Evaluation of the mixtures ammonium phosphate/magnesium nitrate and palladium nitrate/magnesium nitrate as modifiers for simultaneous determination of Cd, Cr, Ni and Pb in mineral water by GFAAS

A method is described for the simultaneous determination of Cd, Cr, Ni and Pb in mineral water samples by graphite furnace atomic absorption spectrometry with a transversely heated graphite atomizer (THGA) and a longitudinal Zeeman-effect background correction system. The electrothermal behavior of analytes during pyrolysis and atomization steps was studied without modifier, in presence of 5 μg Pd and 3 μg Mg(NO3)2 and in presence of 50 μg NH4H2PO4 and 3 μg Mg(NO3)2. A volume of 20 μL of a 0.028 mol L -1 HNO3 solution containing 50 μg L-1 Ni and Pb, 10 μg L-1 Cr and 5 μg L-1 Cd was dispensed into the graphite tube at 20°C. The mixture palladium/magnesium was selected as the optimum modifier. The pyrolysis and atomization temperatures were fixed at 1000°C and 2300°C, respectively. The characteristic masses were calculated as 2.2 pg Cd, 10 pg Cr, 42 pg Ni and 66 pg Pb and the lifetime of the graphite tube was around 600 firings. Limits of detection based on integrated absorbance were 0.02 μg L-1Cd, 0.94 μg L-1 Cr, 0.45 μg L-1 Ni and 0.75 μg L-1 Pb, which exceeded the requirements of Brazilian Food Regulation that establish the maximum permissible level for Cd, Cr, Ni and Pb at 3 μg L-1, 50 μg L-1, 20 μg L-1 and 10 μg L-1, respectively. The recoveries of Cd, Cr, Ni and Pb added to mineral water samples varied within the 93-108%, 96-104%, 87-101% and 98-108% ranges, respectively. Results of analysis of standard reference materials (National Institute of Standards and Technology: 1640-Trace Elements in Natural Water; 1643d-Trace Elements in Water) were in agreement with certified values at the 95% confidence level.

Determination of cadmium in river water samples by flame AAS after on-line preconcentration in mini-column packed with 2-aminothiazole-modified silica gel

A rapid and sensitive method was developed to determine trace levels of Cd2+ ions in an aqueous medium by flame atomic absorption spectrometry, using on-line preconcentration in a mini-column packed with 100 mg of 2-aminothiazol modified silica gel (SiAT). The Cd2+ ions were sorbed at pH 5.0. The preconcentrated Cd2+ ions were directly eluted from the column to the spectrometer's nebulizer-burner system using 100 μL of 2 mol L-1 hydrochloric acid. A retention efficiency of over 95% was achieved. The enrichment factor (calculated as the ratio of slopes of the calibration graphs) obtained with preconcentrations in a mini-column packed with SiAT (A = -1.3 × 10-3 + 1.8 × 10-3 [Cd2+]) and without preconcentrations (A = 4 × 10-5 + 3.5 × 10-3[Cd2+]), was 51 and the detection limit calculated was 0.38 μg L-1. The preconcentration procedure was applied to determine trace levels of Cd in river water samples. The optimum preconcentration conditions are discussed herein.

Use of the internal standardization for difficult sampling by graphite furnace atomic absorption spectrometry

This work shows the potentiality of As as internal standard to compensate errors from sampling of sparkling drinking water samples in the determination of selenium by graphite furnace atomic absorption spectrometry. The mixture Pd(NO 3) 2/Mg(NO 3) 2 was used as chemical modifier. All samples and reference solutions were automatically spiked with 500 μg l -1 As and 0.2% (v/v) HNO 3 by the autosampler, eliminating the need for manual dilutions. For 10 μl dispensed sample into the graphite tube, a good correlation (r=0.9996) was obtained between the ratio of analyte absorbance by the internal standard absorbance and the analyte concentrations. The relative standard deviations (R.S.D.) of measurements varied from 0.05 to 2% and from 1.9 to 5% (n=12) with and without internal standardization, respectively. The limit of detection (LD) based on integrated absorbance was 3.0 μg l -1 Se. Recoveries in the 94-109% range for Se spiked samples were obtained. Internal standardization (IS) improved the repeatability of measurements and increased the lifetime of the graphite tube in ca. 15%. © 2004 Elsevier B.V. All rights reserved.

Determination of copper at wide range concentrations using instrumental features of high-resolution continuum source flame atomic absorption spectrometry

This work describes a method to determine Cu at wide range concentrations in a single run without need of further dilutions employing high-resolution continuum source flame atomic absorption spectrometry. Different atomic lines for Cu at 324. 754 nm, 327. 396 nm, 222. 570 nm, 249. 215 nm and 224. 426 nm were evaluated and main figures of merit established. Absorbance measurements at 324. 754 nm, 249. 215 nm and 224. 426 nm allows the determination of Cu in the 0. 07-5. 0 mg L -1, 5. 0-100 mg L -1 and 100-800 mg L -1 concentration intervals respectively with linear correlation coefficients better than 0. 998. Limits of detection were 21 μg L -1, 310 μg L -1 and 1400 μg L -1 for 324. 754 nm, 249. 215 nm and 224. 426 nm, respectively and relative standard deviations (n = 12) were ≤ 2. 7%. The proposed method was applied to water samples spiked with Cu and the results were in agreement at a 95% of confidence level (paired t-test) with those obtained by line-source flame atomic absorption spectrometry.

Incorporation of dithiooxamide as a complexing agent into cellulose for the removal and pre-concentration of Cu(II) and Cd(II) ions from natural water samples

The present study describes the incorporation of a complexing agent, dithiooxamide, into microcrystalline cellulose for use in the pre-concentration of Cu(II) and Cd(II) ions from aqueous samples. The FTIR spectrum of the adsorbent exhibited an absorption band in the region of 800 cm-1, which confirmed the binding of the silylating agent to the matrix. Elemental analysis indicated the amount of 0.150 mmol g-1 of the complexing agent. The adsorption data were fit to the modified Langmuir equation, and the maximum amount of metal species extracted from the solution, Ns, was determined to be 0.058 and 0.072 mmol g-1 for Cu(II) and Cd(II), respectively. The covering fraction φ, which was 0.39 and 0.48 for Cu(II) and Cd(II), respectively, was used to estimate a 1:2 (metal:ligand) ratio in the formed complex, and a binding model was proposed based on this information. The adsorbent was applied in the pre-concentration of natural water samples and exhibited an enrichment factor of approximately 50-fold for the species studied, which enabled its use in the analysis of trace metals in aqueous samples. The system was validated by the analysis of certified standard (1643e), and the adsorbent was stable for more than 20 cycles, thus enabling its safe reutilization. © 2012 Elsevier B.V. All rights reserved.

The reactive surface of Castor leaf [Ricinus communis L.] powder as a green adsorbent for the removal of heavy metals from natural river water

In this study, a green adsorbent was successfully applied to remove toxic metals from aqueous solutions. Dried minced castor leaves were fractionated into 63-μm particles to perform characterization and extraction experiments. Absorption bands in FTIR (Fourier Transform Infrared Spectroscopy) spectra at 1544, 1232 and 1350 cm-1 were assigned to nitrogen-containing groups. Elemental analysis showed high nitrogen and sulfur content: 5.76 and 1.93%, respectively. The adsorption kinetics for Cd(II) and Pb(II) followed a pseudo-second-order model, and no difference between the experimental and calculated Nf values (0.094 and 0.05 mmol g-1 for Cd(II) and Pb(II), respectively) was observed. The Ns values calculated using the modified Langmuir equation, 0.340 and 0.327 mmol g-1 for Cd(II) and Pb(II), respectively, were superior to the results obtained for several materials in the literature. The method proposed in this study was applied to pre-concentrate (45-fold enrichment factor) and used to measure Cd(II) and Pb(II) in freshwater samples from the Paraná River. The method was validated through a comparative analysis with a standard reference material (1643e). © 2013 Elsevier B.V. © 2013 Elsevier B.V. All rights reserved.

Occurrence of Cu and Cr in the sedimentary humic substances and pore water from a typical sugar cane cultivation area in São Paulo, Brazil

Purpose: The purpose of this paper is to study the interactions of sedimentary humic substances (SHS) from a sugarcane cultivation area with Cu(II) and Cr(III) and to evaluate the occurrence of these metals in the pore water and SHS. Materials and methods: For this study, the northwestern region of the State of São Paulo, Brazil, which is considered the region with the highest production of sugar cane in the state, was selected. Samples of sediment were collected from four sampling sites in the Preto, Turvo, and Grande rivers. The SHS and pore water were extracted from the sediment using the method suggested by the International Humic Substances Society and centrifugation, respectively. The complexing capacity (CC) of the SHS for Cu(II) and Cr(III) was determined by individually titrating these metals with an ultrafiltration system using tangential flow. The total concentrations of Cr and Cu were determined for the pore water, sediments, and humic substances with graphite furnace atomic absorption spectrometry and Zeeman background correction after an acid digestion, according to the methods described in US EPA Method 3050B. Results and discussion: The SHS from a site in the Turvo River, which is typically cultivated with sugarcane, possessed the highest concentration of Cu bound to SHS (25.0%), the largest CC (0.63 mmol Cu g-1 HS) and the highest concentration of this metal in the pore water (1.38 mg Cu Kg-1 sed.). For Cr, the SHS collected from a location on the Preto River dam had the largest CC (0.90 mmol Cr g-1 HS) and the lowest Cr content in the pore water (0.29 mg Cr Kg-1 sed.), indicating that there was an inverse relationship between the CC and the concentration of metal available in the pore water. Conclusions: Sedimentary humic substances might be one of the regulatory factors controlling the availability of Cu and Cr in the sediments found in a typical region that has been planted with sugarcane. Distinct behaviors were observed between the two elements investigated; higher CC and a larger fraction of Cu(II) were found in the pore water of samples originating from sugarcane crops. The opposite behavior was observed for the Cr(III) species. © 2013 Springer-Verlag Berlin Heidelberg.

Cross linked Poly (4-Vinylpyridine-Ethylene Glycol Dimethacrylate) Used for Preconcentration of Cd(II) and its Determination by Flow Injection Flame Atomic Absorption Spectrometry

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Sound absorption coefficient in situ: An alternative for estimating soil loss factors

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

High paracellular nutrient absorption in intact bats is associated with high paracellular permeability in perfused intestinal segments

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

Determination of heavy metals and genotoxicity of water from an artesian well in the city of Vazante- MG, Brazil

The city of Vazante-MG is of great socioeconomic and environmental interest because it is the most important zinc producer district of Brazil. The mineral processing and geochemical processes may determine high concentrations of heavy metals in water intended for human consumption. Thus, the present study aimed to quantify and evaluate the heavy metal genotoxicity of artesian water in the city by Atomic absorption spectrophotometer analysis and testing with the Allium cepa test, respectively. This study reveals a chemical contamination in well water in the city, caused by the presence of heavy metals. Therefore, it can be considered that the high levels of heavy metals found in water samples are correlated with the genotoxic events observed in root cells of A. cepa.

Influence of water immersion and ultraviolet weathering on mechanical and viscoelastic properties of polyphenylene sulfide-carbon fiber composites

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)