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

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

Desenvolvimento de sistemas líquido-cristalinos empregando silicone fluido de co-polímero glicol e poliéter funcional siloxano

For the construction of the phase diagrams, the method of the aqueous titration was used. There were prepared 5 ternary diagrams, varying the surfactant and the oil phase. The liquid-crystalline phases were identified by polarized light microscopy. The formulations prepared with silicon glycol copolymer, polyether functional siloxane (PFS) and water (S1) and with diisopropyl adipate, PFS and water (S4) presented liquid-crystalline phases with lamellar arrangement. Moreover, after 15 days in hot oven (37 ºC), the formulations presented hexagonal arrangement, evidencing the influence of the temperature in the organization of the system.

Argilas bentoníticas da península de Santa Elena, Equador: pilarização, ativação ácida e seu uso como descolorante de óleo de soja

Two samples of calcic bentonite of the Santa Elena Peninsula, Ecuador, were pillared with Al13 ions in the ratio of 10, 15 and 20 meq of Al g-1 of clay, calcinated at 573, 723 and 873 ºK and acid activated with 4, 6 and 8 mol L-1 H2SO4. Analyses by X-ray diffraction, X-ray fluorescence, differential and gravimetric thermal, density, surface area and porosity, were applied in order to study the modifications occurred in the crystalline structure of the montmorillonite. The 8 mol L-1 H2SO4 acid-activated 15 meq of Al g-1 of clay at 573 ºK Al-pillared samples indicated the best results in the bleaching of the soybean oil measured by UV-visible spectrophotometer.

Termocromismo em soluções de alcóxidos de Vanádio(IV): uma abordagem pela modelagem molecular

The thermochromic behavior exhibited by vanadium(IV) alkoxides, [V2(μ-OPr i)2(OPr i) 6] and [V2(μ-ONep)2(ONep)6 ], OPr i = isopropoxide and ONep = neopentoxide, was studied by molecular modeling using DFT, TDDFT and INDO/S methods. The vibrational and electronic spectra calculated for [V2(μ-OPr i)2(OPr i) 6] were very similar to the experimental data registered for crystalline samples of the complex and for its solutions at low temperature (< 210 K), while spectra recorded at high temperature (> 315 K) were compatible with those calculated for the monomeric form, [V(OPr i)4]. These results consistently point to a monomer/dimer equilibrium as an explanation for the solution thermochromism of {V(OPr i)4}n. In spite of the structural similarity between [V2(μ-ONep)2(ONep)6 ] and [V2(μ-OPr i)2(OPr i) 6] in the solid state, the thermochromic behavior of the former could not be explained by the same model, and the possibility of tetranuclear aggregation at low temperatures was also investigated.

Caracterização físico-química e microestrutural de conchas de moluscos bivalves provenientes de cultivos da região litorânea da ilha de Santa Catarina

Samples of shells of oysters and mussels from sea farm around the Santa Catarina Island in south Brazil were collected and analyzed by DRX, FRX, SEM, CHN-S, FTIR, TG, AAS/Flame and AAS /GF. The results showed that the crystalline structure of mussel's shells is mainly formed by aragonite and the oyster's shells by calcite. The calcium percentage in both shells species was in the range of 33 to 35% and also 850 and 1200 mg/kg of strontium was detected in the shells of oysters and mussels, respectively. The content of organic matter was larger in the mussel's shells and the thermal degradation of both shells species occurred by three events at different temperatures from 250 to 830 ºC.

Análise cristalográfica da solução sólida com estrutura tipo Tungstênio Bronze de niobato de potássio e estrôncio dopado com ferro

Solid solution of iron doped potassium strontium niobate with KSr2(FeNb4)O15-Δ stoichiometry was prepared by high efficiency ball milling method. Structural characterization was carried out by X-ray diffraction. Crystalline structure was analyzed by the Rietveld refinements using the FullProf software. The results showed a tetragonal system with the tetragonal tungsten bronze structure - TTB (a = 12.4631 (2) Å and c = 3.9322 (6) Å, V = 610.78 (2) ų). In this work, the sites occupancy by the K+, Sr2+ and Fe3+ cations on the TTB structure were determined. NbO6 polihedra distortion and its correlation with the theoretical polarization are discussed.

Purificação e caracterização da quitinase de uva (Vitis vinífera L. cv Red Globe) para a produção de quitosana a partir de quitina de camarão

Chitinase is produced by a wide variety of plants as a defense against peste attacks. In this study, grape chitinases were purified 16 times by fractionation in 80% ammonium sulfate followed by dialysis and filtration. Purified chitinases exhibited enzymatic activity toward chitin azure. The yield of purified chitinase was 229 mg/L with chitinase activity of 563 U/g. Chitinases had molecular masses of 24 and 30 kDa, as evaluated by SDS-PAGE 12.5%. Two pH optima were determined 3.0 and 6.0. The optimal temperature was 42 °C. Pre hydrolysis of crystalline shrimp chitin by chitinases caused in an increase in the deacetylation ratio triggered by chitin deacetylase producing chitooligosaccharides with DA (degree acetylation) of 58.8%.

Eixo quinário: um elemento de simetria presente em moléculas e quasi-cristais - um experimento didático em cristalografia

Axis of quinary symmetry occur in molecular symmetry, as in the case of fullerenes, and in crystalline symmetry, in the quasicrystals. Minerals with pentagonal faces do not have this element of symmetry, as the pyrite (FeS2) which shows a ridge that is different from the other ones, in any face of the crystal. The purpose of this paper is to demonstrate conceptual differences between pyritohedron and regular pentagonal dodecahedron symmetries, discussing students' difficulties to identify them. Also is proposed a didactic experiment with spatial models of the above-mentioned forms and the demonstration of its symmetries in clinographic projections.

Síntese hidrotermal assistida por micro-ondas como metodologia sintética eficiente para obtenção da rede metalorgânica [ZN(BDC)(H2O)2]n

This work presents the optimization of the microwave-assisted hydrothermal synthesis of [Zn(BDC)(H2O)2]n . The reactions were carried out at the fixed temperature of 120 ºC for 10, 20, 30 and 40 min. Pure crystalline [Zn(BDC)(H2O)2]n was obtained in high yield (ca. 90%) with a reaction time of 10 min. The phase obtained and its purity was confirmed by Rietveld refinement, with a final value for Rwp/Rexp equal to 1.48. Increased reaction times (20, 30 and 40 min) favored the formation of unwanted by products, resulting in mixtures of several crystalline phases.

Thermal and structural study of guava (Psidium guajava L) powders obtained by two dehydration methods

Two food products (powders) were obtained by hot-air drying or lyophilisation methods on the whole guava fruits. The powders were characterised by sensory and thermal analyses (TGA-DSC), infrared spectroscopy (IR), X-ray diffraction (XRD) and scanning electron microscopy (SEM). Thermal, morphological and structural characterisations showed a similar behaviour for the two solids. TGA-DSC and IR showed the presence of pectin as the main constituent of solids. A semi-crystalline profile was evidenced by XRD, and lamellar/spherical morphologies were observed by SEM. Sensory analyses revealed an aroma highly related to guava. These value-added food products are an alternative to process guava and avoid loss during postharvest handling.

Biosilicato®: histórico de uma vitrocerâmica brasileira de elevada bioatividade

This paper presents a historical of the Biosilicate®, a bioactive glass-ceramic developed at the Vitreous Materials Laboratory of the Federal University of São Carlos, Brazil. After decades of study accomplished with bioactive glasses and glass-ceramics, Biosilicate® results from a natural evolution and has similar bioactivity index, but far superior mechanical properties than of all bioactive glasses. Biosilicate® is almost fully crystalline and also exhibits much higher bioactivity than all the currently commercially available bioactive glass-ceramics. Due to its special characteristics, Biosilicate® has been successfully tested for several medical and dental applications as we thoroughly discuss in this review paper.

Properties of silica from rice husk and rice husk ash and their utilization for zeolite y synthesis

This study compared properties of silica (SiO2) from rice husk (RH) and rice husk ash (RHA) extracted by acid- and heat-treatment. The SiO2 from RH was in amorphous phase with nearly 100% purity while that from RHA was in crystalline phase with 97.56% purity. Both extracted SiO2 were used in the synthesis of zeolite NaY but that from RH was better due to the efficiency in product recovery and simplicity of extraction. After the NaY was exchanged to NH4Y and calcined to convert to HY, the product did not carry over the textural properties of the parent NaY and NH4Y.

Efeitos da história térmica nas propriedades do polímero pet: um experimento para ensino de análise térmica

Polyethilenetherephtalate (PET) is commonly used in manufacturing of beverage bottles representing a didactic appeal in thermal analysis education due to its presence in the student's day life. Additionally such polymer presents well defined thermal analytical curves and a well known thermal behavior. TGA curve is used to present the thermal stability. The thermal history effects in the thermal properties of a PET sample from a soft drink bottle are used to demonstrate the effect of different heating/cooling conditions on glass transition, melting, crystallization and crystalline degree using DSC curves.

Hidróxidos duplos lamelares à base de escória de alto forno

Hydrotalcite like compounds (HT) were prepared by co-precipitation (Mg/Al = 3.5), using an acid solution with blast furnace slag and MgCl2.6H2O and aqueous solutions of NaOH. The following synthesis variables were investigated: temperature (30 and 45 ºC) and pH (9 and 12). Depending of the temperature two systems were observed: Mg-Al-CO3 (T = 30 ºC); Mg-Al-Cl-CO3 (T = 45 ºC). An increase in the pH of synthesis and Mg2+ concentration produced HTs well-crystallized and with greater values of all cell parameters. The study showed the potentiality of BFS in the synthesis of well-crystallized LDHs without the presence of other crystalline phases.

Comparação estrutural entre amostras de materiais tipo hidrotalcita obtidas a partir de diferentes rotas de síntese

Three samples of hydrotalcite-like materials (HTC) were synthesized and their structural characteristics were compared with two HTCs obtained commercially. Thermal analyses, FT-IR, PXRD and textural analyses were used to investigate the structural differences between commercial and synthetic samples. Particularly, the memory effect was observed at temperature higher than 600 ºC. The Rietveld refinements were obtained with expressive accuracy and the statistical parameters of goodness of fit are quite satisfactory. In conclusion, the procedures adopted in synthesis of HTC produced crystalline materials with high surface area materials.