35 resultados para Modulated Temperature Differential Scanning Calorimetry
Resumo:
The search for new sources of environmentally friendly energy is growing every day. Among these alternative energies, biodiesel is a biofuel that has had prominence in world production. In Brazil, law 11.097, determine that all diesel sold in the country must be made by mixing diesel/biodiesel. The latter called BX, , where X represents the percent volume of biodiesel in the diesel oil, as specified by the ANP. In order to guarantee the quality of biodiesel and its mixtures, the main properties which should be controlled are the thermal and oxidative stability. These properties depend mainly of the chemical composition on the raw materials used to prepare the biodiesel. This dissertation aims to study the overall thermal and oxidative stability of biodiesel derived from cotton seed oil, sunflower oil, palm oil and beef tallow, as well as analyze the properties of the blends made from mineral oil and biodiesel in proportion B10. The main physical-chemical properties of oils and animal fat, their respective B100 and blends were determined. The samples were characterized by infrared and gas chromatography (GC). The study of thermal and oxidative stability were performed by thermogravimetry (TG), pressure differential scanning calorimeter (PDSC) and Rancimat. The obtained biodiesel samples are within the specifications established by ANP Resolution number 7/2008. In addition, all the blends and mineral diesel analyzed presented in conformed withthe ANP Regularion specifications number 15/2006. The obtained results from TG curves data indicated that the cotton biodiesel is the more stable combustible. In the kinetic study, we obtained the following order of apparent activation energy for the samples: biodiesel from palm oil > sunflower biodiesel > tallow biodiesel > cotton biodiesel. In terms of the oxidative stability, the two methods studied showed that biodiesel from palm oil is more stable then the tallow. Within the B100 samples studied only the latter were tound to be within the standard required by ANP resolution N° 7. Testing was carried out according to the EN14112. This higher stability its chemical composition
Resumo:
This study aimed to apply, thermogravimetriy /derivative Thermogravimetriy (TG/DTG), differential scanning calorimetry (DSC), Differential Thermal Analysis (DTA), to conduct a comparative study on drug reference, generic and whose active principles are similar captopril hydrochlorothiazide, ampicillin, paracetamol, aspirin and mebendazole sold in local pharmacies. Samples of the active ingredients and dosage forms were also characterized by absorption infrared spectroscopy (IR), X-ray diffraction (XRD) and microscopy scanning electron (SEM). The TG / DTG curves showed a general similarity in the thermal behavior of the samples, but also showed the influence of excipients on the thermal stability. The DSC curve of the generic base hydrochlorothiazide showed no peak on the fusion of the drug due to interference of lactose as a diluent, which causes interaction with the active principle causing their degradation before the merger. The DSC curves of the drugs consisting of paracetamol showed reproducibility at the melting point of the active and the other thermal events. The DSC result of binary mixtures involving captopril / magnesium stearate and mebendazole/magnesium stearate showed possible interactions or incompatibilities evidenced by the displacement of the melting point of both drugs. The other mixtures showed no change. The infrared spectra presented were very similar, indicating the presence of functional groups characteristic of the constituents of the samples. The X-ray diffraction showed peaks indicative of crystalline structure of the active ingredients as well as some of the ingredients in the formulation of the drug and the micrographs indicate a general heterogeneity in the size distribution of particles in the samples
Resumo:
In recent years, studies about the physicochemical properties of mixed oxides, call attention of the scientific community, properties like as piezoelectricity, photoluminescence, or applications as catalysts, arise in these compounds, when their chemical compositions are modified, in this context some routes are employed in the synthesis of these materials, among which can be cited these methods: ceramic, combustion, co-precipitation, Pechini or polymeric precursor method, hydrothermal, sol-gel; these routes are divided into traditional routes or chemical routes. In this work were synthesized oxides with variable composition, from the thermal decomposition of titanium, cobalt, nickel and praseodymium nitrilotriacetates. The nitrilotriacetates were characterized by IR Spectroscopy (FTIR), Thermogravimetric (TG/ DTG) and Differential Scanning Calorimetry (DSC), while oxides have been characterized by X-ray diffraction (XRD), Spectrofluorimetry and IR Spectroscopy (FTIR). From FTIR data, it was demonstrated that the displacement of the band corresponding to the carboxylate group (νCOOH) at 1712 cm-1, present in nitrilotriacetic acid (H3NTA), for 1680-1545 cm-1, these stretches are characteristics of coordinated nitrilotriacetates, By thermal analysis (TG/DTG /DSC), it was suggested, that in an oxidizing atmosphere (air) oxides are obtained at lower temperatures than in an inert atmosphere N2(g). By results from X-ray Diffraction (XRD), it was determinated that the oxides are crystalline and the predominant phases obtained are summarized titanate phases rutile and ilmenite. By fluorimetry was observed that the intensity of emission bands are directly proportional to the concentration of ions Ni2+, Co2+ and Pr3+, and IR spectroscopy (FTIR) from oxides, demonstrated the disappearance of characteristic bands by nitrilotriacetates, determining the complete decomposition of the nitrilotriacetates in oxides
Resumo:
Biodiesel is a fuel made up by mono-alkyl-esters of long chain fatty acids, derived from vegetable oils or animal fat. This fuel can be used in compression ignition engines for automotive propulsion or energy generation, as a partial or total substitute of fossil diesel fuel. Biodiesel can be processed from different mechanisms. Transesterification is the most common process for obtaining biodiesel, in which an ester compound reacts with an alcohol to form a new ester and a new alcohol. These reactions are normally catalyzed by the addition of an acid or a base. Initially sunflower, castor and soybean oil physicochemical properties are determined according to standard test methods, to evaluate if they had favorable conditions for use as raw material in the transesterification reaction. Sunflower, castor and soybean biodiesel were obtained by the methylic transesterification route in the presence of KOH and presented a yield above 93% m/m. The sunflower/castor and soybean/castor blends were studied with the aim of evaluating the thermal and oxidative stability of the biofuels. The biodiesel and blends were characterized by acid value, iodine value, density, flash point, sulfur content, and content of methanol and esters by gas chromatography (GC). Also studies of thermal and oxidative stability by Thermogravimetry (TG), Differential Scanning Calorimetry High Pressure (P-DSC) and dynamic method exothermic and Rancimat were carried out. Biodiesel sunflower and soybean are presented according to the specifications established by the Resolution ANP no 7/2008. Biodiesel from castor oil, as expected, showed a high density and kinematic viscosity. For the blends studied, the concentration of castor biodiesel to increased the density, kinematic viscosity and flash point. The addition of castor biodiesel as antioxidant in sunflower and soybean biodiesels is promising, for a significant improvement in resistance to autoxidation and therefore on its oxidative stability. The blends showed that compliance with the requirements of the ANP have been included in the range of 20-40%. This form may be used as a partial substitute of fossil diesel
Resumo:
Biodegradable microspheres used as controlled release systems are important in pharmaceutics. Chitosan biopolymer represents an attractive biomaterial alternative because of its physicochemical and biological characteristics. Chitosan microspheres are expected to become promising carrier systems for drug and vaccine delivery, especially for non-invasive ways oral, mucosal and transdermal routes. Controlling the swelling rate and swelling capacity of the hydrogel and improving the fragile nature of microspheres under acidic conditions are the key challenges that need to be overcomed in order to enable the exploration of the full pharmaceutical potential use of these microparticles. Many studies have focused on the modification of chitosan microsphere structures with cross-linkers, various polymers blends and new organic-inorganic hybrid systems in order to obtain improved properties. In this work, microspheres made of chitosan and nanosized hydrophobic silica (Aerosil R972) were produced by a method consisting of two steps. First, a preparation of a macroscopically homogeneous chitosan-hydrophobic silica dispersion was prepared followed by spray drying. FTIR spectroscopy, X-ray powder diffraction, differential scanning calorimetry, thermal gravimetric analysis, scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (TEM) were used to characterize the microspheres. Also, the were conducted acid stability, moisture sorption capacity, release properties and biological assays. The chitosan-hydrophobic silica composite microspheres showed improved thermal degradation, lower water affinity, better acid stability and ability to retard rifampicin and propranolol hydrochloride (drug models) release under simulated physiological conditions. In vitro biocompatibility studies indicated low cytotoxicity and low capacity to activate cell production of the pro-inflammatory mediator nitric oxide. The results show here encourage further studies on the use of the new chitosan-hydrophobic silica composite microspheres as drug carrier systems via oral or nasal routes.