Obtenção de filmes espessos de seleneto de cobre sobre carbono vítreo, ouro, titânio e cobre

Copper selenide (berzelianite) films were prepared on the title substrates using the chemical bath deposition technique (CBD). Film composition was determined by energy dispersion of x-rays. The kinetics of film growth is parabolic and film adherence limits the film thickness. On titanium, copper selenide forms islands that do not completely cover the surface, unless the substrate is prepared with a tin oxide layer; film composition also depends on the titanium oxide layer. On vitreous carbon, CBD and mechanical immobilization techniques lead to films with similar resistances for the electron transfer across the film/substrate interface. On gold, composition studies revealed that film composition is always the same if the pH is in the range from 8 to 12, in contrast to films prepared by an ion-ion combination route. On copper, a new procedure for obtaining copper selenide films as thick as 5 µm has been developed.

Otimização do banho eletrolítico da liga Fe-W-B resistente à corrosão

A study on optimization of bath parameters for electrodeposition of Fe-W-B alloys from plating baths containing ammonia and citrate is reported. A 2³ full factorial design was successfully employed for experimental design analysis of the results. The corrosion resistance and amorphous character were evaluated. The bath conditions obtained for depositing the alloy with good corrosion resistance were: 0.01 M iron sulfate, 0.10 M sodium tungstate and 0.60 M ammonium citrate. The alloy was deposited at 12% current efficiency. The alloy obtained had Ecorr -0.841 V and Rp 1.463 x 10(4) Ohm cm². The deposit obtained under these conditions had an amorphous character and no microcracks were observed on its surface. Besides this, the bath conditions obtained for depositing the alloy with the highest deposition efficiency were: 0.09 M iron sulfate, 0.30 M sodium tungstate and 0.50 M ammonium citrate. The alloy was deposited at 50% current efficiency, with an average composition of 34 wt% W, 66 wt% Fe and traces of boron. The alloy obtained had Ecorr -0.800 V and Rp 1.895 x 10³ Ohm cm². Electrochemical corrosion tests verified that the Fe-W-B alloy deposited under both conditions had better corrosion resistance than Fe-Mo-B.

Cloud point extraction for the determination of copper in environmental samples by flame atomic absorption spectrometry

A simple cloud point extraction procedure is presented for the preconcentration of copper in various samples. After complexation by 4-hydroxy-2-mercapto-6-propylpyrimidine (PTU), copper ions are quantitatively extracted into the phase rich in Triton X-114 after centrifugation. Methanol acidified with 0.5 mol L-1 HNO3 was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). Analytical parameters including concentrations for PTU, Triton X-114 and HNO3, bath temperature, centrifugation rate and time were optimized. The influences of the matrix ions on the recoveries of copper ions were investigated. The detection limits (3SDb/m, n=4) of 1.6 ng mL-1 along with enrichment factors of 30 for Cu were achieved. The proposed procedure was applied to the analysis of environmental samples.

Avaliação do efeito da concentração de carbonato na eletrodeposição de cobre sobre discos de aço-carbono

Mild steel blankets were covered with electrolytic copper thin layer, from cyanide bath, being evaluated the influence of the carbonate concentration in the physiochemical properties of those deposits. The cell voltage decreased as the current intensity decreased, but the adherence of the deposit was not enhanced, showing that the increment of carbonate concentration causes substantial problems. Chemical solubilization reactions of air-bearing carbon dioxide and oxidation of free cyanide ions through dissolved oxygen evolved in the anodic processes contribute to the copper plating to occur in an inefficient way. The best optimal conditions require a carbonate concentration below 50 g L-1.

Análise de resíduos de agrotóxicos em tomates empregando dispersão da matriz em fase sólida (DMFS) e cromatografia gasosa

This work was aimed on optimization of the matrix solid-phase dispersion (MSPD) technique using gas chromatography for analyzing residues of chlorpyriphos, λ-cyhalothrin, cypermethrin and deltamethrin in tomatoes. The results showed that silica was more efficient for the clean up of extracts, but florisil provided the highest recovery rates. A 2³ complete factorial design was carried out to evaluate the absorbent/sample ratio, presence of co-column (silica) and ultrasonic bath on the extraction rate. The percentage of extraction of the pesticides chlorpyriphos, λ-cyhalothrin, cypermethrin and deltamethrin were 64.7, 88.3, 99.2 and 89.2%, respectively, with relative standard deviations below 5%.

Aplicação de zeólitas sintéticas como coadjuvante em formulação detergente

The study consists is the application of zeolites NaX, NaY and A as builder in detergent formulations to eliminate the hardness of water. Therefore, the adsorption of ions Ca+2 and Mg+2 were evaluated, and the effect of the cleaning action of the surfactant sodium dodecil sulfate (SDS) through tests of detergency. The experiments were conducted in bath system (with shaking) and quantification of metals was performed by atomic absorption spectrometry. Zeolite A showed the best results for adsorption of Ca++ and Mg++ with retention rates of around 90 and 70% respectively and acted positively on the action of cleaning the surfactant SDS.

Sorção do inseticida tiametoxam nas frações orgânica e mineral de um latossolo amarelo

The sorption of thiamethoxam in a Brazilian Oxisol was determined in soil samples with and without organic matter for two different dephs (0-0.1 and 0.4-0.7 m). The results indicated a predominant sorption of thiamethoxam on soil without organic matter. The following Kd values of 4.25 mL g-1 (0-0.1 m, r² = 0.8534) and 5.30 mL g-1 (0.4-0.7 m, r² = 0.9884) and Kf values, 7.65 mL g-1 (0-0.1 m, r² = 0.9623) and 7.72 mL g-1 (0.4-0.7 m, r² = 0.9775) were obtained. Those sorption coefficient values indicated a small interaction between thiamethoxam for both original soil and soil without organic matter.

Avaliação da biodegradabilidade de efluentes têxteis do beneficiamento secundário de malhas de poliéster tratados com Reagente de Fenton

From the environmental point of view, the textile sector is outstanding for the generation of large amounts of biorecalcitrant effluents. In this paper the textile effluent biodegradability, both before and after its treatment with Fenton's Reagent, were compared by means of biologic tests. These tests showed that the Fenton treatment lowered the biodegradabilty of practically all tested effluents, except one specific effluent from a scouring bath of polyester fibers, which achieved a 93% COD removal. This removal was due to a significant phase separation (oil/water).

Hidróxido de níquel suportado em carbono: um catalisador de baixo custo para a eletro-oxidação de alcoóis em meio alcalino

The present manuscript shows the synthesis of nickel hydroxide supported in carbon (Ni(OH)2/C) as a alternative material for catalytic alcohol oxidation in alkaline medium. The Ni(OH)2/C was synthesized in different percentage using a sonic bath. No current densities variation during successive cyclic voltammetry experiments was observed. The Ni(OH)2/C electrodes exhibit a potent and persistent electrocatalytic activity towards the oxidation of different alcohols. In addition, alcohols electooxidation occurs in less positive potential compared with noble metal catalyst.

Electrochemical study about zinc electrodeposition onto GCE and HOPG substrates

We carried out an electrochemical study about zinc electrodeposition onto GCE and HOPG substrates from an electrolytic plating bath containing 0.01M ZnSO4 + 1M (NH4)2SO4 at pH 7. Under our experimental conditions the predominant chemical species was the complex [ZnSO4(H2O)5]. The chronoamperometric study showed that zinc electrodeposition follows a typical 3D nucleation mechanism in both substrates. The average dG calculated for the stable nucleus formation was 6.92 x 10-21 J nuclei"1 and 1.35 x 10-20 J nuclei"1 for GCE and HOPG, respectively. The scanning electron microscopy (SEM) images showed different nucleation and growth processes on GCE and HOPG substrates at same overpotential.

Série histórica da composição química de pilhas alcalinas e zinco-carbono fabricadas entre 1991 e 2009

Mn, Zn, Fe, Cd, Pb and Hg were determined in Zn-C and alkaline batteries manufactured along almost 20 years. After samples disassembly the electroactive components were treated with aqua regia in bath ice for 24 h. Metals were analyzed by ICP-OES. Zn and Mn amounts did not vary significantly. Fe amount decreased, specially after 2000. Hg, Cd and Pb amounts dramatically decreased along time, being virtually absent in alkaline batteries manufactured after 2005. Pb still remains in Zn-C samples. Scanning electron microscopy of batteries manufactured in 1997 and 1998 showed the presence of Bi, In and Cr in the plastic/paper anode-cathode separator.

Sinterabilidade de pós de precursor vitrocerâmico do sistema LZSA tratados por troca iônica

Ion exchange method was employed by means of surface modification of the glass powders of LZSA (Li2O-ZrO2-SiO2-Al2O3) system submitted to a 70wt% NaNO3/30wt% NaSO4 bath salt followed by a heat treatment. Chemical analysis by X-ray fluorescence was used to evaluate the efficiency of ion exchange, while optical dilatometry was employed to evaluate sintering of compacts. Evaluation of the structure of sintered bodies was made by scanning electron microscopy. Substitution of Li+ ions by Na+ ions on the surface of powders during heat treatments of 450 and 600 ºC for 2-10 h promoted an increase in densification of the sintered bodies.

The use of tribromoisocyanuric acid to distinguish among primary, secondary and tertiary alcohols

Primary, secondary and tertiary alcohols can be easily distinguished due to their reactivity towards tribromoisocyanuric acid (TBCA). The test is performed by adding TBCA to the alcohol in a test tube heated in a boiling water bath. Orange color develops in the tube containing the primary alcohol, light yellow is observed in the tube containing the secondary alcohol while the tertiary alcohol results in a colorless mixture.

Electrochemical and physical characterization of Ni-Cu-Fe alloy for chlor-alkali hydrogen cathodes

This work describes the development of an alternative acetate bath for the electrochemical codeposition of Ni-Cu-Fe electrodes at low pH that is stable for several weeks and produces electrodes with good performance for chlor-alkali electrolysis. Physical characterization of the electrode surface was made using X ray absorption spectroscopy (XAS), scanning electron microscopy (SEM) and energy dispersive analysis (EDX). The evaluation of the material as electrocatalyst for the hydrogen evolution reaction (her) was carried out in brine solution (160 g L-1 NaCl + 150 g L-1 NaOH) at different temperatures through steady-state polarization curves. The Ni-Cu-Fe electrodes obtained with this bath have shown low overpotentials for the her, around 0.150 V at 353 K, and good stability under continuous long-term operation for 260 hours. One positive aspect of this cathode is that the polarization behavior of the material shows only one Tafel slope over the temperature range of 298 - 353 K.

Hematological and immunological responses of Nile tilapia after polyvalent vaccine administration by different routes

The efficacy of a polyvalent bacterin vaccine against Aeromonas hydrophila, Pseudomonas aeroginosa and Enterococcus durans administered by different routes in Nile tilapia was assessed by analyzing hematological and immunological parameters 7 and 21 days after vaccination. Treatments consisted of: non-vaccinated tilapia; tilapia vaccinated by intraperitoneal injection with 2x10(8) formalin-inactivated bacteria·mL-1; tilapia vaccinated orally with 2x10(7) formalin-inactivated bacteria·g-1, feed for 5 days; tilapia vaccinated by immersion bath in 2x10(7) formalin-inactivated bacteria·mL-1, for 20 minutes. Vaccinated fish groups presented higher hematocrit, number of erythrocytes and leukocytes than the non-vaccinated group. Serum agglutination titer of intraperitoneally vaccinated fish was higher on both evaluation periods for the three bacteria strains. Only on day 21 post-vaccination fish from the oral and immersion vaccination groups presented higher serum agglutination titer than the non-vaccinated fish for A. hidrophyla and E. durans. Serum antimicrobial activity in vaccinated fish was higher for P. aeroginosa and E. coli than in non-vaccinated fish on both evaluation periods. The different vaccine administration routes stimulated hematological and immunological responses in Nile tilapia 21 days post-vaccination, but intraperitoneal vaccination presented higher total number of leukocytes, lymphocytes and serum agglutination titer.