Determinação quantitativa de TNT e HNS por TG e FT-IR

2,4,6-trinitrotoluene (TNT) is an energetic material that shows scarce crystalline properties that can be improved by addition of 2,2',4,4',6,6'-hexanitrostilbene (HNS) in the crystallization process. HNS is a very important high explosive used in a variety of military, aerospace and industrial formulations owing to its suitable properties. It is an insensitive and thermal stable explosive that can be produced from 2,4,6-trinitrotoluene (TNT). The purpose of this work is the quantitative determination of HNS and TNT in explosives by thermogravimetric analysis (TG) and Fourier transform infrared spectroscopy (FT-IR).

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.

Immobilization of laccase on hybrid layered double hydroxide

Crystals of Mg/Al layered double hydroxide were synthesized by alkaline precipitation and treated in an aqueous solution of glutamic acid. The glutamate ions were not intercalated into the interlayer space, but were detected in the material by Fourier transform infrared spectroscopy, suggesting that only the external surfaces of crystals were modified with glutamate ions. The resulting hybrid material was tested as a support for immobilization of the enzyme laccase (Myceliophthora thermophila). The immobilized enzyme preparation was characterized by electronic paramagnetic resonance spectroscopy and by assays of catalytic activity. The activity of the immobilized laccase was 97% of the activity in the free enzyme. Layered double hydroxide is a suitable support for use in remediation of soil studies.

Biomassa residual para remoção de íons uranilo

Activities related to nuclear industry, production of phosphoric acid and hospitals have generated considerable volumes of radioactive waste containing uranyl ions. Banana pith was characterized by Scanning Electron Microscopy and Fourier Transform Infrared Spectroscopy and was investigated as a biosorbent for uranyl ions from nitric solutions by batch experiments. Influences of adsorbent size, kinetics and equilibrium adsorption were studied. The biosorption of the uranyl ions followed pseudo-second-order kinetics. The adsorption isotherm data were closely fitted to the Freundlich equation.

Obtaining high purity silica from rice hulls

Many routes for extracting silica from rice hulls are based on direct calcining. These methods, though, often produce silica contaminated with inorganic impurities. This work presents the study of a strategy for obtaining silica from rice hulls with a purity level adequate for applications in electronics. The technique is based on two leaching steps, using respectively aqua regia and Piranha solutions, which extract the organic matrix and inorganic impurities. The material was characterized by Fourier-transform infrared spectroscopy (FTIR), powder x-ray diffraction (XRD), x-ray fluorescence (XRF), scanning electron microscopy (SEM), particle size analysis by laser diffraction (LPSA) and thermal analysis.

Poliuretanos elastoméricos obtenidos a partir de aceite de ricino y almidón de yuca original y modificado con anhídrido propiónico: síntesis, propiedades fisicoquímicas y fisicomecánicas

Chemical modification of cassava starch was conducted through an acylation reaction by using pyridine and propionic anhydride to replace the functional groups of starch. Polyurethane elastomers were prepared using suspensions of the mixture obtained from castor oil and yucca starch that was modified by a propionic anhydride reaction. The suspensions were characterized by means of tests based on The Fourier Transform Infrared Spectroscopy and the Hydroxyl Index. The castor oil-AMP suspensions were used for the PU synthesis. The PUs were characterized by their physical-mechanical properties like tension- deformation and Shore A. hardness, thermal gravimetric analysis and swelling test. The density cross-linking of from swelling tests was determined by applying the Flory-Rehner equation.

Avaliação da eficiência das técnicas ESI-MS e ATR/FTIR na determinação de adulteração de BX com querosene e óleo residual

Direct infusion electrospray ionization mass spectrometry in the negative ion mode, ESI(-)-MS and Fourier transform infrared spectroscopy (FTIR) were used together with partial least squares (PLS) as a tool to determine B3 adulteration (B3 - mixture of 3% v/v of biodiesel in diesel) with kerosene and residual oil.

A comparative study of hydroxyapatite nanoparticles synthesized by different routes

In this study, bioactive hydroxyapatite nanoparticles were prepared by two different methods: wet chemical precipitation and biomimetic precipitation. The aim was to evaluate the morphology, particle-size, crystallinity and phases of the powders obtained by traditional wet chemical precipitation and the novel biomimetic precipitation using a supersaturated calcium solution. The nanoparticles were investigated by transmission electron microscopy, Fourier transform infrared spectroscopy and X-ray diffraction. The results revealed that the nanoparticles were formed by hydroxyapatite with a high crystallinity and controlled morphology. Additionally, it was found that the shape and size of the nanoparticles can be modified with each preparation method.

Análise exploratória aplicada a espectros de reflexão total atenuada no infravermelho com transformada de Fourier (ATR-FTIR) de blendas de biodiesel/diesel

In this study, hierarchical cluster analysis (HCA) and principal component analysis (PCA) were used to classify blends produced from diesel S500 and different kinds of biodiesel produced by the TDSP methodology. The different kinds of biodiesel studied in this work were produced from three raw materials: soybean oil, waste cooking oil and hydrogenated vegetable oil. Methylic and ethylic routes were employed for the production of biodiesel. HCA and PCA were performed on the data from attenuated total reflectance Fourier transform infrared spectroscopy, showing the separation of the blends into groups according to biodiesel content present in the blends and to the kind of biodiesel used to form the mixtures.

Poliuretanos obtenidos a partir de aceite de higuerilla modificado y poli-isocianatos de lisina: síntesis, propiedades mecánicas y térmicas y degradación in vitro

Biodegradable polyurethanes (PUR) were prepared from polyols derived from castor oil by transesterification of pentaerythritol-modified castor oil and lysine polyisocyanates (LDI and LTI). The polyurethanes obtained were characterized by Fourier transform infrared spectroscopy, thermogravimetric analysis (TGA), and dynamic mechanical thermal analysis (DMTA). The mechanical behavior of the polyurethanes was measured by Shore A hardness and tensile testing (stress-strain curves). The biodegradable nature of the material was determined by contact angle, water absorption tests, and in vitro degradation in PBS solution. This study aims to examine the effect of the structure and functionality of diisocyanate on the mechanical properties and in vitro degradation of the material. The results were compared with homologous materials obtained from isophorone diisocyanate (IPDI) used in previous works. The objective was to evaluate candidate materials that can be potentially used in tissue engineering.

ANÁLISES FÍSICO-QUÍMICAS DE BIOFILMES DE SULFATO DE CONDROITOINA MODIFICADO

Numerous investigations are dedicated to the research and development of new polymer materials destined for innovation in pharmaceutical forms. The application of these technological resources has allowed the commercialization of new therapeutic systems for modified drug release. This investigation aimed to evaluate the association of modified chondroitin sulfate with an insoluble polymer, Eudragit® RS 30 D, widely available in the pharmaceutical market. Isolated films were prepared by the evaporation process using a Teflon® plate. The aqueous dispersions (4% m/v) of synthetic polymer received the addition of modified chondroitin sulfate at different ratios. The interactions of the polymer chains in the blends were physicochemically characterized by means of Fourier transform infrared spectroscopy, thermal analyses, differential scanning calorimetry, thermogravimetry and scanning electron microscopy combined with hydration and assays in alkaline pH. The results showed appropriate properties of the coating materials for solid oral forms intended for drug deliver in specific environments.

PARÂMETROS TERMODINÂMICOS DA CASCA DE LARANJA DESIDRATADA

The global energy scenario is currently a widely discussed topic, with growing concern about the future supplies. Thus, much attention has been dedicated to the utilization of biomass as an energy resource. In this respect, orange peel has become a material of great interest, especially to Brazil, which generates around 9.5 million tons of this waste per year. To this end, the authors studied the kinetics of the thermal processing of dried orange peel in inert and oxidizing atmosphere. The thermodynamic parameters were determined by the Ozawa-Flynn-Wall method for the global process observed during heating from the 25°C up to 800°C. The thermal analysis in air and nitrogen showed 3-2 stages of mass loss, respectively, with approximately 20% residual mass under a nitrogen atmosphere. The increase in the values of activation energy for the conversion points between 20% and 60% for thermal effects in air and nitrogen atmosphere was observed. The activation energy obtained in an oxidizing atmosphere was higher than that obtained under a nitrogen atmosphere. The fourier-transform infrared spectroscopy and X-ray diffraction analysis showed that the material has a high level of complexity with the presence of alkali and alkaline earth groups as well as phosphate, plus substances such as pectin, cellulose and lignin.

UTILIZAÇÃO DO COMPÓSITO NANOESTRUTURADO SIO2/TIO2NA FOTODEGRADAÇÃO DE CORANTES TÊXTEIS COM LUZ SOLAR NATURAL

SiO2/TiO2 nanostructured composites with three different ratios of Si:Ti were prepared using the sol-gel method. These materials were characterized using energy dispersive X-ray fluorescence, Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, high-resolution transmission electron microscopy, photoluminescence, Raman with Fourier transform infrared spectroscopy, and the specific surface area. The band gaps of materials were determined by diffuse reflectance spectra, and the values of 3.20 ± 0.01, 2.92 ± 0.02, and 2.85 ± 0.01 eV were obtained as a result of the proportional increases in the amount of Ti within the composite. The materials exhibit only the anatase (TiO2) crystalline phase and have crystalline domains ranging from 4 to 5 nm. The photodegradation process of methylene blue, royal blue GRL, and golden yellow GL dyes were studied with respect to their contact times, pH variations within the solution, and the variations in the dye concentration of the solution in response to only sunlight. The maximum amount of time for the mineralization of dyes was 90 min. The kinetics of the process follows an apparently first order model, in which the obtained rate constant values were 5.72 × 10-2 min-1 for methylene blue, 6.44 × 10-2min-1 for royal blue GRL, and 1.07 × 10-1min-1 for golden yellow.

INFLUÊNCIA DO CATALISADOR EM SOLUÇÕES POLIMÉRICAS PARA O PREPARO DE GÉIS ORGÂNICOS DE RESORCINOL-FORMALDEÍDO

Resorcinol-formaldehyde (RF) organic gels have been extensively used to produce carbon aerogels. The organic gel synthesis parameters greatly affect the structure of the resulting aerogel. In this study, the influence of the catalyst quantity on the polymeric solution sol-gel process was investigated. Sodium carbonate was used as a basic catalyst. RF gels were synthesized with a resorcinol to formaldehyde molar ratio of 0.5, a resorcinol to catalyst (R/C) molar ratio equal to 50 or 300, and a resorcinol to solvent ratio of 0.1 g mL-1. The sol-gel process was evaluated in situ by Fourier transform infrared spectroscopy using a universal attenuated total reflectance sensor and measurements of the kinematic viscosity. The techniques showed the evolution of the sol-gel process, and the results showed that the lower catalyst quantity induced a higher gel point, with a lower viscosity at the gel point. Differential scanning calorimetry was used to investigate the thermal behavior of the RF dried gel, and results showed that the exothermic event related to the curing process was shifted to higher temperatures for solutions containing higher R/C ratios.

Ni(II), Cu(II), AND Zn(II) COMPLEXES DERIVED FROM A NEW SCHIFF BASE 2-((Z)-(3-METHYLPYRIDIN-2- YLEIMINO)METHYL)PHENOL AND SYNTHESIS OF NANO SIZED METAL OXIDE PARTICLES FROM THESE COMPOUNDS

Synthesis, spectral identification, and magnetic properties of three complexes of Ni(II), Cu(II), and Zn(II) are described. All three compounds have the general formula [M(L)2(H2O)2], where L = deprotonated phenol in the Schiff base 2-((z)-(3-methylpyridin-2-yleimino)methyl)phenol. The three complexes were synthesized in a one-step synthesis and characterized by elemental analysis, Fourier transform infrared spectroscopy, electronic spectra, X-ray diffraction (XRD), and room temperature magnetic moments. The Cu(II) and Ni(II) complexes exhibited room temperature magnetic moments of 1.85 B.M. per copper atom and 2.96 B.M. per nickel atom. The X-band electron spin resonance spectra of a Cu(II) sample in dimethylformamide frozen at 77 K (liquid nitrogen temperature) showed a typical ΔMS = ± 1 transition. The complexes ([M(L)2(H2O)2]) were investigated by the cyclic voltammetry technique, which provided information regarding the electrochemical mechanism of redox behavior of the compounds. Thermal decomposition of the complexes at 750 ºC resulted in the formation of metal oxide nanoparticles. XRD analyses indicated that the nanoparticles had a high degree of crystallinity. The average sizes of the nanoparticles were found to be approximately 54.3, 30.1, and 44.4 nm for NiO, CuO, and ZnO, respectively.