Potencialidades analíticas do dietilditiofosfato de amônio em espectrometria de massas com plasma indutivamente acoplado empregando extração em fase sólida e sistemas de injeção em fluxo

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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

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

Determination of Copper, Iron, Nickel and Zinc in fuel kerosene by FAAS after adsorption and pre-concentration on 2-aminothiazole-modified silica gel

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

External polyacrylate-coating as alternative material for preparation of photopolymerized sol-gel monolithic column

Photopolymerized sol-gel monolithic columns for use in capillary electrochromatography were prepared in 125 mu m i.d. polyacrylate-coated fused-silica capillaries. The polyacrylate-coating, unlike the polyimide one, is transparent to the radiation used (approximate to 370 nm), and thus, no coating removal is necessary. This is a very important particularity since intrinsic capillary column characteristics, such as flexibility and mechanical resistance, are unchanged. A mixture containing metacryloxypropyltrimethoxysilane (MPTMS) as the polymeric precursor, hydrochloric acid as the catalyst, toluene as the porogen and bis(2,4,6-trimethylbenzoyl)-phenylphosphine oxide (Irgacure 819) as the photoinitiator was irradiated at 370 nm for 20 min inside the capillaries to prepare the columns through sol-gel approach. The versatility and viability of the use of polyacrilate as a new capillary external coating were shown through preparation of two columns under different conditions, which were tested in electrochromatography for separation of standard mixture containing thiourea (marker compound), propylbenzene, phenanthrene and pyrene. (C) 2008 Elsevier B.V. All rights reserved.

Optimization of photo-polymerized sol gel monolithic stationary phases prepared in polyacrylate-coated fused-silica capillaries for capillary electrochromatography

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Comportamento fotofísico do antraceno em sistemas micro-heterogêneos argila-surfactantes-íons metálicos

Argilas constituem uma classe de complexos micro-heterogêneos e podem ser utilizados como substrato para adsorção. O seu comportamento de sorção em fase sólida intensificada pela presença de surfactantes, argilas organofílicas, é um importante fenômeno explorado pela tecnologia ambiental para a remoção de compostos orgânicos policíclicos (hidrocarbonetos aromáticos policíclicos, HPA) da água, introduzidos no ambiente por fontes antropogênicas. Este trabalho tem por objetivo estudar o comportamento fotofísico do antraceno, como modelo de HPA, em sistemas micro-heterogêneos argila-surfactantes-íons metálicos (M(II)= Cd(II), Cu(II), Hg(II), Ni(II) e Pb(II); surfactantes: CTACl; SDS; TR-X100). Os estudos foram conduzidos pelo monitoramento na mudança das propriedades de fluorescência estática e na supressão da emissão do antraceno utilizado como sonda fluorescente. Como supressores foram utilizados os cátions metálicos: Cd(II), Cu(II), Hg(II), Ni(II) e Pb(II). O perfil do espectro de fluorescência e os resultados dos ensaios de supressão da fluorescência da sonda permitiram inferir na localização do sítio de solubilização do antraceno nos sistemas micro-heterogêneos estudados e na conseqüente organização dos mesmos.

Enthalpy-entropy compensation based on isotherms of mango

Dados de equilíbrio da umidade da polpa de manga foram determinados utilizando-se o método estático gravimétrico. As isotermas de adsorção e dessorção foram obtidas na faixa de 30-70 ºC e as atividades de água (a w) de 0,02 a 0,97. A utilização do modelo de GAB nos resultados experimentais, através da análise de regressão não linear, proporcionou um bom ajuste entre os dados experimentais e os valores calculados. O calor isostérico de sorção foi estimado a partir dos dados de equilíbrio de sorção, utilizando-se a equação de Clausius-Clayperon. Notou-se que os calores isostéricos de sorção crescem com o aumento da temperatura e pode ser bem ajustado através de uma relação exponencial. A teoria da compensação entalpia-entropia foi aplicada às isotermas de sorção e gráficos deltaH versus deltaS forneceram as temperaturas isocinéticas, indicando um processo de sorção entalpicamente controlado.

Effect of drying method on the adsorption isotherms and isosteric heat of passion fruit pulp powder

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Study of adsorption isotherms of green coconut pulp

O Brasil é considerado um dos maiores produtores e consumidores de frutas tropicais. O coco verde (Cocos nucifera L.) se destaca tanto em termos de produção e consumo quanto em quantidade de resíduos gerada por indústrias de água de coco e pelo consumo in natura. Portanto, existe uma necessidade de aproveitamento deste subproduto. Este trabalho teve por objetivo estudar as isotermas de adsorção da polpa de coco verde e determinação do calor isostérico de sorção. As isotermas de adsorção para as temperaturas de 30, 40, 50, 60 e 70 °C foram analisadas e evidenciaram curvas do tipo III, típicas de alimentos ricos em açúcares. Os dados experimentais de umidade de equilíbrio foram correlacionados por modelos da literatura. O modelo de GAB apresentou melhor concordância com os dados experimentais, entre os modelos avaliados. O calor isostérico de sorção é considerado um indicativo de forças atrativas intermoleculares entre os sítios de sorção de vapor de água, consequentemente, um importante fator para predizer a vida de prateleira de produtos desidratados.

Phase diagram for freeze-dried persimmon

Phase transitions of freeze-dried persimmon in a large range of moisture content were determined by differential scanning calorimetry (DSC). In order to study this transitions at low and intermediate moisture content domains, samples were conditioned by adsorption at various water activities (a(w) = 0.11-0.90) at 25 degreesC. For the high moisture content region, samples were obtained by water addition. At a(w) less than or equal to 0.75 two glass transitions were visible, with T(g) decreasing with increasing water activity due to water plasticizing effect. The first T(g) is due to the matrix formed by sugars and water, the second one, less visible and less plasticized by water, is probably due to macromolecules of the fruit pulp. At a(w) between 0.80 and 0.90 a devitrification peak appeared after T(g) and before T(m). At this moisture content range, the Gordon-Taylor model represented satisfactorily the matrix glass transition curve. At the higher moisture content range (a(w) > 0.90), the more visible phenomenon was the ice melting. T(g) appeared less visible because the enthalpy change involved in glass transition is practically negligible in comparison with the latent heat of melting. In the high moisture content domain T(g) remained practically constant around T(g)' (-56.6 degreesC). (C) 2001 Elsevier B.V. B.V. All rights reserved.

TiO2 films organofunctionalized with 2-aminothiazole ligand and adsorbed Pd(II) ions applied in the photocatalytic degradation of phenol in an aqueous medium

This paper describes the preparation of thin titanium films via sol-gel route and their subsequent chemical modification by anchoring with 2-aminothiazole ligand and Pd(II) ion sorption, aiming to maximize the photocatalytic activity. The material was characterized by diffuse reflectance infrared Fourier transform spectroscopy, ultraviolet and visible spectrometry, X-ray diffractometry, and scanning electronic microscopy. The amount of palladium adsorbed on the film's surface, determined by graphite furnace atomic absorption spectrometry, showed a value of 2.69 x 10(16) atoms CM-2. The photocatalytic tests indicated that the functionalization with 2-aminothiazole and the adsorption of palladium (II) were determinants in the semiconductor's enhanced photocatalytic activity. (c) 2007 Elsevier B.V. All rights reserved.

Thermodynamic and quality properties of lemon juice powder as affected by maltodextrin and Arabic gum

Sorption isotherms of lemon juice (LE) powders with and without additives-18% maltodextrin (MA) or 18% gum Arabic (GA) were determined at 20-50 degrees C. Addition of additives was shown to affect the isotherms in such a way that, at the same water activity, samples LE + GA and LE + MA presented lower equilibrium moisture content and were not so affected by varying temperature. The net isosteric heats of sorption of juice powders with additives were higher (less negative) than those of lemon juice powders, suggesting that there are more active polar sites in the product without addition of GA or MA. In general, the quality properties decreased with the addition of maltodextrin and gum arabic and it was obtained similar values for LE + GA and LE + MA.

Use of sugar cane bagasse as solid phase extractor for cadmium determination by FAAS

The present paper describes the use of sugar cane bagasse as solid phase extractor for cadmium determination after complexation of the analyte with ammonium diethyldithiophosphate (ADDP) and sorption of the Cd-DDP complexes on the solid support. The concomitants were separated using a flow injection analysis (FIA) system coupled to flame atomic absorption spectrometry (FAAS) for determination. The main parameters such as ADDP concentration, acid medium, flow rate, reaction coil length, and reaction time were investigated.The results obtained with HNO3 showed good accuracy and precision. The enhancement factor was 20.5 times for a 120-second preconcentration time, and the analytical frequency was 25 determinations per hour. The calibration curve was linear over the concentration range of 1-40 mu g L-1 Cd with a LOD of 0.697 mu g L-1 Cd and a relative standard deviation of 0.96% after 12 successive measurements of 30 mu g L-1 Cd.The proposed method was evaluated for the FIA-FAAS analysis of certified reference materials (tomato leaves, spinach leaves, and bovine liver) and Cd-spiked foods (shrimp, sardine, tuna, chicken liver and bovine liver). Good recoveries (80.0-97.1%) for the Cd-spiked samples and certified reference materials were obtained. The results of bagasse-packed minicolumns were compared with Si-C,8 packed minicolumns. The F-test was applied between Si-C-18/Bagasse minicolumns, Si-C-18/certified values, and bagasse/certified values. It was found that the results were in agreement with the certified values at a 95% confidence level.

Phosphate functionalization of spongiolite surface

Spongiolite from Mato Grosso do Sul (Brazil), natural inorganic composite constituted of silica needles, was treated with concentrated phosphoric acid at high temperatures. Superficial coating of the needles was proved to be constituted of silicon diphosphate, a compound offering six-coordinated silicon sites. Owing to the affinity of three charged ions to phosphate groups, this coating acts as specific adsorbent for the rare earth elements which prefer octahedral coordination (starting from samarium, yttrium included). The uptake of lanthanum and neodymium are significantly lower due to different coordination tendencies. Lanthanide fixation upon silica with PO4 groups anchored on its surface may be useful in the manufacturing of special phosphate-silicate glasses. (C) 2003 Elsevier B.V. All rights reserved.

An investigation of cadmium(II) and nickel(II) adsorption by chitin graft covolymer

Chitin hydrogels of poly(vinylpyrrolidone) (VP) were prepared by means of the hydrogen peroxide graft copolymerization process. The effect of the VP grafted chain on water diffusion through the biopolymer was studied. Fourier transform infrared spectra of the VP-g-Ch showed an increase in the intensities of the hydroxyl and carbonyl stretching bands indicating a reduction in the hydrogen bonding of chitin. An investigation was undertaken regarding the adsorption of nickel(II) and cadmium(II) ions from aqueous solutions by the VP grafted chitin and the effects of the grafting degree on the Cd2+ and Ni2+ sorption were studied. The Cd2+ and Ni2+ adsorption equilibrium data correlate well with the Freundlich equation. The results indicate that the Ch-g-VP graft copolymer under investigation is a potentially powerful chelating material that can be employed for Ni2+ and Cd2+ ion removal from wastewater effluents. (C) 2004 Wiley Periodicals, Inc.