Extração líquido-líquido de urânio(VI) do colofanito de itataia (Santa Quitéria, Ceará) por extratantes orgânicos em presença de ácido fosfórico

This work describes the liquid-liquid extraction of uranium after digestion of colofanite (a fluoroapatite) from Itataia with sulfuric acid. The experiments were run at room temperature in one stage. Among the solutions tested the highest distribution coefficient (D > 60) was found for 40%vol. DEHPA (di(2-ethyl-hexyl)phosphoric acid) + 20% vol. TOPO (trioctylphosphine oxide) in kerosene. Thorium in the raffinate was quantitatively extracted by TOPO (0.1% vol.) in cyclohexane. Uranium stripping and separation from iron was possible using 1.5 mol L-1 ammonium or sodium carbonate (room temperature, one stage). However, pH control is essential for a good separation.

Adsorção e dessorção aniônicas individuais por gibbsita pedogenética

Anion adsorption/desorption dynamics was studied as individual processes on surface of particles of a gibbsitic clay. The data suggest a remarkable gibbsite role as nitrate leaching retardant in soil. The opposite behavior of gibbsite towards adsorption/desorption of silicate and phosphate suggests the need of an adequate compromise solution regarding interval and rate applications of anions in cultivated gibbsitic soils. The high P adsorption verified in pH values lower than that reported for the point of zero charge of synthetic Al-hydroxides implies that this process takes place in pedogenic gibbsites through inner sphere complexation.

Determination of nitrate in lettuce by ion chromatography after microwave water extraction

Lettuce is worldwide known as the most important vegetable. In this context, most farmers are searching new techniques for best quality products including hydropony. However, nitrate is of great concern, since it has a negative impact on human metabolism. The main objective of the present work was to evaluate the nitrate content of lettuce produced by conventional and hydroponic systems. The determination was conducted by ion chromatography and a new method of extraction was tested using microwave oven digestion. The results indicated that nitrate level produced in the conventional system was lower than in the hydroponic system.

Caracterização e propriedades do material coloidal nanoestruturado β-FeOOH/bentonita

A new mixed material was obtained through the combination of the suspensions of iron oxy-hydroxide and bentonite clay, denoted BFe. Analysis of its structure (XRD, Mossbauer and TGA) and composition (AAS) suggests the maintenance of the layer structure of the clay and an increase in the thermal stability of the BFe. Electrochemical studies performed in different electrolytes show that only in an alkaline medium it is possible to observe the redox peaks relative to the processes involving Fe+2/Fe+3 pair. Tests that evaluated the potential use of the photo-Fenton process showed an efficient degradation process of the dyes in significantly reduced reaction times.

Utilização de planejamento fatorial no preparo de amostras de detergente em pó para a determinação de fósforo por análise em fluxo

The decomposition of detergent powder samples in a microwave oven and autoclave was evaluated. To establish the best experimental conditions a 2(5) factorial design was performed, varying the conditions in autoclave and microwave digestion and flow system parameters for the determination of phosphorus. The best composition was: 0.2 mL sulfuric acid; 500 W power and a 2 min time interval; 6 mmol L-1 of ascorbic acid and 16 mmol L-1 of molybdate to flow system. This factor levels use less reagents than the reference method. No statistically significant differences were found between the autoclave and microwave oven responses at the 95% confidence level.

Síntese e caracterização de complexos de platina(IV) com derivados N-benzilados da 1,3-propanodiamina

The present work describes the synthesis of a series of platinum(IV) complexes with N-benzyl 1,3-propanediamine derivatives. Since substitution of the axial ligands in the platinum(IV) complexes may alter their pharmacological properties, we have prepared complexes with different groups, such as hydroxide, chloride and acetate using a sequence of substitution reactions. The resulting complexes were fully characterized by IR, ¹H, 13C and 195Pt NMR spectroscopies, and elemental analysis.

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.

Eletrodos modificados por hidróxido de níquel: um estudo de revisão sobre suas propriedades estruturais e eletroquímicas visando suas aplicações em eletrocatálise, eletrocromismo e baterias secundárias

The present review paper describes the main features of nickel hydroxide modified electrodes covering its structural and electrochemical behavior and the newest advances promoted by nanostructured architectures. Important aspects such as synthetic procedures and characterization techniques such as X-Ray diffraction, Raman and Infrared spectroscopy, Electronic Microscopy and many others are detailed herein. The most important aspect concerning nickel hydroxide is related to its great versatility covering different fields in electrochemical-based devices such as batteries, electrocatalytic systems and electrochromic electrodes, the fundamental issues of these devices are also commented. Finally, some of the newest advances achieved in each field by the incorporation of nanomaterials will be shown.

Determinação de enxofre em amostras vegetais por oxidação via seca em meio alcalino com detecção espectrofométrica

The sulphur take an essential role in plants and it is one of the main nutrients in several metabolic processes. The dry ash oxidation, using alkaline oxidizers agent, is the simplest and most economical form for the oxidation of Organic S to sulfate in plants. The objective of this work is to propose a method for sulfur determination in plants samples using dry ash oxidation and agent oxidizers alkaline. The quantification of S-SO4(2-) in samples was accomplished by turbidimetric method. The results demonstrated that the proposed method for oxidation alkaline was appropriate.

Adsorção de arsênio(V) pelo compósito magnético hidrotalcita: óxido de ferro

In this work, hydrotalcite, a layered double hydroxide, had its adsorption and ion exchange properties combined with the magnetic properties of iron oxide to produce a magnetic adsorbent, HT-Fe. The removal of As(V) by a HT-Fe adsorbent was evaluated under various conditions. The Kinetic process was well described by a pseudo-second order rate model. The maximum adsorption capacity, calculated with the Langmuir model showed to be dependent on pH, reaching values of 24.09, 10.19 and 7.44 mg g-1, respectively, for pH values of 4.0, 7.0 and 9.0. The inhibition by competition of anions is dependent on the type of ionic species.

Aplicação de métodos quimiométricos na otimização da extração de Ca, Mg, K, Fe, Zn, Cu e Mn em folhas de braquiária

This work applied a 2² factorial design to the optimization of the extraction of seven elements (calcium, magnesium, potassium, iron, zinc, copper and manganese) in brachiaria leaves, determined by flame atomic absorption spectrometry. The factors sample mass and digestion type were evaluated at two levels: 200/500 mg, and dry/wet, respectively. Principal component analysis allowed simultaneous discrimination of all the significant effects in one biplot. Wet digestion and mass of 200 mg were considered the best conditions. The decrease of 60% in sample mass allowed to save costs and reagents. The method was validated through the estimation of figures of merit.

Biomonitoramento de Cr e Pb em peixes de água doce

Trace metal content of three fish species harvested from a tank located in the City of Guarapuava-PR, Brazil were determined by digestion and voltametry. Trace metal content in fish samples were 0.10-1.30 µg/g (muscle) and 0.45-15.90 µg/g (liver) for chromium, 0.35-2.56 µg/g (muscle) and 2.32-34.30 µg/g (liver) for lead. The levels of lead and chromium in fish samples were higher than the recommended legal limits for human consumption. To assess the dietary intake of Cr and Pb by fish, weekly intake was calculated based on average metals contents and weekly consumption of fish and it compared with PTWI (Provisional Tolerable Weekly Intake). The Cr and Pb have achieved up to 25 and 45%, respectively, of PTWI recommended by WHO/FAO.

Estudio de la contaminación por metales en sedimentos acuáticos de la Bahía de Matanzas

Surface sediments of the Bay of Matanzas (Cuba) were studied to assess its environmental quality by using several criteria (metal content index, pollution load index and sediment quality guidelines). Two partial digestion sediment procedures and a modified BCR sequential extraction were used. The concentrations of metals were measured by atomic spectroscopy methods. The founded contents of Cu (2,4-27,9 mg kg-1), Zn (2,5-55,5 mg kg-1) and Ni (8,8-99,2 mg kg-1) were below those reported by other authors. The results obtained suggested that the most polluted sites were 3, 5, and 6. The sequential extraction procedure showed that most of the studied metals were associated to the more stable fractions.

Highly improved chromium (III) uptake capacity in modified sugarcane bagasse using different chemical treatments

The present paper focuses on improving chromium (III) uptake capacity of sugarcane bagasse through its chemical modification with citric acid and/or sodium hydroxide. The chemical modifications were confirmed by infrared spectroscopy, with an evident peak observed at 1730 cm-1, attributed to carbonyl groups. Equilibrium was reached after 24 h, and the kinetics followed the pseudo-second-order model. The highest chromium (III) maximum adsorption capacity (MAC) value was found when using sugarcane bagasse modified with sodium hydroxide and citric acid (58.00 mg g-1) giving a MAC value about three times greater (20.34 mg g-1) than for raw sugarcane bagasse.

Especiação de cobre e zinco em urina: importância dos metais em doenças neurodegenerativas

Metals such as copper and zinc are essential for the development and maintenance of numerous enzymatic activities, mitochondrial functions, neurotransmission, and also for memorization and learning. However, disruption in their homeostasis can cause neurodegenerative disorders such as the Alzheimer and Parkinson diseases. In this work, the speciation of copper and zinc in urine samples was carried out. To this end, free and total metal concentrations were determined by square wave anodic stripping voltammetry using a glassy carbon electrode coated with bismuth film. The digestion of the samples was performed in a microwave with the addition of oxidant reagents.