Caracterização térmica (TG/DTG, DTA, DSC, DSC-fotovisual) de Hormônios bioidênticos (estriol estradiol)

Bioidentical hormones are defined as compounds that have exactly the same chemical and molecular structure as hormones that are produced in the human body. It is believed that the use of hormones may be safer and more effective than the non-bioidentical hormones, because binding to receptors in the organism would be similar to the endogenous hormone. Bioidentical estrogens have been used in menopausal women, as an alternative to traditional hormone replacement therapy. Thermal data of these hormones are scarce in literature. Thermal analysis comprises a group of techniques that allows evaluating the physical-chemistry properties of a drug, while the drug is subjected to a controlled temperature programming. The thermal techniques are used in pharmaceutical studies for characterization of drugs, purity determination, polymorphism identification, compatibility and evaluation of stability. This study aims to characterize the bioidentical hormones estradiol and estriol through thermal techniques TG/DTG, DTA, DSC, DSC-photovisual. By the TG curves analysis was possible to calculated kinetic parameters for the samples. The kinetic data showed that there is good correlation in the different models used. For both estradiol and estriol, was found zero order reaction, which enabled the construction of the vapor pressure curves. Data from DTA and DSC curves of melting point and purity are the same of literature, showed relation with DSC-photovisual results. The analysis DTA curves showed the fusion event had the best linearity for both hormones. In the evaluation of possible degradation products, the analysis of the infrared shows no degradation products in the solid state

Contribuições sobre estudos térmicos (TG/DTG, DTA, DSC e DSC-Fotovisual) da rifampicina e seus principais produtos de degradação

Since its synthesis over 48 years rifampicin has been extensively studied. The literature reports the characterization of thermal events for rifampicin in nitrogen atmosphere, however, no characterization in synthetic air atmosphere. This paper aims to contribute to the thermal study of rifampicin through thermal (TG / DTG, DTA, DSC and DSC - FOTOVISUAL ) and non-thermal (HPLC, XRPD , IR - FTIR , PCA) and its main degradation products ( rifampicin quinone , rifampicin N-oxide 3- formylrifamicin). Rifampicin study was characterized as polymorph form II from techniques DSC, IR and XRPD. TG curves for rifampicin in synthetic air atmosphere showed higher thermal stability than those in N2, when analyzed Ti and Ea. There was characterized as overlapping events melting and recrystallization under N2 with weight loss in the TG curve, suggesting concomitant decomposition. Images DSCFotovisual showed no fusion event and showed darkening of the sample during analysis. The DTA curve in synthetic air atmosphere was visually different from DTA and DSC curves under N2, suggesting the absence of recrystallization and melting or presence only decomposition. The IV - FTIR analysis along with PCA analysis and HPLC and thermal data suggest that rifampicin for their fusion is concomitant decomposition of the sample in N2 and fusion events and recrystallization do not occur in synthetic air atmosphere. Decomposition products studied in an air atmosphere showed no melting event and presented simultaneously to the decomposition initiation of heating after process loss of water and / or solvent, varying the Ti initiating events. The Coats - Redfern , Madsudhanan , Van Krevelen and Herwitz - Mertzger kinetic parameters for samples , through the methods of OZAWA , in an atmosphere of synthetic air and / or N2 rifampicin proved more stable than its degradation products . The kinetic data showed good correlation between the different models employed. In this way we contribute to obtaining information that may assist studies of pharmaceutical compatibility and stability of substances

Índices de obesidade central e fatores de risco cardiovascular na síndrome dos ovários policísticos

Fundamento: A obesidade abdominal apresenta elevada prevalência em mulheres com síndrome dos ovários policísticos (SOP) e está associada a um aumento do risco cardiovascular. Objetivo: Verificar a acurácia da circunferência da cintura (CC), da relação cintura-quadril (RCQ), da relação cinturaestatura (RCEST) e do índice de conicidade (índice C), no que se refere à detecção de fatores de risco cardiovascular (FRCV) em mulheres com SOP. Métodos: Por meio de estudo transversal, foram alocadas 102 mulheres (26,5 ± 5 anos) com diagnóstico de SOP, de acordo com o consenso de Rotterdam. O colesterol total (CT), os triglicerídeos (TG), o LDL-colesterol (LDL-C), o HDLcolesterol (HDL-C), a glicemia de jejum, a glicemia após teste oral de tolerância à glicose (TOTG) e a pressão arterial (PA) foram avaliados em todas as pacientes, além das variáveis antropométricas. Resultados: A relação cintura-estatura foi o marcador que apresentou correlações positivas significativas com o maior número de FRCV (PA, TG e glicemia após TOTG), destacando-se ainda a correlação negativa com HDL-C. Todos os marcadores antropométricos avaliados se correlacionaram positivamente com PA, enquanto CC e RCQ apresentaram correlação positiva também com TG. No tocante à acurácia para detecção de FRCV, os indicadores antropométricos considerados apresentaram taxas de sensibilidade superiores a 60%, com destaque para a RCEST, que apresentou sensibilidade superior a 70%. Conclusão: A RCEST demonstrou ser o indicador antropométrico com a melhor acurácia para a predição de FRCV. Nesse sentido, propõe-se a inclusão desse parâmetro de fácil mensuração na avaliação clínica para o rastreamento de mulheres com SOP e FRCV----------------------ABSTRACT Background: Women with polycystic ovary syndrome (PCOS) present a high prevalence of abdominal obesity, which is associated with an increased cardiovascular risk. Objective: To verify the accuracy of the waist circumference (WC), waist-to-hip ratio (WHR), waist-to-height ratio (WHtR) and the conicity index (CI) in the detection of cardiovascular risk factors (CVRF) in women with PCOS. Methods: The present transversal study allocated 102 women (26.5 ± 5 years) with a diagnosis of PCOS, according to the Rotterdam criteria. Total cholesterol (TC), triglycerides (TG), LDL-cholesterol (LDL-C), HDL-cholesterol (HDL-C), fasting glucose, glucose after the oral glucose tolerance test (OGTT) and blood pressure (BP) were evaluated in all patients, in addition to the anthropometric variables. Results: The WHtR was the marker that presented significant positive correlations with the highest number of CVRF (BP, TG and post-OGTT glucose), whereas there was a negative correlation with HDL-C. All the evaluated anthropometric markers were positively correlated with BP, whereas WC and WHR also presented a positive correlation with TG. Regarding the accuracy for the detection of CVRF, the anthropometric markers presented a sensibility > 60%, especially the WHtR, which had a sensibility > 70%. Conclusion: The WHtR showed to be the most accurate anthropometric indicator for the prediction of CVRF. In this sense, we propose the inclusion of this easily-measured parameter in the clinical assessment for the screening of women with PCOS and CVRF

Influência do lodo de ETE na massa para fabricação de cerâmica vermelha

The WTP produce many kinds of residue on your treatment stages, but the sludge is the more problematic from the final disposition point view. The actual rate of residue production deriving from technological evolution and the crescent population needs prevents the subtle equilibrium generation between consumption and recycling/reuse, creating problems of pollution resulting from inappropriate management of residues. Thus, is necessary achieve a new equilibrium between the grow from raw materials and energy and the residue generation. This equilibrium should be achieved by technical and economic feasibility of environmental supported models through recycling and reuse. The red ceramic industry stand out in residue absorption question as raw material due their clay mass heterogeneity, constituted by clay minerals and non-clay minerals with wide mineralogical variation, allowing residue inclusion which act like plastic or non-plastic materials, contributing to retain heavy metals contained in residues in the vitreous mass formed during the burning of the ceramic bodies. This work propose the study of the influence of incorporation of 25 wt.% sludge from wastewater treatment plant, according preliminary results, in the mass to produce ceramic bodies. The raw materials was characterized through chemical composition analyses by XRF, mineralogical analyses by XRD, thermal analyses by TG and DTA, Atterberg limits and thermodilatometry. Subsequently was composed the mass with 75 wt.% of clay and 25 wt.% of dried wastewater sludge from UFRN WWTP. Samples with 6,0 x 2,0 x 0,5 cm was produced with unidirectional compacting under pressure of 20MPa and burned in temperatures between 950 and 1,200ºC. After fired, the ceramic bodies have been submitted to physical and mechanical analyses through the measure of firing shrinkage, water absorption, density, apparent porosity and flexural strength; crystallographic analyses through XRD and microstructure analyses by SEM. The technological properties obtained was satisfactory to production of roof tiles with 25 wt.% at 1,200 ºC, but the production of others products at lower temperatures was not feasible

Síntese, caracterização e estudo da regeneração do silicoaluminofosfato-11 (SAPO-11)

heterogeneous catalyst such as a silicoaluminophosphate, molecular sieve with AEL (Aluminophosphate eleven) structure such as SAPO-11, was synthesized through the hydrothermal method starting from silica, pseudoboehmite, orthophosphoric acid (85%) and water, in the presence of a di-isopropylamine organic template. For the preparation of SAPO-11 in a dry basis it was used as reactants: DIPA; H3PO4; SiO4; Pseudoboehmite and distilled water. The crystallization process occurred when the reactive hydrogel was charged into a vessel and autoclaved at 200ºC for a period of 72 hours under autogeneous pressure. The obtained material was washed, dried and calcined to remove the molecular sieves of DIPA. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), infrared spectroscopy (FT-IR), nitrogen adsorption (BET) and thermal analysis (TG/DTG). The acidic properties were determined using adsorption of nbutylamine followed by programmed thermodessorption. This method revealed that SAPO-11 shows an acidity that ranges from weak to moderate. However, a small quantity of strong acid sites could be detected there. The deactivation of the catalysts was conducted by artificial coking followed by the cracking of the n-hexane in a fixed bed with a continuous flow micro-reactor coupled on line to a gas chromatograph. The main products obtained were: ethane, propane, isobutene, n-butane, n-pentane and isopentane. The Vyazovkin (model-free) kinetics method was used to determine the regeneration and removal of the coke

Síntese, caracterização e cinética da decomposição térmica dos materiais cerâmicos PrMO3 (M = Ni ou Co)

In this work have been studied the preparation, characterization and kinetic study of decomposition of the polymerizing agent used in the synthesis under non-isothermal condition ceramics PrMO3 of general formula (M = Co and Ni). These materials were obtained starting from the respective metal nitrates, as a cations source, and making use of gelatin as polymerizing agent. The powders were calcined at temperatures of 500°C, 700°C and 900°C and characterized by X-ray Diffraction (XRD), Thermogravimetric Analysis (TG / DTG/ DTA), Infrared Spectroscopy (FTIR), Temperature Programmed Reduction (TPR) and Scanning Electron Microscopy (SEM). The perovskite phase was detected in all the X-rays patterns. In the infrared spectroscopy observed the oxide formation as the calcination temperature increases with the appearance of the band metal - oxygen. The images of SEM revealed uniform distribution for the PrCoO3 and particles agglomerated as consequence of particle size for PrNiO3. From the data of thermal analysis, the kinetics of decomposition of organic matter was employed using the kinetics methods called Model Free Kinetics and Flynn and Wall, in the heating ratios 10, 20 and 30° C.min-1 between room temperature and 700°C. Finally, been obtained the values of activation energy for the region of greatest decomposition of organic matter in samples that were determined by the degree of conversion (α)

Adição de cascalho de perfuração da bacia potiguar em argilas para uso em materiais cerâmicos: influência da concentração e temperatura de queima.

One of waste produced on large scale during the well drilling is the gravel drilling. There are techniques for the treatment of the same, but there isn t consensus on what are the best in terms of economic and environmental. One alternative for disposal of this waste and objective of this paper is the incorporation and immobilization of gravel clay matrix to assess their technological properties. The Raw Materials used were characterized by the following techniques: Chemical Analysis by X-ray fluorescence (XRF), mineralogical analysis by X-ray Diffraction (XRD), Grain Size Analysis (FA) and Thermal Analysis by Thermogravimetry (TG) and thermodiferential (DTA). After characterizing, samples were formulated in the following percentages: 0, 5, 10, 15, 25, 50, 75, 100% (weight) of gravel drilling, then the pieces were pressed, dried (110 ° C) and sintered at temperatures of 850, 950 and 1050 ° C. After sintering, samples were tested for water absorption, linear shrinkage, flexural strength, porosity, density, XRD and test color. The results concluded that the incorporation of gravel drilling is a viable possibility for solid masonry bricks and ceramic blocks manufacture at concentrations and firing temperature described here. Residue incorporation reduces an environmental problem, the cost of raw materials for manufacture of ceramic products

Obtenção de nanopartículas de hexaferrita de bário pelo método pechini

In this study barium hexaferrite was (general formulae BaFe12O19) was synthesized by the Pechini method under different conditions of heat treatment. Precursors like barium carbonate and iron nitrate were used. These magnetic ceramic, with magnetoplumbite type structure, are widely used as permanent magnet because of its excellent magnetic properties, such as: high Curie temperature, good magnetic anisotropy, high coercivity and corrosion resistance. The samples were characterized by thermal analysis (DTA and TG), X- ray Diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM) end Vibrating sample Magnetometer (VSM). The results confirm the expected phase, which was reinforced according to our analysis. A single phase powder at relatively high temperatures with particle sizes around 100 nm was obtained. The characteristic magnetic behavior one of the phases has been noted (probably superparamagnetic material), while another phase was identified as a ferrimagnetic material. The ferrimagnetic phase showed vortex configuration with two central and slightly inclined plateaus. In general, increase of heat treatment temperature and time, directly influenced the technological properties of the samples

Aproveitamento da fibra do epicarpo do coco babaçu em compósito com matriz epóxi: estudo do efeito do tratamento da fibra

Nowadays the environmental issues are increasingly highlighted since the future of humanity is dependent on the actions taken by man. Major efforts are being expended in pursuit of knowledge and alternatives to promote sustainable development without compromising the environment. In recent years there has been a marked growth in the development of reinforced composite fiber plants, as an alternative for economic and ecological effects, especially in the substitution of synthetic materials such as reinforcement material in composites. In this current study the chemical- physical or (thermophysics )characteristics of the babassu coconut fiber, derived from the epicarp of the fruit (Orbignyda Phalerata), which the main constituents of the fiber: Klason lignin, insoluble, cellulose, holocellulose, hemicellulose and the content of ash and moisture will be determined. A study was conducted about the superficial modification of the fibers of the epicarp babassu coconut under the influence of chemical treatment by alkalinization, in an aqueous solution of NaOH to 2.5% (m/v) and to 5.0% to improve the compatibility matrix / reinforcement composite with epoxy matrix. The results of the changes occurred in staple fibers through the use of the techniques of thermogravimetric analyses (TG) and differential scanning calorimetry (DSC). The results found on thermal analysis on samples of fiber without chemical treatment (alkalinities), and on fiber samples treated by alkalinization show that the proposed chemical treatment increases the thermal stability of the fibers and provides a growth of the surface of area fibers, parameters that enhance adhesion fiber / composite. The findings were evaluated and compared with published results from other vegetable fibers, showing that the use of babassu coconut fibers has technical and economic potential for its use as reinforcement in composites

Desevolvimento de nanocompósitos de poli(metacrilato de metila)/argila processados por mistura no estado fundido

Poly(methyl methacrylate)/clay nanocomposites were prepared by melt mixing using a montmorillonite-rich clay (MMT). The clay in natura was treated with acrylic acid to facilitate the dispersion in the polymer matrix. A masterbatch of PMMA/clay was prepared and combined with the pure PMMA and then subjected to extrusion process using singlescrew and twin-screw extruders followed by injection. Nanocomposites were processed with clay contents of 1, 3, 5 and 8 wt.%. The effect of shear processing on the morphology of the nanocomposites was evaluated by XRD, SEM and TEM. Thermal and mechanical properties of the nanocomposites were investigated through TGA, DSC, HDT, VICAT, tensile and impact tests, to evaluate the effect of the addition of clay to the PMMA matrix. Flammability tests were also conducted to investigate the effect of the addition of clay on the flame retardation properties. SEM images of the nanocomposites indicated the presence of clay agglomerates, which resulted in the reduction of properties such as thermal stability, mechanical strength and impact resistance, and increased the rate of burning for materials processed by both extrusion routes

Influência do uso de combustíveis alternativos na síntese por combustão via microondas para a produção de materiais cerâmicos com estrutura espinélio

The development and study of detectors sensitive to flammable combustible and toxic gases at low cost is a crucial technology challenge to enable marketable versions to the market in general. Solid state sensors are attractive for commercial purposes by the strength and lifetime, because it isn t consumed in the reaction with the gas. In parallel, the use of synthesis techniques more viable for the applicability on an industrial scale are more attractive to produce commercial products. In this context ceramics with spinel structure were obtained by microwave-assisted combustion for application to flammable fuel gas detectors. Additionally, alternatives organic-reducers were employed to study the influence of those in the synthesis process and the differences in performance and properties of the powders obtained. The organic- reducers were characterized by Thermogravimetry (TG) and Derivative Thermogravimetry (DTG). After synthesis, the samples were heat treated and characterized by Fourier Transform Infrared Spectroscopy (FTIR), X-ray Diffraction (XRD), analysis by specific area by BET Method and Scanning Electron Microscopy (SEM). Quantification of phases and structural parameters were carried through Rietveld method. The methodology was effective to obtain Ni-Mn mixed oxides. The fuels influenced in obtaining spinel phase and morphology of the samples, however samples calcined at 950 °C there is just the spinel phase in the material regardless of the organic-reducer. Therefore, differences in performance are expected in technological applications when sample equal in phase but with different morphologies are tested

Desenvolvimento de pastas de cimento flexíveis para poços de petróleo submetidos à injeção de vapor utilizando látex do tipo SBR

Novel cementing materials formulations containing flexible polymeric admixtures have been studied aiming at improving the mechanical behavior of oil well cement slurries submitted to steam injection. However, research activities in this sector are still under development. The steam injected directly into the well causes casing dilation, which after a reduction in temperature, tends to return to its original dimensions, resulting in crack formation and hydraulic isolation loss of the well, which will result in shortening of well life. In this scenario, the objective of the present study was to evaluate the mechanical behavior of Portland-based slurries containing SBR latex, applied in oil well cementing of wells submitted to steam injection. Were formulated slurries with densities of 1.797 g/cm3 (15.0 lb/Gal) and 1.869 g/cm3 (15.6 lb/Gal), containing admixtures with a latex concentration of 0; 66.88; 133.76; 200.64 and 267.52 L/m3 (0, 0.5, 1.0, 1.5 and 2.0 gpc). Tests including rheology, fluid loss control, thickening time, API compressive strength and splitting tensile strength, beyond steam injection simulation. Microstrutural characteristics of the slurries were also performed (XRD, TG, FTIR and SEM). The results showed that increasing the polymer concentration increased in the rheological properties and fluid loss, and a decrease in the elasticity modulus of the cement slurries. The results obtained showed that the slurries can be applied in cementing operations of oil wells submitted to steam injection.

Síntese e caracterização de óxidos de cério e cobalto obtidos por gel-combustão e Pechini aplicados às reações de oxidação de n-hexano

Oxide type spinel AB2O4 presents structure adjusted for application in the automobile industry. The spinel of cobalt has many practical applications had its excellent physical and chemical properties such as catalyst in hydrocarbon oxidation reaction. The CeO2 has been used in many of these processes because it assigns to a material with excellent thermal resistance and mechanics, high capacity of oxygen stockage (OSC) among others properties. This work deals with the synthesis, characterization and catalytic application of spinel of cobalt and CeO2 with fluorita structure, obtained for method of Pechini and method of Gel-Combustion. The process of Pechini, the puff was obtained at 300 ºC for 2 h in air. In the process of Gel-Combustion the approximately at 350 ºC material was prepared and burnt for Pyrolysis, both had been calcined at 500 ºC, 700 ºC, 900 ºC and 1050 ºC for 2 h in air. The materials of the calcinations had been characterized by TG/DTA, electronic microscopy of sweepings (MEV), spectroscopy of absorption in the infra-red ray (FTIR) and diffraction of X-rays (DRX). The obtained material reaches the phase oxide at 450 oC for Pechini method and 500 °C for combustion method. The samples were submitted catalytic reaction of n-hexane on superficies of materials. The reactor function in molar ration of 0, 85 mol.h-1.g-1 and temperature of system was 450 °C. The sample obtained for Pechini and support in alumine of superficial area of 178,63 m2.g-1 calcined at 700 ºC, give results of catalytic conversions of 39 % and the sample obtained for method of gel-combustion and support in alumina of 150 mesh calcined at 500 ºC result 13 % of conversion. Both method were selective specie C1

Síntese e impregnação de peneiras moleculares Fe MCM-41 derivada de sílica da casca do arroz

The mesoporous molecular sieves of the MCM-41 and FeMCM-41 type are considered promissory as support for metals used as catalysts in oil-based materials refine processes and as adsorbents for environmental protection proposes. In this work MCM-41 and FeMCM41 were synthesized using rice husk ash - RHA as alternative to the conventional silica source. Hydrothermal synthesis was the method chosen to prepare the materials. Pre-defined synthesis parameters were 100°C for 168 hours, later the precursor was calcinated at 550°C for 2 hours under nitrogen and air flow. The sieves containing different proportions of iron were produced by two routes: introduction of iron salt direct synthesis; and a modification post synthesis consisting in iron salt 1 % and 5% impregnation in the material followed by thermal decomposition. The molecular sieves were characterized by X ray diffraction XRD, Fourier transform infrared spectroscopy FT-IR, X ray fluorescence spectroscopy XFR, scanning electronic microscopy SEM, specific surface area using the BET method, Termogravimetry TG. The kinetic model of Flynn Wall was used with the aim of determining the apparent activation energy of the surfactant remove (CTMABr) in the MCM- 41 porous. The analysis made possible the morphology characterization, identifying the presence of hexagonal structure typical for mesoporous materials, as well as observation of the MCM41 and iron of characteristic bands.

Adsorção de Pb(II) utilizando adsorvente composto por montmorilonita e dolomita

The destructive impact of improper disposal of heavy metals in the environment increases as a direct result of population explosion, urbanization and industrial expansion and technological developments. Argil are potential materials for adsorption of inorganic and the pelletization of it is required for use in adsorptive columns of fixed bed. The low cost and the possibility of regeneration makes these materials attractive for use in the purification process, capable of removing inorganic compounds in contaminated aquatic environments. In this work was made pellets of a mixture of dolomite and montmorillonite by wet agglomeration, in different percentages. The removal of Pb (II) was investigated through experimental studies, and was modeled by kinetic models and isotherms of adsorption. The materials were characterized using the techniques of XRD, TG / DTA, FT-IR, and surface area by BET method. The results showed the adsorption efficiency of the contaminant by the composite material studied in synthetic solution. The study found that the adsorption follows the Langmuir model, and the kinetics of adsorption follows the model of pseudosecond order