, sodium, water and aluminum in the case of Al-MCM-41. The period of synthesis of the materials was 5 days in autoclave at 100°C. After that time materials were filtered, washed and dried in greenhouse at 100 º C for 4 hours and then calcined at 450 º C. Then the calcined material was functionalized with the Di-isopropylamine (DIPA) by the method of wet impregnation. We used 0.5 g of material mesopores to 3.5 mL of DIPA. The materials were functionalized in a closed container for 24 hours, and after this period were dried at brackground temperature for 2 hours. Were subsequently subjected to heat treatment at 250°C for 1 hour. These materials were used for the adsorption of CO2 and were characterized by XRD, FT-IR, BET / BJH, SEM, EDX and TG / DTG. Tests of adsorption of CO2 was carried out under the following conditions: 100 mg of adsorbent, temperature of 75°C under flow of 100 mL/min of CO2 for 2 hours. The desorption of CO2 was carried out by thermogravimetry from ambient temperature to 900ºC under flow of 25 mL min of He and a ratio of 10ºC/min. The difratogramas X-ray for the synthesized samples showed the characteristic peaks of MCM-41, showing that the structure of it was obtained. For samples functionalized there was a decrease of the intensities of these peaks, with a consequent reduction in the structural ordering of the material. However, the structure was preserved mesopores. The adsorption tests showed that the functionalized MCM-41 is presented as a material promising adsorbent, for CO2 capture, with a loss of mass on the desorption CO2 of 7,52%, while that in Al-MCM- 41 functionalized showed no such loss

Obtenção de novos sistemas nanoautoemulsificantes a partir do óleo das sementes de Azadirachta indica A Juss e suas aplicações como inibidores de corrosão

Corrosion is a natural process that causes progressive deterioration of materials, so, reducing the corrosive effects is a major objective of development of scientific studies. In this work, the efficiency of corrosion inhibition on a AISI 1018 carbon steel of the nanoemulsion system containing the oil of the seeds of Azadirachta indica A. Juss (SNEOAI) was evaluated by the techniques of linear polarization resistance (LPR) and weight loss (CPM), a instrumented cell. For that, hydroalcoholic extract of leaves of A. indica (EAI) was solubilized in a nanoemulsion system (SNEOAI) of which O/W system (rich in aqueous phase). This nanoemulsion system (tested in different concentrations) was obtained with oil from the seeds of this plant species (OAI) (oil phase), dodecylammonium chloride (DDAC) (surfactant), butanol (cosurfactant) and water, using 30 % of C/T (cosurfactant/surfactant), 0.5 % of oil phase and 69.5 % of aqueous phase, and characterized by surface tension, rheology and droplet sizes. This systems SNEOAI and SNEOAI-EAI (nanoemulsion containing hydroalcoholic extract - EAI) showed inhibition efficiencies in corrosive environment in saline (1 %), for the method of LPR with significant value of 70.58 % (300 ppm) to SNEOAI, 74.17 % (100 ppm) and 72.51 % (150 ppm) to SNEOAI-EAI. The best efficiencies inhibitions were observed for the method of CPM with 85.41 % for the SNEOAI (300 ppm) and 83.19 % SNEOAI-EAI (500 ppm). The results show that this formulation could be used commercially for use as a corrosion inhibitor, this research contributed to the biotechnological applicability of Azadirachta indica, considering the large use of this plant species rich in limonoids (tetranortriterpenoids), especially azadirachtin

Avaliação oxidativa do biodiesel de pinhão manso em diferentes processos de purificação

The objective of this study was to analyze the oxidative stability of biodiesel from jatropha obtained from different purification processes, three wet processes with different drying (in a vacuum oven, conventional oven and in anhydrous sodium sulfate) and dry (purification with magnesium silicate adsorbent). Raw materials of different qualities (jatropha crop ancient and recent crop) were used. The Jatropha oil was extracted by mechanical extraction and refined. The Jatropha biodiesel was obtained by the transesterification reaction in ethyl route using alkaline catalysis. The biodiesel samples were characterized by analysis of water content, carbon residue, Absorption Spectroscopy in the Infrared Region and Thermogravimetry. Thermogravimetric curves of purified PUsv* PUsq* and had higher initial decomposition temperatures, indicating that the most stable, followed by samples PU* and PUSC*. Besides the sample SP* is a smaller initial temperature, confirming the sample without purification to be less thermally stable. The percentage mass loss of the purified samples showed conversion of about 98.5%. The results of analyzes carbon residue and infrared suggested that contamination by impurities is the main factor for decreased oxidative stability of biodiesel. The oxidative stability was assessed from periodic monitoring, using the techniques of Rancimat, peroxide index, acid value and Pressurized Differential Scanning Calorimetry. Samples of biodiesel from jatropha which showed better oxidative stability were of the best quality raw material and wet scrubbing: PUsq* with dry chemical, using anhydrous sodium sulfate and PUsv* with vacuum drying, which had oxidative stability 6 hours in Rancimat time 0 days, within the limits established by the Technical Regulation No. 4/2012 of the ANP, without the addition of antioxidant, suggesting that these procedures the least influence on the oxidative stability of biodiesel

Caracterização e aplicação de vermicultura natural e quimicamente modificada na adsorção de azul de metileno

Chemical modification of clays has been extremely studied in the search for improvements of their properties for use in various areas, such as in combating pollution by industrial effluents and dyes. In this work, the vermiculite was chemically modified in two ways, characterized and evaluated the adsorption of methylene blue dye. First was changed with the addition of a surfactant (hexadecyltrimethylammonium bromide, BHTA) making it an organophilic clay and then by adding an acid (HCl) by acid activation. Some analyzes were performed as X-ray fluorescence (FRX), X-ray diffraction (DRX), adsorption isotherms of methylene blue dye, infrared (FTIR) , scanning electron microscopy (SEM), thermal gravimetric analysis and spectroscopy energy dispersive (EDS). Analysis by FRX of natural vermiculite indicates that addition of silicon and aluminum, clay presents in its structure the magnesium, calcium and potassium with 16 % organic matter cations. The DRX analyzes indicated that the organic vermiculite was an insertion of the surfactant in the space between the lamellae, vermiculite and acid partial destruction of the structure with loss of crystallinity. The adsorption isotherms of methylene blue showed that there was a significant improvement in the removal of dye to the vermiculite with the addition of cationic surfactant hexadecyltrimethylammonium bromide and treatment with acid using HCl 2 mol/L. In acid vermiculites subsequently treated with surfactant, the adsorption capacity increased with respect to natural vermiculite, however was much lower compared vermiculite modified with acid and surfactant separately. Only the acidic vermiculite treated with surfactant adjusted to the Langmuir model. As in the infrared spectrometry proved the characteristics of natural vermiculite. In the organic vermiculite was observed the appearance of characteristic bands of CH3, CH2, and (CH3)4N. Already on acid vermiculite, it was realized a partial destruction with decreasing intensity of the characteristic band of vermiculite that is between 1074 and 952 cm-1. In the SEM analysis, it was observed that there was partial destruction to the acid treatment and a cluster is noted between the blades caused by the presence of the surfactant. The TG shows that the higher mass loss occurs at the beginning of the heating caused by the elimination of water absorbed on the surface between layers. In the organic vermiculite also observed a loss of mass between 150 and 300 °C caused decomposition of the alkylammonium molecules (surfactants)

Estudo cinético da degradação térmica e catalítica de petróleo pesado usando Al-MCM-41

The mesoporous nanostructured materials have been studied for application in the oil industry, in particular Al-MCM-41, due to the surface area around 800 to 1.000 m2 g-1 and, pore diameters ranging from 2 to 10 nm, suitable for catalysis to large molecules such as heavy oil. The MCM-41 has been synthesized by hydrothermal method, on which aluminum was added, in the ratio Si/Al equal to 50, to increase the generation of active acid sites in the nanotubes. The catalyst was characterized by X-ray diffraction (XRD), surface area by the BET method and, the average pore volume BJH method using the N2 adsorption, absorption spectroscopy in the infrared Fourier Transform (FT-IR) and determination of surface acidity with application of a probe molecule - n-butylamine. The catalyst showed well-defined structural properties and consistent with the literature. The overall objective was to test the Al-MCM-41 as catalyst and thermogravimetric perform tests, using two samples of heavy oil with API º equal to 14.0 and 18.5. Assays were performed using a temperature range of 30-900 ° C and heating ratios (β) ranging from 5, 10 and 20 °C min-1.The aim was to verify the thermogravimetric profiles of these oils when subjected to the action of the catalyst Al- MCM-41. Therefore, the percentage ranged catalyst applied 1, 3, 5, 10 and 20 wt%, and from the TG data were applied two different kinetic models: Ozawa-Flynn-Wall (OFW) and Kissinger-Akahrira-Sunose (KAS).The apparent activation energies found for both models had similar values and were lower for the second event of mass loss known as cracking zone, indicating a more effective performance of Al-MCM-41 in that area. Furthermore, there was a more pronounced reduction in the value of activation energy for between 10 and 20% by weight of the oil-catalyst mixture. It was concluded that the Al-MCM-41 catalyst has applicability in heavy oils to reduce the apparent activation energy of a catalyst-oil system, and the best result with 20% by weight of Al-MCM-41

Síntese, caracterização e estudo fotofísico de complexos de 4,4- diaminoestilbeno-2,2-dissulfonato com íons lantanídeos

This is a work involving fundamental studies of chemistry where the synthesis and structural characterization, as well as a possible future application of these new compounds as luminescent sensors or sunscreen agents, complexes with 4,4 diaminostilbene-2,2-disulfonic (DSD) and trivalent lanthanide ions La3+, Nd3+, Eu3+, Gd3+ and Yb3+, were synthesized in the ratio of 3 mmol: 1 mmol (DSD: lanthanides). The complexes obtained with these ions were present in powder form and were characterized by complexometric titration with EDTA CHN Elemental analysis, molecular absorption spectroscopy in the ultraviolet region, the absorption spectroscopy in the infrared, thermal analysis (TG / DTG), Nuclear Magnetic Resonance - NMR 1H and Luminescence Spectroscopy. The complexometric titration and CHN analysis, confirmed the TG / DTG which suggest that these complexes have the following general chemical formulas: [La2(C14H12S2O6N2)2(H2O)2Cl2].7H2O,[Nd2(C14H12S2O6N2)2(H2O)2Cl2].6H2O,[Eu2(C14 H12S2O6N2)2(H2O)2Cl2].7H2O,[Gd2(C14H12S2O6N2)2(H2O)2Cl2].4H2O e [Yb2(C14H12S2O6N2)2(H2O)2].6H2O. The disappearance of the bands in the infrared spectrum at 2921 cm-1 and 2623 cm-1 and the displacement of the bands in the spectra of the amine complex indicate that the lanthanide ion is coordinated to the oxygen atoms and the sulfonate groups of the nitrogens amines, suggesting the formation of the dimer. The disappearance of the signal and the displacement signal SO3H amines in the 1H NMR spectrum of this complex are also indicative coordination and dimer formation. The Thermogravimetry indicates that the DSD is thermally stable in the range of 40º to 385°C and their complexes with lanthanide ions exhibit weight loss between 4 and 5 stages. The Uv-visible spectra indicated that the DSD and complexes exhibit cis isomers. The analysis of luminescence indicates that the complexes do not exhibit emission in the region of the lanthanides but an intense emission part of the binder. This is related to the triplet states of the ligand, which are in the lowest energy state emitting lanthanide ions, and also the formation of the dimer that suppress the luminescence of ion Eu3+. The formation of dimer was also confirmed by calculating the europium complex structure using the model Hamiltonian PM6 and Sparkle

Trissoralen um medicamento de baixa dosagem: estudos termoanalíticos da compatibilidade do fármaco-excipientes e determinação de parâmetros de qualidade para cápsulas magistrais

The trioxsalen (Tri) is a low-dose drug used in the treatment of psoriasis and other skin diseases. The aim of the study was applying the thermal analysis and complementary techniques for characterization, evaluation of the trioxsalen stability and components of manipulated pharmaceutical formulations. The thermal behavior of the Tri by TG/DTG-DTA in dynamic atmosphere of synthetic air and nitrogen showed the same profile with a melting peak followed by a volatilization-related event. From the curves TG / DTG is observed a single stage of mass loss. By heating the drug in the stove at temperatures of 80, 240 and 260 °C, it had no change in chemical structure through the techniques of XRD, HPLC, MIR, OM and SEM. From the non-isothermal and isothermal TG kinetic studies was possible to calculate the activation energy and reaction order for the Tri. The drug showed good thermal stability. Studies on drug-excipient compatibility showed interaction of trissoralen with sodium lauryl sulfate 1:1. There was no interaction with aerosol, pregelatinized starch, sodium starch glycolate, cellulose, croscarmellose sodium, magnesium stearate, lactose and mannitol.The characterization of three trioxsalen formulations at concentrations of 2.5, 5, 7.5, 10, 12.5 and 15 mg was performed by DSC, TG / DTG, XRD, NIR and MIR. The PCA classification method based on spectral data from the NIR and MIR of trissoralen formulations allows successful differentiation into three groups. The formulation 3 was the one that best showed analytical profile with the following composition of aerosil excipients, pre-gelatinized starch and cellulose. The activation energy of the volatilization process of the drug was determined in binary mixtures and formulation 3 through fitting and isoconversional methods. The binary mixture with sodium starch glycolate and lactose showed differences in kinetic parameters compared to the drug isolated. The thermoanalytical techniques (DSC and TG / DTG) were shown to be promising methodologies for quantifying trioxsalen obtained by the linearity, selectivity, no use solvents, without sample preparation, speed and practicality.

Determinação da energia de ativação e pureza de medicamentos de referência, genérico e similar utilizando técnicas termoanalíticas

In this work, the reference drugs, generic and similar to the active ingredients acetylsalicylic acid, paracetamol, captopril, hydrochlorothiazide and mebendazole were purchased from local pharmacies and studied by thermogravimetry (TG) and Differential Scanning Calorimetry (DSC). Thermal decomposition was assessed to obtain from the Ozawa method the activation energy in inert atmosphere (nitrogen), using three different heating ratios (5, 10 and 20 o C min-1). The pharmaceutical formulation of the AAS reference was the one who presented different from the others (generic and similar) Thermogravimetric profile indicating likely interaction between the active ingredient and excipients. Was observed at the heating rate of the inverse temperature that no linearity of the data, ie, there was no correlation between the percentage of mass loss and the activation energy involved in the thermal decomposition of the pharmaceutical formulation of the AAS reference log graph. The analysis by differential scanning calorimetry was performed in nitrogen atmosphere with a heating rate of 10 ° C min-1. In the analysis of these same drugs, the data curves found on the melting point were, except for hydrochlorothiazide, are consistent with the literature. Hydrochlorothiazide presented a melting point well below that found in the literature, which may be justified due to the interaction of the active ingredient with the excipient lactose. In the study of purity, using the Van't Hoff equation, the reference drugs hydrochlorothiazide and mebendazole reference generic and showed similar impurity content below the limit established that this equation must be greater than 2.5 mol%

Aplicação da destilação simulada por cromatografia gasosa e da termogravimetria para a avaliação da influência da redução do teor de enxofre sobre as propriedades físico-químicas do óleo diesel

One of the main problems related to the use of diesel as fuel is the presence of sulfur (S) which causes environmental pollution and corrosion of engines. In order to minimize the consequences of the release of this pollutant, Brazilian law established maximum sulfur content that diesel fuel may have. To meet these requirements, diesel with a maximum sulfur concentration equal to 10 mg/kg (S10) has been widely marketed in the country. However, the reduction of sulfur can lead to changes in the physicochemical properties of the fuel, which are essential for the performance of road vehicles. This work aims to identify the main changes in the physicochemical properties of diesel fuel and how they are related to reduction of sulfur content. Samples of diesel types S10, S500 and S1800 were tested according with the methods of the American Society for Testing and Materials (ASTM). The fuels were also characterized by thermogravimetric analysis (TG) and subjected to physical distillation (ASTM D86) and simulated distillation gas chromatography (ASTM D2887). The results showed that the reduction of sulfur turned the fuel lighter and fluid, allowing a greater applicability to low temperature environments and safer for transportation and storage. Through the simulated distillation data was observed that decreasing sulfur content resulted in higher initial boiling point temperatures and the decreasing of the boiling temperature of the medium and heavy fractions. Thermogravimetric analysis showed a loss event mass attributed to volatilization or distillation of light and medium hydrocarbons. Based on these data, the kinetic behavior of the samples was investigated and it was observed that the activation energies (Ea) did not show significant changes throughout conversion. Considering the average of these energies, the S1800 had the highest Ea during the conversion and the S10 the lowest values