Determination of Cu, Ni and Pb in Aqueous Medium by FAAS after Pre-Concentration on 2-Aminothiazole Modified Silica Gel

This work describes the synthesis and characterization of 2-aminothiazole modified silica gel (SiAT), and the results of a study of the adsorption and pre-concentration (in batch and using a flow-injection system coupled to an absorption atomic spectrometer) of Cu(II), Ni(II) and Pb(II) in aqueous medium. The adsorption capacities for each metal ions in mmol g -1 were: Cu(II)= 1.18, Ni(II)= 1.15 and Pb(II)= 1.10. The results obtained in the flow experiments showed a recovery of practically 100% of the metal ions adsorbed in a mini-column packed with 100 mg of SiAT, using 100 μL of 2.0 mol L -1 HCl solution as eluent. The sorption-desorption of the metal ions made possible the application of a flow-injection system for the pre-concentration and quantification by FAAS of metal ions at trace level in natural water samples digested and not digest by an oxidizing UV photolysis.

Final stages of the Brasiliano Orogenesis in SE Brazil: U-Pb and 40Ar/39Ar evidence for overprinting of the Brasília Belt by the Ribeira Belt Tectonics

Around the southern margins of the São Francisco Craton, there is a zone of tectonic interference between the Brasília belt to the west and the younger Ribeira belt to the east. U-Pb monazite and 40Ar/39Ar cooling age determinations carried out in the area reveal the cooling histories of these belts and the timing of tectonic overprint, unraveling the final stages of Brasiliano Orogeny in SE Brazil. The U-Pb monazite data from migmatized paragneisses and late-stage pegmatites in the Socorro-Guaxupé Nappe System of the southern Brasília belt show that migmatization peaked between ca. 613±1 and 607±3 Ma. 40Ar/39Ar biotite and muscovite ages of paragneisses and schists in this area indicate that the northern high-grade core of the Nappe System (Guaxupé Domain) was uplifted and cooled through the 350°C isotherm between 599±1 and 587±1 Ma. In contrast, samples from the southern high-grade core of the Nappe System, the Socorro Domain, south of the Jacutinga shear zone, yields a broader and younger spectrum of 40Ar/39Ar biotite ages between 571±1 and 562±1 Ma, attributed to a later uplift and cooling of the crust. The cooling ages can be assigned to local resetting of the 40Ar/39Ar system during transpressive tectonic overprint due to reactivation as a result of collision of the Ribeira belt. A younger group of 40Ar/39Ar mica ages (537±1 to 521±1Ma) in schists of the Socorro Domain, are associated with transpressional structures of the Ribeira belt. Rock samples from the Jacutinga and Três Corações shear zones, yield 40Ar/39Ar biotite-muscovite ages around 520 Ma. These are typical cooling ages of the Ribeira belt, and are interpreted to mark the western limit of the Ribeira belt transpressional regime within the Brasília belt. The youngest biotite-muscovite cooling ages in schists of the Socorro Domain, between 510±2 and 491±1 Ma, mark the final cooling and exhumation of that part of the Brasília belt.

Simultaneous determination of Cd and Pb in antibiotics used in sugar-cane fermentation process by GFAAS

A method has been developed for the simultaneous determination of Cd and Pb in antibiotics used in sugar-cane fermentation by GFAAS. The integrated platform of transversely heated graphite atomizer was treated with tungsten to form a coating of tungsten carbide. Six samples of commercial solid antibiotics were analyzed by injecting 20 μL of digested samples into the pretreated graphite platform with co-injection of 5 μL of 1000 mg L-1 Pd as chemical modifier. Samples were mineralized in a closed-vessel microwave-assisted acid-digestion system using nitric acid plus hydrogen peroxide. The pyrolysis and atomization temperatures of the heating program of the atomizer were selected as 600°C and 2200°C, respectively. The calculated characteristic mass for Cd and Pb was 1.6 pg and 42 pg, respectively. Limits of detection (LOD) based on integrated absorbance were 0.02 μg L -1 Cd and 0.7 μg L-1 Pb and the relative standard deviations (n = 10) for Cd and Pb were 5.7% and 8.0%, respectively. The recoveries of Cd and Pb added to the digested samples varied from 91% to 125% (Cd) and 80% to 112% (Pb).

Evaluation of Ir-based modifiers in the simultaneous determination of As, Bi, Pb, Sb, and Se in milk by graphite furnace atomic absorption spectrometry

Different modifiers (IrCl3, W+IrCl3, Zr+IrCl 3) and coatings (Ir, W-Ir, Zr-Ir) were evaluated for the simultaneous determination of arsenic, bismuth, lead, antimony, and selenium in milk by graphite furnace atomic absorption spectrometry using the 'end-capped' transversely heated graphite atomizer (THGA). Integrated platform, pretreated with Zr-Ir as permanent modifier, was elected as the optimum surface modification resulting in up to 250 firings. Two additional recoatings were possible without significant changes in the analytical performance (750 firings). For 20 μL of matrix-matched standard solutions using diluted (1:10) milk samples, typical correlation coefficients between integrated absorbance and analyte concentration (5.00-20.0 μg/L) was always better than 0.999. The levels of the analytes found in commercial milk samples were lower than the limit of detection: 2.9 μg/L As, 2.9 μg/L Bi, 1.8 μg/L Pb, 1.9 μg/L Sb, and 2.5 μg/L Se. Recoveries were found within the following intervals: 88-114% for As, 89-118% for Bi, 89-113% for Pb, 91-115% for Sb, and 92-115% for Se. The relative standard deviations (n = 12) were ≤2% (As), ≤ 5% (Bi), ≤ 1.4% (Pb), ≤ 3% (Sb), and 5% (Se), and the respective calculated characteristic masses were 54 pg As, 55 pg Bi, 40 pg Pb, 56 pg Sb, and 51 pg Se.

Dielectric properties of Pb Nb2 O6 ferroelectric ceramics at cryogenic temperatures

Complex dielectric permittivity measurements in Pb Nb2 O6 ceramics were performed in a frequency and temperature range of 1 kHz-1 MHz and from 15 to 900 K, respectively. The results revealed two dielectric anomalies showing typical characteristics of relaxor ferroelectric materials at cryogenic temperatures. Comparison with other tetragonal tungsten bronze (TTB) structure-type materials suggests the existence of successive phase transitions, which until now were not reported. The observed low temperature dielectric behaviors seem to be due to intrinsic physical characteristics related to the TTB structure. © 2007 American Institute of Physics.

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.

Avaliação das condutas de biossegurança em laboratórios de prótese dentária de João Pessoa, PB, Brasil

Objective: To evaluate the biosecurity measures adopted in dental prosthesis laboratories of the city of João Pessoa, PB, Brazil with respect to prosthetic works sent by dentists. Method: Twenty-five dental prosthesis technicians (DPT) of the city of João Pessoa, PB, filled out a questionnaire referring to their knowledge of the biosecurity principles, disinfection of impressions and other prosthetic items, and the use of individual protection equipment (IPE). Results: Although 92% of the interviewees believed in the possible occurrence of cross-infection between dental prosthesis laboratories and dental offices, 64% declared that the prosthetic works received in their laboratories do not undergo any disinfection procedure. It was also observed that, for disinfection of impressions and stone casts, the chemical substances are not used as recommended by the manufacturers or are innocuous to microorganisms. Regarding the use of IPE, 60% of the DPT used mask, but only 4% used gowns. With respect to the measures taken regarding the impressions received from dental offices, 56% of the interviewees only wash them in running tap water, and 56% of the stone casts that arrive at the laboratory are not disinfected in any way. Conclusion: There is a need for more motivation and instructions to DPT regarding the prevention of cross-contamination during sending and receiving of prosthetic works between dental prosthesis laboratories and dental offices because the DPT evaluated in this study were found negligent with respect to disinfection procedures.

Dielectric tunability in (1-x)[Pb(Mg 1/3Nb 2/3)O 3]-xPbTiO 3 ceramics for tunable devices application

The dielectric properties of the 0.65[Pb(Mg 1/3Nb 2/3)O 3]-0.35PbTiO 3 ferroelectric ceramic composition were investigated viewing the capability to be used for tunable microwave applications. The dielectric response has been studied for three selected temperatures (300 K, 370 K and 400 K), below the paraelectric- ferroelectric phase transition temperature, as a function of the applied 'bias' electric field. The obtained dielectric tunability was found to be around 60 %, under an electric field of 19 kV/cm, which makes the studied ceramic composition an excellent candidate for application in the electro-electronic industry, as tunable devices. © 2010 IEEE.

Direct simultaneous determination of Pb(II) and Cu(II) in biodiesel by anodic stripping voltammetry at a mercury-film electrode using microemulsions

A mercury film electrode was used to determine direct and simultaneously Pb(II) (at -410 mV) and Cu(II) (at -100 mV) in biodiesel by anodic stripping voltammetry. A linear response was obtained for Pb(II) and Cu(II) in the 2.00 × 10-8-1.00 × 10-7 mol L-1 concentration range and detection limits were 2.91 × 10-9 mol L-1 and 4.69 × 10-9 mol L-1 for Pb(II) and Cu(II), respectively, with recovery around of 100.0%. © 2012 Elsevier Ltd. All rights reserved.

Measurement of the azimuthal anisotropy of neutral pions in Pb-Pb collisions at √sNN=2.76 TeV

First measurements of the azimuthal anisotropy of neutral pions produced in Pb-Pb collisions at a center-of-mass energy of √sNN=2.76 TeV are presented. The amplitudes of the second Fourier component (v2) of the π0 azimuthal distributions are extracted using an event-plane technique. The values of v2 are studied as a function of the neutral pion transverse momentum (pT) for different classes of collision centrality in the kinematic range 1.6

Zircon fission track and U-Pb dating methods applied to São Paulo and Taubaté Basins located in the southeast Brazil

Zircon samples from the Cenozoic São Paulo and Taubaté Basins and Mantiqueira Mountain Range (southeast Brazil) were concomitantly dated by zircon Fission Track Method (FTM) and in situ U-Pb dating method. While FTM detrital-zircon data are ideally used to provide low-temperature information, U-Pb single detrital grain ages record the time of zircon formation in igneous or high grade metamorphic environments. This methodology may be used to study the possible sources of the basins sediments. The results suggest that the São Paulo Basin is composed of sediments from just one source, the Mantiqueira Mountain Range. On the other hand, the Taubaté Basin presents further sediment sources besides the Mantiqueira Mountain Range. © 2012 Elsevier Ltd. All rights reserved.

Sequential Determination of Cd, Cu and Pb in Tea Leaves by Slurry Introduction to Thermospray Flame Furnace Atomic Absorption Spectrometry

A simple procedure for the sequential determination of Cd, Cu and Pb in tea leaves by slurry introduction to thermospray flame furnace atomic absorption spectrometry was developed. Detection limits were 0.05 mg kg-1 for Cd, 2.1 mg kg-1 for Cu and 0.68 mg kg-1 for Pb using 0.67 % (m/v) slurries (100 mg/15 mL). © 2013 Springer Science+Business Media New York.

Fe K-edge X-ray absorption spectroscopy study of Pb(Fe2/3W 1/3)O3-PbTiO3 multiferroic ceramics

The present paper is a comprehensive study concerning Fe K-edge X-ray absorption spectroscopy (XAS) measurements, which were performed to characterize the local structure of (1 - x)Pb(Fe2/3W1/3)O 3-xPbTiO3 samples as a function of temperature and PbTiO3 content. Results obtained by the fits of extended X-ray absorption fine structure consist with rhombohedral symmetry for Pb(Fe 2/3W1/3)O3 composition at temperatures lower than room temperature. This result is in apparent disagreement with X-ray and neutron diffraction characterization which have been reported. This apparent disagreement is related to the fact that XAS probes the short-range order, whereas X-ray diffraction provides structural information about the average structure. Moreover, as the PbTiO3 content increases, a disorder has been detected at local structure of the FeO6 octahedron. Analysis of X-ray absorption near edge structure spectra did not show modifications in intensity nor energy of transitions. © 2013 American Institute of Physics.

Anthropogenic influences on Cd, Cr,Cu, Ni, Pb and Zn concentrations in soils and sediments in a watershed with sugar cane crops at São Paulo State, Brazil

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