Níveis de contaminantes inorgânicos em cachaças da região do Quadrilátero Ferrífero armazenadas em copos in natura de esteatito (pedra-sabão)

The levels of inorganic contaminants (As, Cd, Cu, Ni and Pb) were measured in 18 Brazilian spirit beverages, before and after 4 contact cycles of 24h each with in natura soapstone (steatite) cups. Results were compared to Brazilian regulation levels. Spirits contained As, Cd, Ni and Pb within permitted levels. For Cu, 5.6% of the brands were above the limit. The contact with soapstone cups decreased Cu levels in the spirits, while the other elements remained unchanged. The use of in natura soapstone cups was considered safe because this kind of vessel did not transfer inorganic contaminants to the spirits.

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DETERMINAÇÃO DE Cd E Pb EM AMOSTRAS DE GOMA XANTANA POR GF AAS

This paper describes the evaluation of a method for determination of Cd and Pb in xanthan gum samples by Graphite Furnace Atomic Absorption Spectrometry (GF AAS) using NH4H2PO4 as the chemical modifier. The sample preparation was performed using a reflux system adapted in the digestion tubes. With this system it was possible to increase the temperature of the digester block above the boiling point of the reaction medium, preventing loss of analyte and excessive evaporation of acids during heating. Samples were digested with HNO3 for 3 h in a digester block at 220 ºC. The limits of detection for Cd and Pb were 2.2 and 33.8 ng g-1, respectively. The RSDs for both analytes were, on average, lower than 5.0% and accuracy was verified by recovery tests, yielding values in the 83-100% range.

SYNGAS PRODUCTION FROM CO2-REFORMING OF CH4 OVER SOL-GEL SYNTHESIZED Ni-Co/Al2O3-MgO-ZrO2 NANOCATALYST: EFFECT OF ZrO2 PRECURSOR ON CATALYST PROPERTIES AND PERFORMANCE

Ni-Co/Al2O3-MgO-ZrO2 nanocatalyst with utilization of two different zirconia precursors, namely, zirconyl nitrate hydrate (ZNH) and zirconyl nitrate solution (ZNS), was synthesized via the sol-gel method. The physiochemical properties of nanocatalysts were characterized by XRD, FESEM, EDX, BET and FTIR analyses and employed for syngas production from CO2-reforming of CH4. XRD patterns, exhibiting proper crystalline structure and homogeneous dispersion of active phase for the nanocatalyst ZNS precursor employed (NCAMZ-ZNS). FESEM and BET results of NCAMZ-ZNS presented more uniform morphology and smaller particle size and consequently higher surface areas. In addition, average particle size of NCAMZ-ZNS was 15.7 nm, which is close to the critical size for Ni-Co catalysts to avoid carbon formation. Moreover, FESEM analysis indicated both prepared samples were nanoscale. EDX analysis confirmed the existence of various elements used and also supported the statements made in the XRD and FESEM analyses regarding dispersion. Based on the excellent physiochemical properties, NCAMZ-ZNS exhibited the best reactant conversion across all of the evaluated temperatures, e.g. CH4 and CO2 conversions were 97.2 and 99% at 850 ºC, respectively. Furthermore, NCAMZ-ZNS demonstrated a stable yield with H2/CO close to unit value during the 1440 min stability test.

METHANE DRY REFORMING OVER Ni SUPPORTED ON PINE SAWDUST ACTIVATED CARBON: EFFECTS OF SUPPORT SURFACE PROPERTIES AND METAL LOADING

The influence of metal loading and support surface functional groups (SFG) on methane dry reforming (MDR) over Ni catalysts supported on pine-sawdust derived activated carbon were studied. Using pine sawdust as the catalyst support precursor, the smallest variety and lowest concentration of SFG led to best Ni dispersion and highest catalytic activity, which increased with Ni loading up to 3 Ni atoms nm-2. At higher Ni loading, the formation of large metal aggregates was observed, consistent with a lower "apparen" surface area and a decrease in catalytic activity. The H2/CO ratio rose with increasing reaction temperature, indicating that increasingly important side reactions were taking place in addition to MDR.

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.

AVALIAÇÃO DE PROPRIEDADES FÍSICAS E QUÍMICAS DE ELETRODEPÓSITOS DE Ni-W-P OBTIDOS EM CÉLULA DE HULL

Ni–W–P electrodeposits were synthesized in a Hull cell in order to simulate the obtainment under industrial conditions. Complete coverage of panels was accomplished by applying total currents of 1.0 and 2.0 A. Panels obtained with a current of 1.0 A appeared brighter. The best compositional uniformities, as determined by Energy Dispersive Spectrometer (EDS) occurred in the current density ranges of 0.6 to 3.0 A dm−2 and 1.6 to 6.0 A dm−2 obtained with 1.0 and 2.0 A, respectively. However, the best morphological characteristics, as determined by Scanning Electro Microscope (SEM), were observed in those obtained with a total current of 1.0 A. Analysis of corrosion resistance by Electrochemical Impedance Spectroscopy (EIS) and Potentiodynamic Linear Polarization (PLP) in NaCl have shown significant variations in the amount of corrosion potential, polarization resistance, and even total impedance. The alloys exhibited amorphous character (XRD) and crystallized above 400 °C to Ni and Ni3P phases, and possibly Ni–W, with a subsequent increase in hardness. The results suggest that under industrial conditions, current density variations due to the large and complex geometric shapes of substrates lead to formation of distinct alloys. Furthermore, these materials are potential substitutes for chromium deposits in many applications.

AVALIAÇÃO DA BIOACUMULAÇÃO DE METAIS EM Cyprinus carpio PELA INTERAÇÃO COM SEDIMENTO E ÁGUA DE RESERVATÓRIO

Bioaccumulation of Ag, Al, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb and Zn was determined in the gills and liver of Cyprinus carpio and related to concentrations in the sediment and water of the Alagados Reservoir, Ponta Grossa/Paraná. Cd and Fe exceeded the legal limit for water. Fe was the most abundant metal in the reservoir's water and sediment. The metals in the sediment were below the level of probable adverse effects on biota. There were no significant differences between sampling sites for water and sediment. Liver and gills had higher concentrations of Al, Fe and Zn, with a significant increase in Al (P > 0.05) compared to the increase in weight and size of the specimens. Statistically, gills showed higher concentrations of Al, Cd, Co, Cr, Mn and Zn and liver higher concentrations of Cu and Fe. Co, Cu, Fe, Mn and Zn showed significant differences (P < 0.01) between the organs. The bioaccumulation factors (BAF) showed that the interaction of water with gills promotes greater accumulation of metals in this organ. Despite the low concentrations in the reservoir, bioaccumulation of metals in gills and liver of C. carpio occurs by its interaction with contaminated water and sediment, respectively.

USO DO PLANEJAMENTO EXPERIMENTAL PARA OTIMIZAÇÃO DE UM PROCEDIMENTO VOLTAMÉTRICO PARA DETERMINAÇÃO SIMULTÂNEA DAS CONCENTRAÇÕES DOS METAIS Zn, Cd, Pb E Cu LIVRES EM ÁGUA DE COCO

Optimization of the main parameters of SWASV using boron-doped diamond electrode was described for the simultaneous determination of Zn, Cd, Pb and Cu free in coconut water. The values of electroanalytical parameters studied were optimized with the factorial design and center composite design. The optimized parameters for the preconcentration of metals were -1.50 V for potential, and 240 s for deposition time. For SWV, the optimized value was 11.56 mV for step potential. In addition, frequency and pulse height were defined at 100 Hz and 55 mV, respectively. Furthermore, the concentration of the supporting electrolyte (acetate buffer, pH 4.7) was optimized in 0.206 mol L-1. The optimized procedure was applied in two samples of coconut water: natural and processed. The limits of detection (LOD) obtained for Zn, Cd, Pb and Cu were 7.2; 4.4; 3.3 and 1.5 µg L-1, respectively. The concentrations of Cd and Pb were not detected. On the other hand, the values found for the concentrations of Zn and Cu were: < LOD (29 µg L-1) and (6.8 ± 0.9) µg L-1 for the natural sample; and (85.8 ± 4.2) µg L-1 and (7.7 ± 0.6) µg L-1 for the processed sample, respectively.

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Efeitos ópticos - eletrônicos de solventes nas polarizabilidades eletrônicas do íon Ni2+ no complexo [Ni(C3H4N2)6](CF3SO3)2

Polarizabilidades eletrônicas foram determinadas para o sal de tifluorometanosulfonato de níquel e para o complexo com imidazol, em soluções de metanol e de acetonitrila. A partir dos espectros eletrônicos, registrados numa concentração de 10-3 mol L-1 e pelo uso de um programa SIMP2FOS para o cálculo da força do oscilador experimental e POLAZ-F para o cálculo das polarizabilidades eletrônicas, foi possível perceber a distinta influência dos solventes na deformação da nuvem eletrônica do níquel (II).

A FTIR study of the metal-support interactions and hydrogen spillover on Pd/TiO2 and Ni/TiO2

Nickel and palladium dispersed on titania support were submitted to reductive treatment, under hydrogen, at 200 and 500 ºC. After the reductive thermal treatment the materials were exposed to carbon monoxide (10 Torr) and analyzed in the infrared region. The increasing of the electronic density in the metallic d subshell, produced by the reductive thermal treatment, was monitored by the infrared stretching band shift of carbon monoxide adsorbed and it was interpreted as a consequence of the metal-support interactions. The highest effect was observed for Pd/TiO2 system. From the FTIR spectra was also observed that the hydrogen spillover was stronger on Pd/TiO2 than Ni/TiO2 system.

Determinação de Cd por FAAS em meio aquoso após pré-concentração em linha sobre SiAT

Este trabalho descreve a síntese e caracterização da sílica gel modificada com grupos 2-aminotiazol (SiAT), os resultados de um estudo de adsorção e de pré-concentração (em batelada, e em fluxo utilizando-se a técnica de coluna) de íons Cd(II) em meio aquoso. A capacidade máxima de adsorção de íons Cd(II) determinada para SiAT foi de 1,12 mmol g-1 . Os resultados obtidos nos experimentos em fluxo, mostraram uma recuperação de 98% dos íons Cd(II) adsorvidos em coluna empacotada com 1 g de SiAT, utilizando-se 5 mL de HCl 1 mol L-1 como eluente. A metodologia proposta mostrou-se linear na faixa de concentração de 10 - 100 mg L-1, com limite de detecção de 0,80 mg L-1 e desvio padrão relativo de 3%. O fator de enriquecimento determinado foi de 29 vezes (considerando-se a percolação de 150 mL de solução 25 mg L-1 de Cd(II), 5 mL de eluato). A sorção-desorção quantitativa dos íons Cd(II), permitiram a aplicação do método na pré-concentração e posterior quantificação de traços de Cd(II) em amostras de águas naturais por espectrometria de absorção atômica com chama.