Synthesis, characterization and electropolymerization of a new polypyrrole iron(II) Schiff-base complex

This work presents the synthesis of the complex [Fe(L)(2)](PF6)(2) (.) H2O (L = 2,6-bis[1-(3-pyrrol-1-yl-propylimino)ethyl]pyridine (Fig. 1) and its characterization through elemental and thermal analysis, X-ray diffraction and UV-Vis, IR and H-1 NMR spectra. The use of this compound in the preparation of modified electrodes is also described. The best electrochemical parameters to achieve optimum film formation have been established and the effects of both the upper-limit of the applied scanning potential (E-aul) and the number of scans on the efficiency of film formation have been investigated. Film surface morphology has been characterized by atomic force microscopy. (C) 2004 Elsevier Ltd. All rights reserved.

Effect of presence of an acid catalyst on structure and properties of iron-doped siloxane-polyoxyethylene nanocomposites prepared by sol-gel

In this work we investigate the effect of hydrochloric acid (HC) addition on the structure and thermal and magnetic properties of iron-doped siloxane-polyoxyethylene (POE) hybrids prepared by the sol-gel route. X-ray powder diffraction (XRD) and X-ray absorption near edge structure (XANES) results reveal the dominance of ferrihydrite nanoparticles and a mixture of this phase with FeCl4- species in the hybrid prepared without and with HCl, respectively. Thermal analysis reveals the existence of two crystalline polymeric phases in the hybrid prepared with HCl whereas hybrids prepared without HCl are amorphous. The 105 and 60 Angstrom sized ferrihydrite nanoparticles were detected by SAXS analysis of the composite prepared without and with HCl, respectively. The magnetic results suggest that in both samples antiferromagnetic nanoparticles coexist with small clusters/isolated ions. In the sample without HCl addition, larger particles dominate the magnetic behavior, while the opposite occurs for the sample prepared using HCl catalyst. (C) 2004 Elsevier B.V. All rights reserved.

Morphological caste differences and non-sterility of workers in Brachygastra augusti (Hymenoptera, Vespidae, Epiponini), a neotropical swarm-founding wasp

Morphological caste differences and ovary conditions were analyzed in four colonies of Brachygastra augusti collected in different stages of the colony cycle. Differences between castes are distinct suggesting pre-imaginal determination. Many intermediates (non-inseminated ovary-developed females) were found. Because these intermediate females were morphologically similar to workers, it is suggested that they are young ovary-developed workers. Because there is a more evident overlap between queens and workers in the colony in pre-emergence of workers stage, and in three colonies in latter stages, especially in worker-production colonies, it is suggested that smaller queens are probably less viable than larger queens as observed in previously studied epiponines.

Effect of an iron mouthrinse on enamel and dentine erosion subjected or not to abrasion: An in situ/ex vivo study

Objectives: This in situ/ex vivo study evaluated whether a rinse with an iron solution could reduce wear and the percentage of microhardness change of human enamel and dentine submitted to erosion followed by brushing after 1 or 30 min.Design: During 2 experimental 5-day crossover phases (wash-out period of 10 days), 10 volunteers wore intraoral palatal devices, with 12 specimens (6 of enamel and 6 of dentine) arranged in 3 horizontal rows (4 specimens each). In one phase, the volunteers immersed the device for 5 min in 150 mL of cola drink, 4 times a day. Immediately after immersion, no treatment was performed in one row. The other row was brushed after 1 min using a fluoride dentifrice and the device was replaced into mouth. After 30 min, the remaining row was brushed. In the other phase, the procedures were repeated, but after immersion the volunteers rinsed for 1 min with 10 mL of a 10 mM ferrous sulphate solution. Changes in surface microhardness (%SMH) and wear (profilometry) of enamel and dentine were measured. Data were tested using ANOVA and Tukey's tests (p < 0.05).Results: the enamel presented more wear than dentine, under all experimental conditions. The iron solution caused a significant reduction on the %SMH in enamel, and a significant reduction on the wear in dentine, regardless the other conditions.Conclusions: Rinsing with an iron solution after an erosive attack, followed or not by an abrasive episode, may be a viable alternative to reduce the loss of dental structure. (c) 2006 Elsevier Ltd. All rights reserved.

Preparation and properties of colloidal particles. Silica on yttrium iron garnet

Various properties of particles can be altered by coating them with a layer of different chemical composition. Yttrium iron garnet (YIG) particles has been coated with silica for control of their sintering, corrosion resistance, and stabilization of magnetic properties. This silica cover was obtained by hydrolysis of tetraethylorthosilicate (TEOS) in 2-propanol. This material was characterized by transmission (TEM) electron microscopy, (XEDS) X-ray energy-dispersive spectrometry, (XPS) X-ray photoemission spectroscopy and (VSM) vibrating sample magnetometry. YIG was heterocoagulated by silica as indicated by TEM micrographies. XPS measurements indicated that only binding energy for silicon and oxygen was found on the silica shell, which confirms that the YIG was covered. The values of the saturation magnetization differ from the heterocoagulated system to well-crystallized YIG.

Development and Evaluation of a Nanoporous Iron (Hydr)oxide Electrode for Phosphate Sensing

Nanoporous iron (hydr) oxide electrodes are evaluated as phosphate sensors using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The intensity of the reduction peak current (I-cp) of the ferrihydrite working electrode is tied to phosphate concentration at low pH; however, a hematite electrode combined with the use of EIS provided reliable sensing data at multiple pH values. Nanoporous hematite working electrodes produced an impedance phase component (theta) that shifts with increasing phosphate, and, at chosen frequencies, theta values were fitted for the range 1 nM to 0.1 mM phosphate at pH 4 and pH 7 in 5 mM NaClO4.

Transplacental Transfer of Iron in the Water Buffalo (Bubalus bubalis): Uteroferrin and Erythrophagocytosis

The objectives of this investigation were to understand transplacental transport of iron by secreted uteroferrin (UF) and haemophagous areas of water buffalo placenta and clarify the role(s) of blood extravasation at the placental-maternal interface. Placentomes and interplacentomal region of 51 placentae at various stages of gestation were fixed, processed for light and transmission electron microscopy, histochemistry and immunohistochemistry. Haemophagous areas were present in placentomes collected between 4 and 10 months of pregnancy. Perl's reaction for ferric iron was negative in placentomes, but positive in endometrial glands. Positive staining for UF indicated areas in which it was being taken up by phagocytosis and/or fluid phase pinocytosis in areolae of the interplacentomal mesenchyme, with little staining in endometrial stroma. Imunohistochemistry detected UF in trophectoderm of haemophagous regions of placentomes and in other parts of the foetal villous tree, but the strongest immunostaining was in the epithelial cells and lumen of uterine glands. Ultrastructural analyses indicated that erythrophagocytosis was occurring and that erythrocytes were present inside cells of the chorion that also contained endocytic vesicles and caveolae. Results of this study indicate that both the haemophagous areas of placentomes and the areolae at the interface between chorion and endometrial glands are important sites for iron transfer from mother to foetal-placental tissues in buffalo throughout pregnancy.

Organic complexation and translocation of ferric iron in podzols of the Negro River watershed. Separation of secondary Fe species from Al species

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Construction and application of an electrochemical sensor for paracetamol determination based on iron tetrapyridinoporphyrazine as a biomimetic catalyst of P450 enzyme

This work describes the construction and application of a biomimetic sensor for paracetamol determination in different samples. The sensor was prepared by modifying a glassy carbon electrode surface with a Nafion (R) membrane doped with FeTPyPz. The best performance of the sensor in 0.1 mol L-1 acetate buffer was at pH 3.6. Under these conditions, an oxidation potential of paracetamol was observed at 445 mV vs. Ag vertical bar AgCl. The sensor presented a linear response range between 4.0 and 420 mu mol L-1, a sensitivity of 46.015 mA L mol(-1) cm(-2), quantification and detection limits of 4.0 mu mol L-1 and 1.2 mu mol L-1, respectively. A detailed investigation about its electrochemical behavior and selectivity was carried out. The results suggested that FeTPyPz presents catalytic properties similar to P450 enzyme for paracetamol oxidation. Finally, the sensor was applied for paracetamol determination in commercial drugs and for the monitoring of its degradation in an electrochemical batch reactor effluent.

Spherical particles of phenolic resin treated with iron oxide

This paper describes the preparation and characterization of phenolic resins' thermospheres covered by a magnetic phase of iron oxide. The thermospheres were prepared by allowing phenol and formaldehyde to react under dispersion polymerization conditions and the iron oxide phase was incorporated in situ onto the phenolic resin particles by adding concentrated NH3 to FeCl2 in DMSO. This reaction was conducted at 70 degrees C under nitrogen atmosphere in a controlled temperature vessel, and the modified resin was isolated and dried in vacuo. Both pure and modified resins were characterized by DRX, TG- DTA, and MEV/ EDX. The modified particles were attracted by a magnetic field, indicating the fixation of magnetic iron oxide. No diffraction peaks were observed in DRX analysis; thermal analysis ( DTA) of both pure and modified resins presented exothermic events between 300 and 680 degrees C, and 300 and 570 degrees C, respectively, indicating the microstructure of the resin was modified after the treatment. Thermogravimetric analysis ( TGA) of the pure resin registered a 2.0% residue, compared to 8.0% for the modified resin. These residues correspond to about 7.0% of fixed iron oxide. MEV/ EDX analyses confirm the modification of the resins by the process of fixing iron oxide.

Chemical process to separate iron oxides particles in pottery sample for EPR dating

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Application of a Biomimetic Sensor Based on Iron Phthalocyanine Chloride: 4-Methylbenzylidene-Camphor Detection

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Changes on iron electrode surface during hydrogen permeation in borate buffer solution

Hydrogen interaction with oxide films grown on iron electrodes at open circuit potential (E-oc) and in the passive region (+0.30 V-ECS) was studied by chronopotentiometry, chronoamperometry and electrochemical impedance spectroscopy techniques. The results were obtained in deaerated 0.3 mol L-1 H3BO3 + 0.075 mol L-1 Na2B4O7 (BB, pH 8.4) solution before, during and after hydrogen permeation. The iron oxide film modification was also investigated by means of in situ X-ray absorption near-edge spectroscopy (XANES) and scanning electrochemical microscopy (SECM) before and during hydrogen permeation. The main conclusion was that the passive film is reduced during the hydrogen diffusion. The hydrogen permeation stabilizes the iron surface at a potential close to the thermodynamic water stability line where hydrogen evolution can occur. The stationary condition required for the determination of the permeation parameters cannot be easily attained on iron surface during hydrogen permeation. Moreover, additional attention must be paid when obtaining the transport parameters using the classical permeation cell. (c) 2007 Elsevier Ltd. All rights reserved.

Mossbauer spectroscopy study of iron oxide nanoparticles obtained by spray pyrolysis

Mossbauer spectroscopy was used in this study to investigate magnetite nanoparticles, obtained by spray pyrolysis and thermal treatment under H-2 reduction atmosphere. Room temperature XRD data indicate the formation of magnetite phase and a second phase (metallic iron) which amount increases as the time of reduction under H2 is increased. While room temperature Mossbauer data confirm the formation of the cubic phase of magnetite and the occurrence of metallic iron phase, the more complex features of 77 K-Mossbauer spectra suggest the occurrence of electronic localization favored by the different crystalline phase of magnetite at low temperatures which transition to the lower symmetry structure should occur at T similar to 120 K (Verwey transition).