Absorção de bário por plantas de arroz (Oryza sativa L.) e mobilidade em solo tratado com baritina sob diferentes condições de potencial redox

Two parallel tests were carried out to evaluate barium solubility in soils treated with barite under reducing conditions: one in leaching columns and another with potted plants cultivated with rice. Soils were treated with three doses of barite and kept at two humidity levels. The reduction (-200 mV) condition promoted an increase in barium in the geochemical fraction of higher liability, higher concentrations of barium in the leached extracts, and higher absorption by rice plants. As a result of increased uptake and accumulation of barium, the plants showed stunted growth

Distribuição de Zn, Pb, Ni, Cu, Mn e Fe nas frações do sedimento superficial do Rio Cachoeira na região sul da Bahia, Brasil

The metal distribution in the surface sediment fractions of the Cachoeira River was evaluated based on the fractionation method using a five-step sequential extraction. The determination of metals was made by flame atomic absorption spectrophotometry (F AAS). Zn, Pb and Cu exhibit higher concentrations in the residual fraction of the sediment from sites that receive discharges from urban and industrial zones. High levels of Ni (60 ± 1 to 447 ± 9 µg L-1) were found in the river water, which may be detrimental to the "health" of rural communities that utilize the river water for domestic purposes without treatment.

Desenvolvimento de um método analítico baseado em microextração líquido-líquido para a determinação de cromo (VI) em amostras aquosas com detecção por espectrometria de absorção atômica em chama

In this study, a method for determination of hexavalent chromium in aqueous samples using liquid-liquid microextraction (LLME) and detection by Flame Atomic Absorption Spectrometry (F AAS) was developed. The LLME procedure was based on the extraction of Cr (VI) by acetone at a sample pH of 1.2. The use of saturated ammonium sulphate solution allowed effective separation of the aqueous and organic phases and acetone extracted chromium. The sample pH, acetone volume and stirring time were optimized by a full factorial design.

Método hidrometalúrgico para reciclagem de metais terras raras, cobalto, níquel, ferro e manganês de eletrodos negativos de baterias exauridas de Ni-MH de telefone celular

A hydrometallurgical method for the recovery of rare earth metals, cobalt, nickel, iron, and manganese from the negative electrodes of spent Ni - MH mobile phone batteries was developed. The rare earth compounds were obtained by chemical precipitation at pH 1.5, with sodium cerium sulfate (NaCe(SO4)2.H2O) and lanthanum sulfate (La2(SO4)3.H2O) as the major recovered components. Iron was recovered as Fe(OH)3 and FeO. Manganese was obtained as Mn3O4.The recovered Ni(OH)2 and Co(OH)2 were subsequently used to synthesize LiCoO2, LiNiO2 and CoO, for use as cathodes in ion-Li batteries. The anodes and recycled materials were characterized by analytical techniques.

Avaliação da combinação da nebulização discreta e processos de microextração aplicados à determinação de molibdênio por espectrometria de absorção atômica com chama (FAAS)

Simple and sensitive procedures for the extraction/preconcentration of molybdenum based on vortex-assisted solidified floating organic drop microextraction (VA-SFODME) and cloud point combined with flame absorption atomic spectrometry (FAAS) and discrete nebulization were developed. The influence of the discrete nebulization on the sensitivity of the molybdenum preconcentration processes was studied. An injection volume of 200 µL resulted in a lower relative standard deviation with both preconcentration procedures. Enrichment factors of 31 and 67 and limits of detection of 25 and 5 µg L-1 were obtained for cloud point and VA-SFODME, respectively. The developed procedures were applied to the determination of Mo in mineral water and multivitamin samples.

Avaliação de diferentes métodos para a determinação de cobre em óleo mineral isolante por espectrometria de absorção atômica com forno de grafite

This aim of this work was to compare two methods for copper determination in insulating oils from power transformers by GFAAS. The first method was extraction induced by emulsion breaking, which determined the preconcentration of copper in an aqueous solution and exhibited a limit of quantification of 0.27 µg L-1. Also, a second method based on the direct introduction of samples into GFAAS in the form of detergent emulsions, prepared with Triton X-114 and HNO3, was investigated. In this case, the limit of quantification was 1.7 µg L-1. Seven samples of used oils were successfully analyzed by both methods.

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.

SÍNTESE DE DERIVADOS DE FENANTRIDINONAS POR ARILAÇÃO DIRETA. CARACTERIZAÇÃO DOS ESPECTROS DE ABSORÇÃO E EMISSÃO DE EXEMPLOS REPRESENTATIVOS

The phenanthridinone heterocyclic system has attracted considerable attention in recent years due to the diverse array of physical, chemical and pharmacological properties demonstrated by natural and synthetic derivatives. As a consequence there has been considerable development of synthetic methodology for the synthesis of this and related heterocyclic ring systems. The synthetic literature is discussed and is compared with a direct arylation methodology for the intramolecular cyclization of tertiary (2-iodo)benzoylamides to generate the biaryl bond of these compounds. The efficient methodology allowed the synthesis of a number of previously unknown phenanthridinone products. The photoluminescent properties of representative examples were characterized and it is proposed that the previously unknown compound 1s reveals dual fluorescence in a manner similar to the known compound 1r.

Espectrometria de absorção atômica multielementar simultânea com atomização eletrotérmica em forno de grafite - uma revisão da técnica e aplicações

Este trabalho descreve uma revisão a respeito do emprego da técnica de espectrometria de absorção atômica simultânea em forno de grafite (SIMAAS) em determinações multielementares de elementos-traço em diferentes matrizes. Os principais parâmetros envolvidos e que devem ser considerados em medidas multielementares, tais como, fonte de radiação, geometria do forno, programa de aquecimento e natureza e quantidade de modificador químico, são descritos.

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.

Distribuição de Cr, Ni, Cu, Cd e Pb em frações húmicas de diferentes tamanhos moleculares extraídas de amostras de água e de sedimentos do reservatório de captação de água superficial Anhumas - Araraquara-SP

Estudou-se a distribuição de Cr, Ni, Cu, Cd e Pb em frações de substâncias húmicas (SH) de diferentes tamanhos moleculares. As SH foram extraídas de amostras de água (SHA) e de sedimentos de superfície (SHSS), interface/água (SHSI) e fundo (SHSF) coletados no reservatório de captação de água superficial Anhumas, localizado no município de Araraquara-SP. Para a extração das SH utilizaram-se os procedimentos recomendados pela Sociedade Internacional de Substâncias Húmicas. Após purificação por diálise, as SH foram fracionadas com base no tamanho molecular utilizando-se sistema de fracionamento seqüencial por ultrafiltração e fluxo tangencial. O fracionamento das amostras de SHA permitiu caracterizar uma distribuição de massa relativamente uniforme dentre as frações de diferentes tamanhos moleculares, com valores maiores nas frações F2 (20,8%) e F4 (23,8%). Exceto para os íons Pb(II) e Cu(II) os quais apresentaram concentrações relativamente mais altas nas frações F2 e F4, respectivamente, de maneira geral, crômio, níquel, cádmio e chumbo têm distribuições similares nas cinco frações com tamanhos moleculares maiores e médios (F1 a F5). Quanto às distribuições de massa nas diferentes frações de substâncias húmicas extraídas de amostras de sedimento de superfície (SHSS), sedimento interface/água (SHSI) e sedimento de fundo (SHSF), as três amostras apresentaram 42-48% das SH nas frações com maiores tamanhos moleculares (F1 e F2), 29-31% nas frações intermediárias (F3 e F4) e 13-20% nas frações com menores tamanhos moleculares (F5 e F6). De modo geral, caracterizaram-se para os íons metálicos, distribuições similares dentre as respectivas frações F1 a F6. Exceções para Pb(II) e Ni(II) em sedimento de superfície com concentrações relativamente menores nas frações F2 e F4, respectivamente.