Preparação e caracterização de substratos SERS ativos: um estudo da adsorção do cristal violeta sobre nanopartículas de prata

The structural characterization of molecules used in the sterilization of blood for transfusions, such as crystal violet (CV), is relevant for understanding the action of these prophylactic drugs. The characterization is feasible by surface enhanced resonance Raman spectroscopy (SERRS) of CV in solution or on surfaces. The limit of detection of CV by SERRS, in the presence of colloidal particles, using 514.5 nm as excitation radiation, was found to be around 1 ppb. The characterization of CV was also made by SERS, by using different active-particles-containing substrates, proving the versatility of this technique for the study of such structures. The results suggest that the controlled production of highly efficient SERS-active substrates may allow qualitative and quantitative analysis, with high sensitivity, with potential applications in medical and environmental fields.

Preparação de amostra de fígado bovino e estudo de micro homogeneidade para a determinação de Cd E Pb por espectrometria de absorção atômica com atomização eletrotérmica e amostragem direta de sólido

This work describes a systematic study for bovine liver sample preparation for Cd and Pb determination by solid sampling electrothermal atomic absorption spectrometry. Samples were prepared using different procedures: (1) drying in a household microwave oven followed by drying in a stove at 60 ºC until constant mass, and (2) freeze-drying. Ball and cryogenic mills were used for grinding. Particle size, sample size and micro sample homogeneity were investigated. All prepared samples showed good homogeneity (He < 10) even for low sample mass, but samples dried in a microwave oven/stove and ground in a ball mill presented the best homogeneity.

Adsorção de íons dicromato nos compósitos celulose/ZrO2.nH2O preparados pelos métodos da precipitação convencional e em solução homogênea

This article describes the preparation and characterization of the cellulose/ hydrated zirconium oxide composites prepared by conventional precipitation (PC) and homogeneous solution precipitation (PSH) methods. The composite obtained by the PC method was prepared by using an ammonia solution as the precipitating agent, while the composite obtained by the PSH method was prepared by using urea as the precipitating agent. The adsorption of dichromate ions on the composites was studied using factorial design 2³. The variables were: initial concentration, agitation time and mass of the composite. The data obtained agree better for the composite obtained by the PC method.

O emprego de quitosana quimicamente modificada com anidrido succínico na adsorção de azul de metileno

The adsorption capacity of alpha-chitosan and its modified form with succinic anhydride was compared with the traditional adsorbent active carbon by using the dye methylene blue, employed in the textile industry. The isotherms for both biopolymers were classified as SSA systems in the Giles model, more specifically in L class and subgroup 3. The dye concentration in the supernatant in the adsorption assay was determined through electronic spectroscopy. By calorimetric titration thermodynamic data of the interaction between methyene blue and the chemically modified chitosan at the solid/liquid interface were obtained. The enthalpy of the dye/chitosan interaction gave 2.47 ± 0.02 kJ mol-1 with an equilibrium constant of 7350 ± 10 and for the carbon/dye interaction this constant gave 5951 ± 8. The spontaneity of these adsorptions are reflected by the free Gibbs energies of -22.1 ± 0.4 and -21.5 ± 0.2 kJ mol-1, respectively, found for these systems. This new adsorbent derived from a natural polysaccharide is as efficient as activated carbon. However 97% of the bonded dye can be eluted by sodium chloride solution, while this same operation elutes only 42% from carbon. Chitosan is efficient in dye removal with the additional advantage of being cheap, non-toxic, biocompatible and biodegradable.

Funciones termodinámicas relativas a la transferencia del ketoprófen desde el agua hasta algunos sistemas orgánicos

The thermodynamics of molal partitioning of ketoprofen (KTP) was studied in cyclohexane/buffer (CH/W), octanol/buffer (ROH/W), and dimyristoyl phosphatidylcholine (DMPC), dipalmitoyl phosphatidylcholine (DPPC), and egg lecithin (EGG/W) liposome systems. In all cases the partition coefficients (Kmo/w)were greater than unity; therefore the standard free energies of transfer were negative indicating affinity of KTP for organic media. The Kmo/w values were approximately seventy-fold higher in the ROH/W system compared with the CH/W system. On the other hand, the Kmo/w values were approximately ten or fifty-fold higher in the liposomes compared with the ROH/W system. In all cases, the standard enthalpies and entropies of transfer of KTP were positive indicating some degree of participation of the hydrophobic hydration on partitioning processes.

Adsorção de aminoácidos sobre minerais e a origem da vida

Minerals adsorb more readily amino acids with charged R groups than those with uncharged R groups, so that the incorporation of amino acids with charged R groups into peptides would be more frequent than that of amino acids with uncharged R groups. However, 74% of the amino acids in the proteins of modern organisms contain uncharged R groups. Thus, what could have been the mechanism that produced peptides/proteins with more amino acids with uncharged R groups than precursors with charged R groups? The lipid world offers an alternative view of the origin of life. In the present paper, several other mechanisms are also discussed.

Elucidando os estados de oxidação do nitrogênio através da espectroscopia de absorção de raios-X na borda K do nitrogênio

The potentialities of X-ray Absorption Near Edge Spectroscopy (XANES) of the N K edge (N K) obtained with the spherical grating monochromator beam line at the Brazilian National Synchrotron Light Laboratory are explored in the investigation of poly(aniline), nanocomposites and dyes. Through the analysis of N K XANES spectra of conducting polymers and many other dye compounds that are dominated by 1s®p* transitions, it was possible to correlate the band energy value with the nitrogen oxidation states. An extensive N K XANES spectral database was obtained, thus permitting the elucidation of the nature of different nitrogens present in the intercalated conducting polymers.

Adsorção de glifosato sobre solos e minerais

Glyphosate, an enzyme inhibitor herbicide, has been widely used around the world in agriculture. Dr. John Franz from Monsanto Corporation (USA) discovered glyphosate in 1970. It has been showed that glyphosate is strongly adsorbed by inorganic soil components especially aluminium and iron oxides, and the phosphate group is involved in this interaction. The inactivation of glyphosate in soils can last for days or even months depending on soil characteristics. The addition of phosphate from fertilizers can displace glyphosate from the soils and this could be the cause of decreased productivity of some crops.

Integração de técnicas analíticas e proposta de experimentos para cursos de graduação em análise instrumental: uso de espectrômetro de absorção atômica para medidas de absorção molecular

Simple experiments are proposed for measuring molecular absorption of chromate and dichromate ions using an atomic absorption spectrometer. The experiments can help undergraduate students in instrumental analysis courses understand important aspects involving conceptual and instrumental similarities and differences between frequently used analytical techniques. Hollow cathode lamps were selected with wavelengths in the region of molecular absorption of chromate and dichromate. Calibration curves were obtained and the linear dynamic range was evaluated. Results were compared with those obtained in a molecular absorption spectrometer. The molar absorptivities obtained were also compared.

Influência da espessura nas propriedades de absorção e emissão e na morfologia de filmes automontados de poli(p-fenileno vinileno)

In this report, we studied the thickness effect on the optical and morphological properties of self-assembled (SA) poly(p-phenylenevinylene) (PPV) films, wich were processed with 5 and 75 layers from a PPV precursor polymer and dodecylbenzenesulfonate, and then, thermally converted at 230 °C. The increase of the film thickness yielded more intense peaks in the vibrational spectral range. The electron-phonon coupling was quantified by the Huang - Rhys factor, that shows the effects on the polymer chain mobility in the interface substrate/polymer. A strong emission anisotropy r=0.57 was observed for the film with 5 layers of thickness decreasing to 0.34 for the film with 75 layers. Finally, the surface topology of the films was measured using Atomic Force Microscopy.

Adsorção de fenol sobre carvão ativado em meio alcalino

The present study describes phenol adsorption on commercial active carbon (CAF) under alkaline conditions in the concentration range of 0.01 to 2.08 mmol L-1. Surface characterization has been performed by means of surface area measurements, IR spectroscopy and Boehm titration. The effect of temperature on the adsorption equilibrium isotherm was investigated at 23, 30, 40, 50 and 60 °C. The results showed that adsorption capacity decreased with increasing temperature. The adsorption kinetics and the role of surface characteristics on the adsorption of phenol also discussed.

Estudo termogravimétrico do efeito da temperatura e da atmosfera na absorção de dióxido de enxofre por calcário

Thermogravimetry was applied to investigate the effects of temperature and atmosphere on conversion of sulfur dioxide (SO2) absorbed by limestone. Ranges of temperature and particle size were studied, typical of fluidized-bed coal combustion. Isothermal experiments were performed at different temperatures (between 750 and 950 ºC) under local atmospheric pressure (~ 697 mmHg) in dynamic atmospheres of air and nitrogen. The maximum conversion was 29% higher in nitrogen atmosphere than in air atmosphere. The optimum conversion temperature was found at 831 ºC in air atmosphere and at 894 ºC in nitrogen atmosphere.

Desempenho de biomassas na adsorção de hidrocarbonetos leves em efluentes aquosos

Removal of hydrocarbons from aqueous effluents using biosorbents was investigated. The effluent was simulated by a dispersion of gasoline (simple hydrocarbons) in water. Corn-cob, wood powder, coconut mesocarp and sugar-cane bagasse were used as adsorbents and their performance verified by means of batch experiments performed in an agitated vessel. The influence of input variables such as hydrocarbon concentration, mass of biomass and agitation level on the adsorbents' capacity was studied by means of factorial design. The results indicated that, among the materials studied, coconut mesocarp and sugar-cane bagasse can be considered promising biomasses for treating aqueous effluents contaminated by hydrocarbons.

Adsorção de íons cobre(II) pela quitosana usando coluna em sistema sob fluxo hidrodinâmico

The adsorption of Cu(II) ions from aqueous solution by chitosan using a column in a closed hydrodynamic flow system is described. The adsorption capacities as a function of contact time of copper(II) ions and chitosan were determined by varying the ionic strength, temperature and the flow of the metal solution. The Langmuir model reproduced the adsorption isothermal data better than the Freundlich model. The experimental kinetic data correlate properly with the second-order kinetic reaction for the whole set of experimental adsorption conditions. The rate constants exercise great influence on the time taken for equilibrium to be established by complexation or electrostatic interaction between the amino groups of chitosan and the metal.

Influência da adição de plastificante do processo de reticulação na morfologia, absorção de aguá e propriedades mecânicas de filmes de alginato de sódio

The effects of sorbitol and formaldehyde on the morphology, water absorption and mechanical properties of sodium alginate films were analyzed. The morphology of the films indicated the presence of small aggregates in the surface of uncrosslinked films, which disappeared with the crosslinking process. The water uptake and percentage of elongation increased with the addition of sorbitol in uncrosslinked films. At the same time, a decrease in tensile strength and Young's modulus occurred. The swelling ratio and water uptake of crosslinked alginate/sorbitol films decreased with an increase in sorbitol content suggesting an enhanced crosslinking density due to the presence of plasticizer.