Degradação de espécies nitroaromáticas e remediação de efluentes da indústria de explosivos, utilizando-se processos redutivos-oxidativos fundamentados no uso de ferro metálico

In this work the potentiality of reductive-oxidative processes based on zero-valent iron was studied aiming the degradation of nitroaromatic compounds and the remediation of residues from the explosive industry. The reductive process was applied as a continuous treatment system, using steel-wool as zero-valent iron source. The process permitted an almost total degradation of nitrobenzene, nitrophenol, nitrotoluene, dinitrotoluene and trinitrotoluene, probably with generation of the respective amine-derivative. The yellow-water residue, containing soluble trinitrotoluene, was notably modified by the reductive process, a fact that permitted a substantial enhancement of its biodegradability. Furthermore, the subsequent photo-Fenton process allowed TOC removal of about 80%.

Remoção de compostos orgânicos em água empregando carvão ativado impregnado com óxido de ferro: ação combinada de adsorção e oxidação em presença de H2O2

In this work, composites based on activated carbon/iron oxide (AC/Fe) were prepared in two different proportions (AC/Fe 5/1 and 1/1) and evaluated in the removal of the organic dye methylene blue (MB). Physical-chemical properties of the composites were determined by X-ray diffraction (XRD), adsorption/dessorption of N2 isotherm, temperature programmed reduction (TPR) and scanning electron microscopy (SEM). Results showed that goethite (α- FeOOH), with nanometer particle size, was formed over carbon surface for both composites. These materials showed high efficiency to remove MB from solution by combined adsorption and oxidation process. The AC/Fe 1/1 showed to be more active in (MB) oxidation then AC/Fe 5/1.

Síntese e caracterização de nanopartículas de óxido de ferro suportadas em matriz carbonácea: remoção do corante orgânico azul de metileno em água

In this work were prepared composites of iron oxide and carbonaceous materials in two different weight proportions (Carbon/Fe 1/1 and 1/2). The physico-chemical properties of the composites were determined by temperature programmed reduction (TPR), adsorption/dessorption of N2, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and pulse titration H2. The XRD and XPS analysis showed a cubic iron oxide phase, identified as maghemite, formed over the carbon surface. The particle size of maghemite showed to be within 10-30 nm. Carbon/Fe 1/2 was the most active in MB removal kinetics and ESI-MS studies showed that MB removal by both composites leads to oxidized intermediates.

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.

Influência da quantidade de amônio na síntese de nanopartículas de óxido de ferro por microemulsão

Iron oxide nanoparticles were synthesized in microemulsion systems composed by Triton X-100/hexyl alcohol/cyclohexane/aqueous solution. The nanoparticles were synthesized in microemulsions containing different amounts of ammonium, in order to evaluate the influence of this parameter on the size of the nanoparticles and on the phase transformation after heat treatment. Powder materials were obtained after centrifugation, washing and drying, and they were analyzed as synthesized and after heating at 350, 500 and 1000 °C. It was observed that the higher amount of ammonium induced smaller particles and minor phase transformation, possibly due to a preferential nucleation process.

Acetatos homo e heterotrinucleares de ferro: um experimento para o laboratório de química de coordenação

Homo and heterotrinuclear acetates are unique compounds having μ3-oxo bridge and many interesting properties of such compounds are derived from this structure. Some undergraduate inorganic textbooks discuss several aspects of these compounds and we present here an undergraduate experiment for the high-yield synthesis of [Fe2MO(CH3CO2)6(H 2O)3], with M = Fe3+, Co2+ and Ni2+, as well as their characterization using infrared spectroscopy and cyclic voltametry. The proposed experiment gives the opportunity to discuss several concepts of coordination chemistry that follow the characterization techniques, such as: types of acetate coordination, reversibility of electrochemical processes, quelate and trans effects and lability.

Adsorção de arsênio(V) pelo compósito magnético hidrotalcita: óxido de ferro

In this work, hydrotalcite, a layered double hydroxide, had its adsorption and ion exchange properties combined with the magnetic properties of iron oxide to produce a magnetic adsorbent, HT-Fe. The removal of As(V) by a HT-Fe adsorbent was evaluated under various conditions. The Kinetic process was well described by a pseudo-second order rate model. The maximum adsorption capacity, calculated with the Langmuir model showed to be dependent on pH, reaching values of 24.09, 10.19 and 7.44 mg g-1, respectively, for pH values of 4.0, 7.0 and 9.0. The inhibition by competition of anions is dependent on the type of ionic species.

Co2 na desidrogenação oxidativa do etilbenzeno utilizando catalisadores compostos de óxido de ferro e óxido de alumínio

Materials containing aluminum and iron oxide were synthesized through the preparation of hybrid spheres and tested in the dehydrogenation of ethylbenzene in the presence of CO2. The catalytic results suggest that the high initial ethylbenzene conversion is due to the contribution of basic sites. These results also point to a competitive process between CO2 adsorption and the oxidative dehydrogenation of ethylbenzene for the basic sites (lattice oxygen). In spite of the coke deposition is originating from ethylbenzene and CO2, the amount of carbonaceous deposits was smaller with the presence of CO2, if compared with the dehydrogenation in the absence of CO2.

Quantificação de antimônio em garrafas de politereftalato de etileno (PET) brasileiras por fluorescência de raios-X e avaliação quimiométrica para verificar a presença de pet reciclado através do teor de ferro

Antimony is a common catalyst in the synthesis of polyethylene terephthalate used for food-grade bottles manufacturing. However, antimony residues in final products are transferred to juices, soft drinks or water. The literature reports mentions of toxicity associated to antimony. In this work, a green, fast and direct method to quantify antimony, sulfur, iron and copper, in PET bottles by X-ray fluorescence spectrometry is presented. 2.4 to 11 mg Sb kg-1 were found in 20 samples analyzed. The coupling of the multielemental technique to chemometric treatment provided also the possibility to classify PET samples between bottle-grade PET/recycled PET blends by Fe content.

Dispersive liquid-liquid microextraction based on solidification of floating organic drop for simultaneous separation/preconcentration of nickel, cobalt and copper prior to determination by electrothermal atomic absorption spectrometry

A dispersive liquid-liquid microextraction based on solidification of floating organic drop for simultaneous extraction of trace amounts of nickel, cobalt and copper followed by their determination with electrothermal atomic absorption spectrometry was developed. 300 µL of acetone and 1-undecanol was injected into an aqueous sample containing diethyldithiocarbamate complexes of metal ions. For a sample volume of 10 mL, enrichment factors of 277, 270 and 300 and detection limits of 1.2, 1.1 and 1 ng L-1 for nickel, cobalt and copper were obtained, respectively. The method was applied to the extraction and determination of these metals in different water samples.

Óxidos de ferro e suas aplicações em processos catalíticos: uma revisão

A review of most of the reported studies on the use of iron oxides as catalyst in specific processes, namely Haber-Bosch reaction, Fischer-Tropsch synthesis, Fenton oxidation and photolytic molecular splitting of water to produce gaseous hydrogen, was carried out. An essential overview is thus presented, intending to address the fundamental meaning, as well as the corresponding chemical mechanisms, and perspectives on new technological potentialities of natural and synthetic iron oxides, more specifically hematite (α-Fe2O3), goethite (α-FeOOH), magnetite (Fe3O4) and maghemite (γ-Fe2O3), in heterogeneous catalysis.

Remoção de cromo (VI) de soluções aquosas utilizando o compósito magnético calcinado hidrotalcita-óxido de ferro: estudo cinético e de equilíbrio termodinâmico

In this work, hydrotalcite, a layered double hydroxide, had its ion exchange properties combined with the magnetic properties of iron oxide to produce a magnetic adsorbent, HT-Fe 500. These magnetic composites can be used as adsorbents for anionic contaminants in water and subsequently removed from the medium by a simple magnetic process. Removal of chromium (VI) from aqueous solutions using HT-Fe 500 was achieved using batch adsorption experiments. The adsorption capacity, calculated with the Langmuir-Freundlich model showed to be dependent on temperature, reaching values of 25.93 and 48.31 mg g-1, respectively, for temperatures of 25 and 30 ºC.

Constituintes fenólicos e atividade antioxidante da geoprópolis de duas espécies de abelhas sem ferrão amazônicas

We investigated the phenolic constituents and antioxidant activity of geopropolis from two species of stingless Amazonian bees, Melipona interrupta and Melipona seminigra. The chemical investigation of geopropolis from Melipona interrupta led to the isolation of 5,7,4'-trihydroxyflavonone, 3,5,6,7,4'-pentahydroxyflavonol, naringenine-4'-O-b-D-glucopyranoside and myricetin-3-O-b-D-glucopyranoside. Their structures were assigned based on spectroscopic analyses, including two-dimensional NMR techniques. Antioxidant activity of methanol and ethanol extracts of M. interrupta and M. seminigra were measured using the 1,2-diphenyl-2-picryl-hydrazyl (DPPH) free radical scavenging assay. This is also the first work reporting the chemical investigation of stingless bee species from the Amazonian region.

Conversão química de no e co sobre catalisadores à base de óxidos de cobalto ou de ferro

Cobalt or iron oxides supported or not on zeolite Hbeta were prepared and evaluated in the reduction reaction of NO by CO in presence of O2, SO2 or H2O. XRD results evidenced the Hbeta structure and the formation of Co3O4 and Fe2O3. TPR-H2 analysis showed complete reduction of cobalt oxide at lower temperatures than for iron oxide. The catalysts are quite active and the activity depends on the reaction temperature. The highest conversions rates were observed for pure iron oxide, which can be a relatively low cost catalyst for reduction of NO by CO, with high selectivity towards the N2 formation.

Experimento didático de quimiometria para planejamento de experimentos: avaliação das condições experimentais na determinação espectrofotométrica de ferro II com o-fenantrolina. Um tutorial, parte III

The objective of this manuscript is to describe a practical experiment that can be employed for teaching concepts related to design of experiments using Matlab or Octave computing environment to beginners, undergraduate and graduate students. The classical experiment for determination of Fe (II) using o-phenanthroline was selected because it is easy to understand, and all the required materials are readily available in most analytical laboratories. The approach used in this tutorial is divided in two steps: first, the students are introduced to the concept of multivariate effects, how to calculate and interpret them, and the construction and evaluation of a linear model to describe the experimental domain by using a 2³ factorial design. Second, an extension of the factorial design by adding axial points is described, thereby, providing a central composite design. The quadratic model is then introduced and used to build the response surface.