José Soares dos Santos

Determination of organic and inorganic mercury species in water and sediment samples by HPLC on-line coupled with ICP-MS

This paper describes a preconcentration method for Hg(2+) and MeHg(+) in water samples using sodium diethyldithiocarbamate immobilized in polyurethane foam (PU-NaDDC) and an extraction method for several mercury species in sediment samples, including MeHg(+), EtHg(+) and PhHg(+), which is simple, rapid, and uses a single organic solvent. Separation and measurement were done by high-performance liquid chromatography on-line with inductively coupled plasma mass spectrometry (HPLC/ICP-MS). Initially, the test of recovery was applied using procedures compatible with HPLC. Under the optimum extraction conditions, recoveries of 96.7, 96.3 and 97.3% were obtained for MeHg(+), EtHg(+), and PhHg(+), respectively, from n=4 spiked sediment samples. This study also demonstrates that the combination of solid-phase extraction on PU-NaDDC with HPLC separation and ICP-MS detection is an effective preconcentration procedure for simultaneous measurement of Hg(2+) and MeHg(+) at ultra-trace levels in water samples. The application of the proposed procedure to the determination of mercury species in drinking water sample was investigated. The proposed method clearly gave satisfactory average recoveries between 93.7 and 101.5%.

Honey classification from semi-arid, Atlantic and transitional forest zones in Bahia, Brazil

In this study, samples of honey produced in three different regional climates in the southwest Bahia, Brazil (semi-arid, Atlantic and Transitional Forest Zones) were characterized on the basis of their mineral and trace elements, ash content and electrical conductivity. The metals were determined by atomic absorption spectrophotometry. The cluster and principal component analysis (PCA) methods were applied to the chemical concentration data in order to study the chemistry variables capable of promoting a characterization of the honey produced in each area. Cluster analysis and PCA distinguishes the different groups of honey samples corresponding to each region of the three geographical origins. The high correlation between electrical conductivity and Cu observed in honey samples from transitional forest zones suggested a coupling to the nutrient cycle, and can be attributed to use of copper compounds in coffee production, a major activity developed in all transitional forest zones.

Comparative study of metal contents in Brazilian coffees cultivated by conventional and organic agriculture applying principal component analysis

The aim of this study was to evaluate of availability of nutrients and toxic elements in green coffees produced in traditional, technological and transitional organic farms in Southwest Bahia-Brazil. Levels of the nutrients minerals were determined directly in samples of soils and coffee tissues from four farms by flame atomic absorption spectrometry (FAAS) and toxic elements (Cr, Ni, Cd and Pb) by inductively coupled plasma optical emission spectrometry (ICP OES). The application of statistical methods (cluster and principal components analysis) revealed the importance of the conversion period to guarantee a product genuinely organic during the change to organic agriculture. On the other hand, the study of correlations between agricultural methods and metals concentrations in coffee suggested that Cd, Cu, Zn and other toxic elements contained in some inorganic fertilizers used in the traditional and technological coffee farms may cause an increase of toxic metals concentration in the crop soil, be taken up by plants, and passed on in the food chain.

Estudo da mobilização de metais e elementos traços em ambientes aquáticos do semi-árido brasileiro aplicando análises de componentes principais

The spatial and temporal retention of metals has been studied in water and sediments of the Gaviao River, Anage and Tremedal Reservoirs, located in the semi-arid region, Bahia - Brazil, in order to identify trends in the fluxes of metals from the sediments to the water column. The determination of metals was made by ICP OES and ET AAS. The application of statistical methods showed that this aquatic system presents suitable conditions to move Cd2+ and Pb2+ from the water column to the sediment.

Influência das características físico-químicas e composição elementar nas cores de méis produzidos por Apis mellifera no sudoeste da Bahia utilizando análise multivariada

In this study honey samples produced in the southwest of Bahia were characterized based on physicochemical and mineral (Ca, Mg, Na, K, Mn, Fe and Zn) composition. The metals were determined by atomic absorption spectrophotometry. The application of multivariate analysis showed that the honey colors are consequence of the mineral and physicochemical compositions. The darkest honey samples are characterized by higher values of pH and for presenting a strong relationship with Ca and Fe content.

Validação de método para a determinação de 5-hidroximetilfurfural em mel por cromatografia líquida e sua influência na qualidade do produto

In honey 5-hydroxymethyl-2-furaldehyde (HMF) is one of the most typical products of degradation: it is usually absent in fresh honey, but its concentration tends to rise as a result of heating processes or long-term storage. The validation protocol was performed in terms of detection and quantification limits, precision (by repeatability and intermediate precision), linearity and accuracy (by recovery tests). The method has been tested on 15 honey samples of different ages and geographical origin. HMF correlated highly with the age of the samples has been considered a very important parameter to put these honeys on the market or not and/or to estimate their shelf life.

Validação de um método para determinação simultânea de quatro ácidos orgânicos por cromatografia líquida de alta eficiência em polpas de frutas congeladas

BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY. Validation of a rapid method for the determination of ascorbic, citric, fumaric and tartaric acids in stored pulp fruit and its application as a quality parameter was performed. The validation parameters showed that for the four evaluated acids, the method presented low limits of detection (LOD) and quantification (LOQ), indicating good precision and accuracy, thus representing an important tool for quality assessment of stored fruit pulp. The results showed that the concentration of organic acids generally decreased with longer storage time in the fruit pulp under study. Amongst all the organic acids under investigation, ascorbic proved the least stable.

Influence of the rainfall regime on the mobility of zn, cd, ni, cu, mn and fe in the surface sediments of the contas river located in the Brazilian semi-arid region

In this study, the influences of the rainfall regimes and of the land use in the mobility of Zn, Cd, Ni, Cu, Mn and Fe in the surface sediment of the Contas River (Bahia State, Brazil) was evaluated with basis on the fractionation method that uses a three-step sequential extraction. The study was conducted in the middle of the Contas River, in an area that encompasses the urban perimeter and part of the rural zone of Jequie City that is influenced by agricultural, urban and industrial activities. The determinations of metals were conducted by flame atomic absorption spectrometry (FAAS). The result obtained from this study indicates that the concentrations of the metals in the soluble fractions of the sediments are directly associated with rainfall indices in the region. The study also indicated that the metals Zn, Cu, Cd and Ni exhibit higher concentrations in the sediments within the city.

Avaliação da salinização de açudes no semi-árido brasileiro por ICP-AES

The salt accumulation process in some reservoirs of regular and irregular use (from 10 to 50 years of constrution), located in the Southeast of Bahia State was evaluated. Inductively coupled plasma atomic emission spectrometry was used to evaluate the concentrations of Na, K, Ca and Mg in water samples from inside and upstream of the reservoirs. The results showed that for reservoirs of irregular use, the salt accumulation, indicated by the tracer Na, increases with the age of the reservoirs, however for the reservoirs of regular use the hydraulic retention time is the main parameter.

Efeitos dos escoamentos urbanos e rurais na qualidade das águas do córrego verruga em vitória da conquista - Bahia, Brasil

This study examined the spatial and temporal variations of 13 physico-chemical parameters in water and sediment samples collected along the rural and urban section of Verruga Stream. The metal concentrations were determined by FAAS. The conductivity and the concentration of Na+, Cl-, and Ca2+ showed the largest variations in the urban area demonstrating that these parameters are appropriate indicators of urban contamination. The application of cluster and principal component analysis showed that the Cd2+ and Mn2+ are associated with the use of fertilizers in the rural area.