Direct and simultaneous determination of As, Cu, and Pb in Brazilian sugar cane spirits by graphite furnace AAS using tungsten permanent modifier with co-injection of Pd/Mg(N03)2

A method was developed using the multi-element graphite furnace atomic absorption spectrometry technique for the direct and simultaneous determination of As, Cu, and Pb in Brazilian sugar cane spirit (cachaça) samples. Also employed was the end-capped transversely heated graphite atomizer (THGA) with platforms pre-treated with W permanent modifier and co-injection of Pd/Mg(N03)2. Pyrolysis and atomization temperature curves were established in a cachaça medium (1+1; v/v) containing 0.2% (v/v) HN03 and spiked with 20 μg L-1 As and Pb and 200 μg L-1Cu. The effect of the concentration of major elements usually present in cachaça matrices (Ca, Mg, Na, and K) and ethanol on the absorbance of As, Cu, and Pb was investigated. Analytical working solutions of As, Cu, and Pb were prepared in 10% (v/v) ethanol plus 5.0 mg L-1 Ca, Mg, Na, and K. Acidified to 0.2% (v/v) HNO3, these solutions were suitable to build calibration curves by matrix matching. The proposed method was applied to the simultaneous determination of As, Cu, and Pb in commercial sugar cane spirits. The characteristic mass for the simultaneous determination was 16 pg As, 119 pg Cu, and 28 pg Pb. The pretreated tube lifetime was about 450 firings. The limit of detection (LOD) was 0.6 μg L-1As, 9.2 μg L-1 Cu, and 0.3 μg L-1Pb. The found concentrations varied from 0.81 to 4.28 μg L-1As, 0.28 to 382 mg L-1 Cu and 0.82 to 518 μg L-1 Pb. The recoveries of the spiked samples varied from 94-112% (As), 97-111% (Cu), and 95-101% (Pb). The relative standard deviation (n=12) was 6.9%, 7.4%, and 7.7% for As, Cu, and Pb, respectively, present in a sample at 0.87 μgL-1, 0.81 mgL-1, and 38.9 μgL-1concentrations.

Manganese determination by GFAAS in feces and fish feed slurries

This paper presents a simple, fast and sensitive method to determine manganese in samples of feces and fish feed by graphite furnace atomic absorption spectrometry (GFAAS) by the direct introduction of slurries into the graphite tube. The limits of detection (LOD) and quantification (LOQ) calculated for 20 readings of the blank of the standard slurries (0.50 % m/v of feces or feed devoid of manganese) were 28 and 92 μg kg-1 for the standard feces slurries and 34 and 110 μg kg-1 for the standard feed slurries. The proposed method was applied in bioavailability studies of manganese in different fish feeds and their results proved compatible with those obtained for samples mineralized by acid digestion using microwave oven. ©2007 Sociedade Brasileira de Química.

Microwave-induced fast decalcification of rat bone for electron microscopic analysis: An ultrastructural and cytochemical study

Bone decalcification is a time-consuming process. It takes weeks and preservation of the tissue structure depends on the quality and velocity of the demineralization process. In the present study, a decalcification methodology was adapted using microwaving to accelerate the decalcification of rat bone for electron microscopic analysis. The ultrastructure of the bone decalcified by microwave energy was observed. Wistar rats were perfused with paraformaldehyde and maxillary segments were removed and fixed in glutaraldehyde. Half of specimens were decalcified by conventional treatment with immersion in Warshawsky solution at 4oC during 45 days, and the other half of specimens were placed into the beaker with 20 mL of the Warshawsky solution in ice bath and thereafter submitted to irradiation in a domestic microwave oven (700 maximum power) during 20 s/350 W/±37°C. In the first day, the specimens were irradiated 9 times and stored at 40°C overnight. In the second day, the specimens were irradiated 20 times changing the solution and the ice after each bath. After decalcification, some specimens were postfixed in osmium tetroxide and others in osmium tetroxide and potassium pyroantimonate. The specimens were observed under transmission electron microscopy. The results showed an increase in the decalcification rate in the specimens activated by microwaving and a reduction of total experiment time from 45 days in the conventional method to 48 hours in the microwave-aided method.

Microwave fixation in rat fetuses tissues: Histological and immunohistochemical analysis

The aim of this study was to show the microwaves action in fixation of rat fetuses, dermal and cartilaginous tissues, using histological and immunohistochemistry methods for analysis. It was possible to conclude in this study using the rat as experimental model that the two methods for antibody retrieval, presented an excellent ways for the use of Ki67 antibody in the immunohistochemical analysis.

Damping behavior of hygrothermally conditioned carbon fiber/epoxy laminates

Carbon fiber reinforced polymer composites have been used in wide variety of applications including, aerospace, marine, sporting equipment as well as in the defense sector due to their outstanding properties at low density. In many of their applications, moisture absorption takes place which may result in a reduction in mechanical properties even at lower temperature service. In this work, the viscoelastic properties, such as storage modulus (E′) and loss modulus (E″), were obtained through vibration damping tests for three carbon fiber/epoxy composite families up to the saturation point (6 weeks). Three carbon fiber/epoxy composites having [0/0] s, [0/90] s, and [±45] s orientations were studied. During vibration tests the storage modulus (E′) and loss modulus (E″) were monitored as a function of moisture uptake, and it was observed that the natural frequencies and E′ values decreased with the increase during hygrothermal conditioning due to the matrix plasticization. © 2007 Wiley Periodicals, Inc.

Influence of microwave polymerization method and thickness on porosity of acrylic resin

Purpose: This study evaluated the influence of polymerization cycle and thickness of maxillary complete denture bases on the porosity of acrylic resin. Materials and Methods: Two heat-activated denture base resins - one conventional (Clássico) and one designed for microwave polymerization (Onda-Cryl) - were used. Four groups were established, according to polymerization cycles: A (Onda-Cryl, short microwave cycle), B (Onda-Cryl, long microwave cycle), C (Onda-Cryl, manufacturing microwave cycle), and T (Clássico, water bath). Porosity was evaluated for different thicknesses (2.0, 3.5, and 5.0 mm; thicknesses I, II, and III, respectively) by measurement of the specimen volume before and after its immersion in water. The percent porosity data were submitted to Kruskal-Wallis for comparison among the groups. Results: The Kruskal-Wallis test detected that the combinations of the different cycles and thicknesses showed significant differences, and the mean ranks of percent porosity showed differences only in the thinnest (2.0 mm) microwave-polymerized specimens (A = 53.55, B = 40.80, and C = 90.70). Thickness did not affect the results for cycle T (I = 96.15, II = 70.20, and III = 82.70), because porosity values were similar in the three thicknesses. Conclusions: Microwave polymerization cycles and the specimen thickness of acrylic resin influenced porosity. Porosity differences were not observed in the polymerized resin bases in the water bath cycle for any thickness. © 2007 by The American College of Prosthodontists.

Effect of different exposure times on microwave irradiation on the disinfection of a hard chairside reline resin

Purpose: This study evaluated the effectiveness of different exposure times of microwave irradiation on the disinfection of a hard chairside reline resin. Materials and Methods: Sterile specimens were individually inoculated with one of the tested microorganisms (Pseudomonas aeruginosa, Staphylococcus aureus, Candida albicans, and Bacillus subtilis) and incubated for 24 hours at 37°C. For each microorganism, 10 specimens were not microwaved (control), and 50 specimens were microwaved. Control specimens were individually immersed in sterile saline, and replicate aliquots of serial dilutions were plated on selective media appropriate for each organism. Irradiated specimens were immersed in water and microwaved at 650 W for 1, 2, 3, 4, or 5 minutes before serial dilutions and platings. After 48 hours of incubation, colonies on plates were counted. Irradiated specimens were also incubated for 7 days. Some specimens were prepared for scanning electron microscopic (SEM) analysis. Results: Specimens irradiated for 3, 4, and 5 minutes showed sterilization. After 2 minutes of irradiation, specimens inoculated with C. albicans were sterilized, whereas those inoculated with bacteria were disinfected. One minute of irradiation resulted in growth of all microorganisms. SEM examination indicated alteration in cell morphology of sterilized specimens. The effectiveness of microwave irradiation was improved as the exposure time increased. Conclusion: This study suggests that 3 minutes of microwave irradiation can be used for acrylic resin sterilization, thus preventing cross-contamination. © 2008 by The American College of Prosthodontists.

Voltammetry of mercury (II) based on an organo-clay modified graphite electrode

Organo-clay complex of ligand-hexadecyltrimethylammonium with montmorillonite was made for the purpose of application as a preconcentration agent in a chemically modified carbon paste electrode for determination of mercury (II) in aqueous solution. It was found out that the adsorption of Hg(II) by organo-clay complex is independent of the pH of the solution. It was also found out that the adsorption of the remaining metals Cd(II), Ps(II), Cu(II), Zn(II), and Ni(II) was dependent on the changes in pH solutions and increased when it varies from 1 to 8. The resultant material was characterized by cyclic and differential pulse anodic voltammetry using a modified graphite paste electrode in different supporting electrolytes. The mercury response was evaluated with respect to pH, electrode composition, preconcentration time, mercury concentration, possible interferences and other variables.

Effect of microwave disinfection on physical and mechanical properties of acrylic resins

This study evaluated the effect of microwave energy on the hardness, impact strength and flexural strength of the Clássico, Onda-Cryl and QC-20 acrylic resins. Aluminum die were embedded in metallic or plastic flasks with type III dental stone, in accordance with the traditional packing technique. A mixing powder/liquid ratio was used according to the manufacturer's instructions. After polymerization in water batch at 74°C for 9 h, boiling water for 20 min or microwave energy at 900 W for 10 min, the specimens were deflasked after flask cooling at room temperature, and submitted to finishing. Specimens non-disinfected and disinfected by microwave irradiation were submitted to hardness, impact and flexural strength tests. Each specimen was immersed in distilled water and disinfected in a microwave oven calibrated to 650 W for 3 min. Knoop hardness test was performed with 25 g load for 10 s, impact test was carried out using the Charpy system with 40 kpcm, and 3-point bending test with a crosshead speed of 0.5 mm/min until fracture. Data were submitted to statistical analysis by ANOVA and Tukey's test (α=0.05). Disinfection by microwave energy decreased the hardness of Clássico and Onda-Cryl acrylic resins, but no effect was observed on the impact and flexural strength of all tested resins.

Turning of compacted graphite iron using commercial tiN coated Si 3N4 under dry machining conditions

Due to their high hardness and wear resistance Si3N4 based ceramics are one of the most suitable cutting tool materials for machining hardened materials. Therefore, their high degree of brittleness usually leads to inconsistent results and sudden catastrophic failures. Improvement of the functional properties these tools and reduction of the ecological threats may be accomplished by employing the technology of putting down hard coatings on tools in the state-of-the-art PVD processes, mostly by improvement of the tribological contact conditions in the cutting zone and by eliminating the cutting fluids. However in this paper was used a Si3N4 based cutting tool commercial with a layer TiN coating. In this investigation, the performance of TiN coating was assessed on turning used to machine an automotive grade compacted graphite iron. As part of the study were used to characterise the performance of cutting tool, flank wear, temperature and roughness. The results showed that the layer TiN coating failed to dry compacted graphite iron under aggressive machining conditions. However, using the measurement of flank wear technique, the average tool life of was increased by VC=160 m/min.The latter was also observed using a toolmakers microscope and scanning electron microscopy (SEM).

Fatigue behaviour study on repaired aramid fiber/epoxy composites

Aramid fiber reinforced polymer composites have been used in a wide variety of applications, such as aerospace, marine, sporting equipment and in the defense sector, due to their outstanding properties at low density. The most widely adopted procedure to investigate the repair of composites has been by repairing damages simulated in composite specimens. This work presents the structural repair influence on tensile and fatigue properties of a typical aramid fiber/epoxy composite used in the aerospace industry. According to this work, the aramid/epoxy composites with and without repair present tensile strength values of 618 and 680MPa, respectively, and tensile modulus of 26.5 and 30.1 GPa, respectively. Therefore, the fatigue results show that in loads higher than 170 MPa, both composites present a low life cycle (lower than 200,000 cycles) and the repaired aramid/epoxy composite presented low fatigue resistance in low and high cycle when compared with non-repaired composite. With these results, it is possible to observe a decrease of the measured mechanical properties of the repaired composites.

Testing gaussianity, homogeneity, and isotropy with the cosmic microwave background

We review the basic hypotheses which motivate the statistical framework used to analyze the cosmic microwave background, and how that framework can be enlarged as we relax those hypotheses. In particular, we try to separate as much as possible the questions of gaussianity, homogeneity, and isotropy from each other. We focus both on isotropic estimators of nongaussianity as well as statistically anisotropic estimators of gaussianity, giving particular emphasis on their signatures and the enhanced cosmic variances that become increasingly important as our putative Universe becomes less symmetric. After reviewing the formalism behind some simple model-independent tests, we discuss how these tests can be applied to CMBdata when searching for large-scale anomalies. Copyright © 2010 L. Raul Abramo and Thiago S. Pereira.

Influence of microwave energy on structural and piezoelectric response of Bi 4Ti 3O 12 ceramics

Bismuth titanate ceramics (Bi 4Ti 3O 12) with 10 wt% in excess of bismuth (BIT10) were prepared by the polymeric precursor method and sinterized in microwave (MW) and conventional furnaces (CF). The effect of microwave energy on structural and electrical behavior of BIT10 ceramics was investigated by means of X-ray diffraction (XRD), Scanning electron microscopy (SEM) and electrical measurements. The results of the BIT10 ceramics processed in the microwave furnace (MW) showed a high structural organization compared to conventional treatment (CF). Size of grains and dieletrical properties are influenced by annealing conditions while coercitive field is not dependent on it. The maximum dielectric permittivity (12000) was obtained for the sample sintered in the microwave furnace. Piezoelectric force microscopy images reveals that in-plane response may not change its sign upon polarization switching, while the out-of-plane response does with the influence of microwave energy. Copyright © 2010 American Scientific Publishers All rights reserved.

Sintering temperature influence on microwave dielectric properties of TiO2-ZrO2 ceramics

Dielectric ceramics have been widely investigated and used for microwave applications such as resonators and filters. The present study deals with the influence of sintering temperature on microwave dielectric properties of TiO2 ceramics with 10, 20, and 30 wt% ZrO2. Three compositions have been developed through mixing procedures and then tested for each sintering temperature: 1500 and 1400°C. X-ray diffraction and scanning electron microscopy are carried out aiming to explain the ceramic behavior of each sample. The dielectric constants of different ceramics for both temperatures varied from 85.4 to 62.6, while their quality factor due to dielectric losses varied from 3110 to 1630. The Q decrease is attributed to the non uniform grain growth and to the obtained crystalline phases. The best microwave parameters were obtained for the ceramics sintered at 1400°C, which can be applied in microwave circuits as dielectric resonators. © (2010) Trans Tech Publications.

SnO 2 ceramics with low electrical resistivity obtained by microwave sintering

The main aim of this study was to develop dense and conducting SnO 2 ceramics without precipitated phases on the grain boundaries, which was verified using field emission scanning microscopy (FE-SEM) coupled with an energy-dispersive X-ray spectroscopy (FE-SEM/EDS). Two sample groups were investigated, where the first sample group was doped with zinc while the second one was doped with cobalt. The ceramics were prepared using the oxides mixture method and the sintering was carried out in a conventional muffle oven as well as in microwave oven. The results obtained were found to be similar regarding the relative density for the two sintering methods while time and temperature gains were observed for the microwave sintering method. The relative densities obtained were nearly 95%, for the two sintering methods. Concerning the electrical characterization measurements-electric field x current density as well as the environment temperature, the ceramics obtained through the conventional sintering method presented non-ohmic behavior. For the microwave sintered ceramics, we observed an ohmic behavior with electrical resistivity of 1.3 Ωcm for the samples doped with ZnO/Nb 2O 5 and 2.5 Ωcm for that of the samples doped with CoO/Nb 2O 5. The FE-SEM/EDS results for the microwave sintered ceramics indicated a structure with a reduced number of pores and other phases segregated at the grain boundaries, which leads to a better conductive ceramic than the conventional oven sintered samples. The dilatometry analysis determined the muffle sintering temperature and the difference between the densification of cobalt and zinc oxides. The addition of niobium oxide resulted in the decrease in resistivity, which thus led us to conclude that it is possible to obtain dense ceramics with low electrical resistivity based on SnO 2 using commercial oxides by the oxides mixture technique and the microwave oven sintering method. Copyright © 2011 American Scientific Publishers All rights reserved.