Aplicação da termogravimetria na determinação do teor de ferro em comprimidos: um estudo comparativo com a espectrofotometria

This study used the Thermogravimetry (TG) and molecular absorption spectroscopy in UV-visible region to determine the iron content in herbal medicinal ferrous sulfate used in the treatment of iron deficiency anemia. The samples were characterized by IR, UV, TG / DTG, DTA, DSC and XRD. The thermoanalytical techniques evaluated the thermal stability and physicochemical events and showed that the excipients interfere in the decomposition of the active ingredients. The results of thermogravimetry showed that the decomposition temperature of the active principle Fe2(SO4)3 (T = 602 °C) is higher as compared to samples of tablets (566 586 °C). In the DTA and DSC curves were observed exothermic and endo events for samples of medicines and active analysis. The infrared spectra identified key functional groups exist in all samples of active ingredients, excipients and compressed studied, such as symmetric and asymmetric stretching of OH, CH, S=O. The analysis by X-ray diffraction showed that all samples had crystallinity and the final residue showed peaks indicating the presence of silicon dioxide, titanium dioxide and talc that are excipients contained in pharmaceutical formulations in addition to iron oxide. The results obtained by TG to determine the iron content of the studied drugs showed a variance when compared with those obtained by theoretical and UV-visible, probably due to formation of a mixture of Fe2O3 and Fe2(SO4)3. In one tablet was obtained FE content of 15.7 % and 20.6 % for TG by UV-visible, the sample EF 2 was obtained as a percentage of 15.4 % and 21.0 % for TG by UV-visible . In the third SF samples were obtained a content of 16.1 % and 25.5 % in TG by UV-visible, and SF 4 in the percentage of TG was 16.7 % and 14.3 % UV-visible

Síntese e caracterização de redes metalorgânicas baseadas em zinco e ácidos benzenodicarboxílicos

Metal Organic Frameworks (MOFs) are supramolecular structures consisted of ions or metal clusters coordinated to organic ligands which are repeated in two or three dimensions. These structures have atracted much attention due to their properties such as low density, high specific surface area and large volume of pores. In this work, MOFs consisted of zinc clusters connected by ditopic ligands, terephthalic acid (1,4- H2BDC) or isophthalic acid (1,3-H2BDC) were synthesized. To obtain the proposed materials, different routes and synthetic parameters were tested, such as the molar ratio of the precursors, the addition of template molecules, the type of solvente, the addition of organic base or the type of a counter-ion of Zn salt. It was found that the variation of these parameters led to the formation of different metalorganic structures. The solids obtained were characterized by XRD, SEM and IR. For the samples identified as MOF- 5, it was verified that the structure was composed of both interpenetrated and non interpenetrated structures. These samples showed a low stability, becoming totally transformed into another structure within less than 72 hours. The addition of the nickel and/or cobalt was found to be a promissing method for increasing the stability of MOF- 5, which in this case, still remained unconverted to another structure even after 15 days of exposure to air. The samples prepared from 1,3-H2BDC were probably new, still unknown Metal Organic Frameworks

Preparo e caracterização de membranas de quitosana modificadas com poli (ácido acrílico)

The aim of this study was to generate an asymmetric biocompactible and biodegradable chitosan membrane modified by the contact with a poly(acrylic acid) solution at one of its sides at room temperature and 60◦C. The pure chitosan membrane, as well as the ones treated with poly(acrylic acid) were characterized by infrared spectroscopy (FTIRATR) at angles of 39◦, 45◦ and 60◦ , swelling capacity in water, thermal analysis (TG/DTG), scanning electronic microscopy (SEM) and permeation experiments using metronidazole at 0,1% and 0,2% as a model drug. The results confirmed the presence of ionic interaction between chitosan and poly(acrylic acid) by means of a polyelectrolyte complex (PEC) formation. They also showed that such interactions were more effective at 60◦C since this temperature is above the chitosan glass transition temperature wich makes the diffusion of poly(acrylic acid) easier, and that the two treated membranes were asymmetrics, more thermically stable and less permeable in relation to metronidazole than the pure chitosan membrane

Síntese e caracterização da ferrita de MnZn obtida pelo método dos citratos precursores

It was synthesized MnZn ferrite with general formulae Mn1-xZnxFe2O4 (mol%), 0,3 ≤ x ≤ 0,7 by using the citrate precursor method. The precursors decomposition was studied by thermogravimetric analysis (TGA), differential thermogravimetric analysis (DTG), differential thermal analysis (DTA) and Fourier transform infrared (FTIR) of powder calcined at 350ºC/3,5h. X-ray diffraction pattern (XRD) of samples was done from 350 to 1200ºC/2h using various atmospheres. The power calcined at 350ºC/3,5h formed spinel phase. It is necessary atmosphere control to avoid secondary phase such as hematite. From 900 to 1200ºC was obtained 90,66 and 100% of MnZn spinel ferrite phase, respectively. Analysis by dispersive energy scanning (EDS) at 350ºC shows high Mn and Zn dispersion, indicating that the diffusion process was homogeneous. Semi-quantitative analysis by EDS verified that despite the atmosphere control during calcinations at high temperatures (< 800ºC) occurred ZnO evaporation causing stoichiometric deviation. Vibrating sample magnetometer (VSM) measures show soft ferrite material characteristics with Hc from 6,5 x 10-3 to 11,1 x 10-2 T. Saturation magnetization (Ms) and initial permeability (µi) of MnZn spinel phase obtained, respectively, from 14,3 to 83,8 Am2/kg and 14,1 to 62,7 (Am2/kg)T

Caracterização estrutural de Perovskitas Lax-1AxCoO3 (x=0 e 0,2) ,dopadas com cálcio e bario, por espectroscopia de absorção de raios X (XAS).

In this work, the structures of LaCoO3, La0,8Ba0,2CoO3 and La0,8Ca0,2CoO3 perovskites were characterized as a function of temperature (LaCoO3 structure being analyzed only at room temperature). The characterization of these materials were made by X-Ray Absorption Spectroscopy (XAS), in the cobalt K-edge, taking into account the correlated Einstein model X-ray absorption fine structure (EXAFS). The first part of the absorption spectrum corresponded the X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS). These materials were prepared by the combustion method. The combustion products were calcinated at 900 0C, for 6 hours in air. Noted that the sample LaCoO3 at room temperature and samples doped with Calcium and Barium in the temperature range of 50 K to 298 K showed greater distortion to monoclinic symmetry with space group I2/a. However, the sample doped with barium at the temperatures 50 K, 220 K, and 260 K showed a slight distortion to rhombohedral symmetry with space group R-3c. The La0,8Ca0, 2CoO3 structure was few sensitive to temperature variation, showing a higher local distortion in the octahedron and a higher local thermal disorder. These interpretations were in agreement with the information electronic structural on the XANES region and geometric in the EXAFS region

Encapsulação de nanopartículas de magnetita em matriz de poli(metacrilato de metilacoácido metacrílico) por processo de polimerização em miniemulsão

Magnetic particles are systems with potential use in drug delivery systems, ferrofluids, and effluent treatment. In many situations, such as in biomedical applications, it is necessary to cover magnetic particles with an organic material, as polymers. In this work, magnetic particles were obtained through covering magnetite particles with poly(methyl methacrylate‐comethacrylic acid) via miniemulsion polymerization process. The resultant materials were characterized X‐ray diffraction (XRD), Fourier Transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), zeta potential (��) measurements and vibrating sample magnetometry (VSM). XRD results showed magnetite as the predominant cristalline phase in all samples and that cristallites had nanometric dimensions. Thermogravimetric analysis revealed an increase in polymer thermal stability as a result of magnetite encapsulation. TGA results showed also that the encapsulation efficiency was directly related to nanoparticles s hidrofobicity degree. VSM measurements showed that magnetic polymeric particles were superparamagnetic, so that they may be potentially used for magnetic (bio)separation

Reciclagem química de Polietileno utilizando Sílica Mesoporosa tipo SBA-15 avalizada por Termogravimetriae Espectrometria de Massas

The chemical recycling of polyolefins has been the focus of increasing attention owing potential application as a fuel and as source chemicals. The use of plastic waste contributes to the solution of pollution problems.The use of catalysts can enhance the thermal degradation of synthetic polymers, which may be avaliated by Themogravimetry (TG) and mass spectrometry (MS) combined techniques. This work aims to propose alternatives to the chemistry recycling of low-density polyethylene (LDPE) on mesoporous silica type SBA-15 and AlSBA-15.The mesoporous materials type SBA-15 and AlSBA-15 were synthesized through the hydrothermal method starting from TEOS, pseudobohemite, cloridric acid HCl and water. As structure template was used Pluronic P123. The syntheses were accomplished during the period of three days. The best calcination conditions for removal of the organic template (P123) were optimized by thermal analysis (TG/DTG) and through analyses of Xray diffraction (XRD), infrared spectroscopy (FT-IR), nitrogen adsorption and scanning electron microscopy (SEM) was verified that as much the hydrothermal synthesis method as the calcination by TG were promising for the production of mesoporous materials with high degree of hexagonal ordination. The general analysis of the method of Analog Scan was performed at 10oC/min to 500 oC to avoid deterioration of capillary with very high temperatures. Thus, with the results, we observed signs mass/charge more evident and, using the MID method, was obtained curve of evolution of these signals. The addition of catalysis produced a decrease in temperature of polymer degradation proportional to the acidity of the catalyst. The results showed that the mesoporous materials contributed to the formation of compounds of lower molecular weight and higher value in the process of catalytic degradation of LDPE, representing an alternative to chemical recycling of solid waste

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

Desenvolvimento de metodologia capaz de detectar e quantificar misturas de corantes em sucos artificiais em pó

Foi desenvolvido um método para detectar e quantificar misturas de corantes em sucos artificiais em pó fabricados no Brasil, de diferentes marcas e sabores. Foram estudados 6 corantes artificiais: amarelo tartrazina, amarelo crepúsculo, vermelho ponceau 4R, vermelho bordeaux S, vermelho 40 e azul brilhante presentes de forma unitária ou em misturas nos sucos com sabores laranja, tangerina, maracujá, abacaxi, limão e uva. A identificação dos corantes nas amostras foi feita através da comparação com os espectros dos padrões, utilizando-se a análise por infravermelho médio e pelos respectivos valores de absorção máxima nos comprimentos de onda relativos aos padrões e valores de referência na literatura. Também foram estudados os perfis de decomposição térmica por termogravimetria, termogravimetria derivada e calorimetria diferencial exploratória dos corantes e dos sucos em pó, sendo determinados os teores de umidade, de matéria orgânica e de cinzas. O teor de umidade encontrado não ultrapassou 4% para todas as amostras de suco analisadas. Com relação ao teor de matéria orgânica obteve-se para 57% dos sucos analisados um teor médio de 51,3% e para 43% das outras amostras obteve-se uma média de 67,2 %. Os resultados obtidos para o teor de cinzas indicaram que 29% das amostras apresentaram um teor de 26,7% para esse parâmetro enquanto 71% das amostras apresentaram um teor de cinzas de 46,4%. Os resultados obtidos por análise térmica mostraram-se adequados considerando-se que para obter os resultados pelo método tradicional há um investimento maior de tempo, de pessoal envolvido e de material, além da proteção ao meio ambiente. Para a análise por espectroscopia de absorção molecular foi proposta uma equação simplificada para a determinação de cada corante na mistura utilizando-se a lei de Beer. Para validação, empregou-se a espectroscopia de absorção molecular no visível, onde foi investigada a influência dos interferentes (TiO2 e açúcar) presentes nas amostras de sucos, os testes de fotodegradação e a avaliação do efeito do pH. Para quantificação tomou-se como referência 512 amostras sintéticas contendo um e dois corantes (1,5625 a 25,000 mg L-1) para obtenção das curvas analíticas que foram aplicadas à análise dos sucos em pó. Os resultados indicaram que o teor máximo do amarelo crepúsculo foi encontrado nos sucos com os sabores laranja, tangerina e manga que correspondeu a 25,6% da ingestão diária aceitável (para ser ultrapassada corresponderia a ingestão de 4 copos). O teor máximo encontrado para o amarelo tartrazina nos sucos foi para o sabor maracujá que correspondeu a 8,5% da ingestão diária aceitável, (para ser alcançado corresponderia a ingestão de 12 copos). O método proposto foi testado e validado com sucesso para amostras de sucos em pó sendo de simples execução e de rapidez na obtenção dos resultados

Obtenção de polímeros graftizados de quitosana e estudo das propriedades físico-químicas para aplicação na indústria do petróleo

Chitosan is a biopolymer derived from the shells of crustaceans, biodegradable, inexpensive and renewable with important physical and chemical properties. Moreover, the different modifications possible in its chemical structure generate new properties, making it an attractive polysaccharide owing to its range of potential applications. Polymers have been used in oil production operations. However, growing concern over environmental constraints has prompted oil industry to search for environmentally sustainable materials. As such, this study sought to obtain chitosan derivatives grafted with hydrophilic (poly(ethylene glycol), mPEG) and/or hydrophobic groups (n-dodecyl) via a simple (one-pot) method and evaluate their physicochemical properties as a function of varying pH using rheology, small-angle Xray scattering (SAXS), dynamic light scattering (DLS) and zeta potential. The chitosan derivatives were prepared using reductive alkylation under mild reaction conditions and the chemical structure of the polymers was characterized by nuclear magnetic resonance (1H NMR) and CHN elemental analysis. Considering a constant mPEG/Chitosan molar ratio on modification of chitosan, the solubility of the polymer across a wide pH range (acidic, neutral and basic) could only be improved when some of the amino groups were submitted to reacetylation using the one-pot method. Under these conditions, solubility is maintained even with the simultaneous insertion of n-dodecyl. On the other hand, the solubility of derivatives obtained only through mPEG incorporation using the traditional methodology, or with the ndodecyl group, was similar to that of its precursor. The hydrophilic group promoted decreased viscosity of the polymer solutions at 10 g/L in acid medium. However, at basic pH, both viscosity and thermal stability increased, as well as exhibited a pronounced pseudoplastic behavior, suggesting strong intermolecular associations in the alkaline medium. The SAXS results showed a polyelectrolyte behavior with the decrease in pH for the polymer systems. DLS analyses revealed that although the dilute polymer solutions at 1 g/L and pH 3 exhibited a high density of protonated amino groups along the polymer chain, the high degree of charge contributed significantly to aggregation, promoting increased particle size with the decrease in pH. Furthermore, the hydrophobic group also contributed to increasing the size of aggregates in solution at pH 3, whereas the hydrophilic group helped reduce their size across the entire pH range. Nevertheless, the nature of aggregation was dependent on the pH of the medium. Zeta potential results indicated that its values do not depend solely on the surface charge of the particle, but are also dependent on the net charge of the medium. In this study, water soluble associative polymers exhibit properties that can be of great interest in the petroleum industry

Desenvolvimento de catalisadores bifuncionais de óxido de zircônio modificado por óxidos de tungstênio e molibdênio contendo platina para a reação de isomerização de n-parafinas

Bifunctional catalysts based on zircon oxide modified by tungsten (W = 10, 15 and 20 %) and by molybdenum oxide (Mo= 10, 15 e 20 %) containg platinum (Pt = 1%) were prepared by the polymeric precursor method. For comparison, catalysts the tungsten base was also prepared by the impregnation method. After calcinations at 600, 700 and 800 ºC, the catalysts were characterized by X-ray diffraction, fourier-transform infrared spectroscopy, thermogravimetric and differential thermal analysis, nitrogen adsorption and scanning electron microscopy. The profile of metals reduction was determined by temperature programmed reduction. The synthesized catalysts were tested in n-heptane isomerization. X-ray diffractogram of the Pt/WOx-ZrO2 and Pt/MoOx-ZrO2 catalysts revealed the presence of tetragonal ZrO2 and platinum metallic phases in all calcined samples. Diffraction peaks due WO3 and ZrO2 monoclinic also were observed in some samples of the Pt/WOx-ZrO2 catalysts. In the Pt/MoOx-ZrO2 catalysts also were observed diffraction peaks due ZrO2 monoclinic and Zr(MoO4)2 oxide. These phases contained on Pt/WOx-ZrO2 and Pt/MoOx-ZrO2 catalysts varied in accordance with the W or Mo loading and in accordance with the calcination temperature. The infrared spectra showed absorption bands due O-W-O and W=O bonds in the Pt/WOx-ZrO2 catalysts and due O-Mo-O, Mo=O and Mo-O bonds in the Pt/MoOx-ZrO2 catalysts. Specific surface area for Pt/WOx-ZrO2 catalysts varied from 30-160 m2 g-1 and for the Pt/MoOx-ZrO2 catalysts varied from 10-120 m2 g-1. The metals loading (W or Mo) and the calcination temperature influence directly in the specific surface area of the samples. The reduction profile of Pt/WOx-ZrO2 catalysts showed two peaks at lower temperatures, which are attributed to platinum reduction. The reduction of WOx species was evidenced by two reduction peak at high temperatures. In the case of Pt/MoOx-ZrO2 catalysts, the reduction profile showed three reduction events, which are attributed to reduction of MoOx species deposited on the support and in some samples one of the peak is related to the reduction of Zr(MoO4)2 oxide. Pt/WOx-ZrO2 catalysts were active in the n-heptane isomerization with high selectivity to 3-methyl-hexane, 2,3- dimethyl-pentane, 2-methyl-hexane among other branched hydrocarbons. The Pt/MoOx-ZrO2 catalysts practically didn't present activity for the n-heptane isomerization, generating mainly products originating from the catalytic cracking

Influência do pré-aquecimento na adaptação marginal de dois materiais seladores de fóssulas e fissuras, analisada através de tomografia de coerência ótica

Among the non-invasive techniques employed in the prevention of caries highlights the sealing pits and fissures which is a conservative maneuver, in order to obliterate them to protect them from attack acid bacteria. Influenced by the studies of pre-heating composite resin, which has experienced great improvement in some of their physical properties, this study aimed to evaluate in vitro the superficial and internal marginal adaptation of different materials and sealants in pre-heating or not. A total of 40 extracted human third molars (n=10) that had their occlusal surfaces prepared to receive sealant. We tested two types of sealing materials: resin sealant (Fluoroshield) and low-viscosity resin (Permaflo), where 50% of previously received heated material and the other half received sealant material at room temperature. All samples were subjected to thermal cycling and pH, simulating a cariogenic oral environment, and later were analyzed appliance OCT (optical coherence tomography). The images obtained alterations were recorded and analyzed statistically. Change was considered as the emergence of bubbles, gaps and cracks in the sealant. Comparisons of the same material, assessing the fact that it is not sealed or preheated material, as well as comparisons between different materials subjected to the same temperature were carried out. The nonparametric Tukey test was used (p < 0,05). The results showed that there was statistically significant difference between both the materials analyzed, as between the situations in which the sealant material was submitted (preheated or not). On the issue of marginal adaptation and internal surface, seen through Optical coherence tomography, may suggest that there is a difference between the use of one type or another of the sealing material analyzed, with superiority attributed to resin Permaflo compared to sealant Fluroshield, telling is the same for the different techniques used

The influence of sour taste and cold temperature in pharyngeal transit duration in patients with stroke

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

Caracterização tectono-estratigráfica da sequência transicional na sub-bacia de Sergipe

This thesis deals with the tectonic-stratigraphic evolution of the Transitional Sequence in the Sergipe Sub-basin (the southern segment of the Sergipe-Alagoas Basin, Northeast Brazil), deposited in the time interval of the upper Alagoas/Aptian stage. Sequence boundaries and higher order internal sequences were identified, as well as the structures that affect or control its deposition. This integrated approach aimed to characterize the geodynamic setting and processes active during deposition of the Transitional Sequence, and its relations with the evolutionary tectonic stages recognized in the East Brazilian Margin basins. This subject addresses more general questions discussed in the literature, regarding the evolution from the Rift to the Drift stages, the expression and significance of the breakup unconformity, the relationships between sedimentation and tectonics at extensional settings, as well as the control on subsidence processes during this time interval. The tectonic-stratigraphic analysis of the Transitional Sequence was based on seismic sections and well logs, distributed along the Sergipe Sub-basin (SBSE). Geoseismic sections and seismic facies analysis, stratigraphic profiles and sections, were compiled through the main structural blocks of this sub-basin. These products support the depositional and tectonic-stratigraphic evolutionary models built for this sequence. The structural analysis highlighted similarities in deformation styles and kinematics during deposition of the Rift and Transitional sequences, pointing to continuing lithospheric extensional processes along a NW trend (X strain axis) until the end of deposition of the latter sequence was finished by the end of late Aptian. The late stage of extension/rifting was marked by (i) continuous (or as pulses) fault activity along the basin, controling subsidence and creation of depositional space, thereby characterizing upper crustal thinning and (ii) sagstyle deposition of the Transitional Sequence at a larger scale, reflecting the ductile stretching and thinnning of lower and sub crustal layers combined with an increasing importance of the thermal subsidence regime. Besides the late increments of rift tectonics, the Transitional Sequence is also affected by reactivation of the border faults of SBSE, during and after deposition of the Riachuelo Formation (lower section of the Transgressive Marine Sequence, of Albian age). It is possible that this reactivation reflects (through stress propagation along the newlycreated continental margin) the rifting processes still active further north, between the Alagoas Sub-basin and the Pernambuco-Paraíba Basin. The evaporitic beds of the Transitional Sequence contributed to the development of post-rift structures related to halokinesis and the continental margin collapse, affecting strata of the overlying marine sequences during the Middle Albian to the Maastrichtian, or even the Paleogene time interval. The stratigraphic analysis evidenced 5 depositional sequences of higher order, whose vertical succession indicates an upward increase of the base level, marked by deposition of continental siliciclastic systems overlain by lagunar-evaporitic and restricted marine systems, indicating that the Transitional Sequence was deposited during relative increase of the eustatic sea level. At a 2nd order cycle, the Transitional Sequence may represent the initial deposition of a Transgressive Systems Tract, whose passage to a Marine Transgressive Sequence would also be marked by the drowning of the depositional systems. At a 3rd order cycle, the sequence boundary corresponds to a local unconformity that laterally grades to a widespread correlative conformity. This boundary surface corresponds to a breakup unconformity , being equivalent to the Pre-Albian Unconformity at the SBSE and contrasting with the outstanding Pre-upper Alagoas Unconformity at the base of the Transitional Sequence; the latter is alternatively referred, in the literature, as the breakup unconformity. This Thesis supports the Pre-Albian Unconformity as marker of a major change in the (Rift-Drift) depositional and tectonic setting at SBSE, with equivalent but also diachronous boundary surfaces in other basins of the Atlantic margin. The Pre-upper Alagoas Unconformity developed due to astenosphere uplift (heating under high lithospheric extension rates) and post-dates the last major fault pulse and subsequent extensive block erosion. Later on, the number and net slip of active faults significantly decrease. At deep to ultra deep water basin segments, seaward-dipping reflectors (SDRs) are unconformably overlain by the seismic horizons correlated to the Transitional Sequence. The SDRs volcanic rocks overly (at least in part) continental crust and are tentatively ascribed to melting by adiabatic decompression of the rising astenospheric mantle. Even though being a major feature of SBSE (and possibly of other basins), the Pre-upper Alagoas Unconformity do not correspond to the end of lithospheric extension processes and beginning of seafloor spreading, as shown by the crustal-scale extensional structures that post-date the Transitional Sequence. Based on this whole context, deposition of the Transitional Sequence is better placed at a late interval of the Rift Stage, with the advance of an epicontinental sea over a crustal segment still undergoing extension. Along this segment, sedimentation was controled by a combination of thermal and mechanical subsidence. In continuation, the creation of oceanic lithosphere led to a decline in the mechanical subsidence component, extension was transferred to the mesoceanic ridge and the newly-formed continental margin (and the corresponding Marine Sequence) began to be controlled exclusively by the thermal subsidence component. Classical concepts, multidisciplinary data and new architectural and evolutionary crustal models can be reconciled and better understood under these lines

Avaliação da eficiência da técnica de obturação pela compressão hidrùlica vertical após instrumentação automatizada

The purpose of this study was to evaluate through radiographic and microscopic analysis the efficiency of the filling techniques by vertical hidraulic compression after the root canal mechanical instrumentation in vitro as well to evaluate the marginal apical leakage through macroscopic and microscopic analysis. Thirty human mandibular molars were used , they were divided on three groups, these were subdivided on six subgroups with five specimens each, come down to 106 root canals filled. Initially, the teeth were instrumented with Profile system series 29 and filled with two ways: single accessory cone or single cone associated with gutta-percha secundary cone, with Fill Canal sealer or Sealer 26. Completed the filling, the teeth were coated with araldit and finger -nail polish except for the apical 2 mm and dried for 3 hours, thep radiographs were taken of the teeth in orto and disto-radiai directions. Next, the coronal seal was carried out with composite resin photopolymerized and with their process of making impermeable. Teeth of positive controls were used without araldit and finger-nail polish whereas the negative controls were used with total coat of araldit and finger-nail polish. The specimens were placed in 2% Methylene Blue dye for 24 hours and thermocycled for 7 days. Afterwards, sections were made of each tooth at mesial and distal roat, after this the teeth were radiographed at buccolíngual direction for a macroscopic analysis and at buccolingual and mesiodistal directions for assessment of the marginal apical leakage. Cross sections were made 3 mm to 3mm since the tooth apice. The sections obtained for each group were observed with a stereomicroscope to evaluate the quality of the root canal filling and the marginal apical leakage. The results showed that: In the four techniques the marginal dye leakage was present in the apical third; in all groups the quality of the root canal filling in the radiography was better at mesial root canal and the single cone technique showed inefficient when only a single distal root canal was present. In the radiographic evaluation the best quality of the root canal filling was observed in the 1A group (single accessory cone + FiIl Canal), as in the mesial root as in the distal root wich Shcwed twe root canals: when the distaI root had only one canal. the best result was showed by 28 group (single accessory cone associated with secundary cone + Fill Canal) In the macroscopic analysis of longitudinal !eaKage (outside surface). less leakage was showed as In the mesial root as in the distal root in the negative control group (3) followed 2A group (single accessory cone + Sealer 26). When the microscopic analysis of tranversal leakage of both roots (inside surface) was carried out. the groups that showed less dye leakage were the negative control (38) followed the 28 group (single acessory cone associated with secundary cone + Sealer 26). The homogeneity o filling was best noted in the 1 A group (.single accessoty cone + Fill Canal). The groups that showed less dye penetration in the tranversal leakage (total area) were negative control (3B) and 2B