Removal of mercury(II) ions in aqueous solution using the peel biomass of Pachira aquatica Aubl: kinetics and adsorption equilibrium studies.

Mercury is a highly toxic substance that is a health hazard to humans. This study aims to investigate powders obtained from the peel of the fruit of Pachira aquatica Aubl, in its in natura and/or acidified form, as an adsorbent for the removal of mercury ions in aqueous solution. The materials were characterized by Fourier transform infrared spectroscopy and thermogravimetric analysis. The infrared spectra showed bands corresponding to the axial deformation of carbonyls from carboxylic acids, the most important functional group responsible for fixing the metal species to the adsorbent material. The thermograms displayed mass losses related to the decomposition of three major components, i.e., hemicellulose, cellulose, and lignin. The adsorption process was evaluated using cold-vapor atomic fluorescence spectrometry (CV AFS) and cold-vapor atomic absorption spectrometry (CV AAS). Three isotherm models were employed. The adsorption isotherm model, Langmuir-Freundlich, best represented the adsorption process, and the maximum adsorption capacity was predicted to be 0.71 and 0.58 mg g(-1) at 25 °C in nature and acidified, respectively. Adsorption efficiencies were further tested on real aqueous wastewater samples, and removal of Hg(II) was recorded as 69.6 % for biomass acidified and 76.3 % for biomass in nature. Results obtained from sorption experiments on real aqueous wastewater samples revealed that recovery of the target metal ions was very satisfactory. The pseudo-second-order model showed the best correlation to the experimental data. The current findings showed that the investigated materials are potential adsorbents for mercury(II) ion removal in aqueous solution, with acidified P. aquatica Aubl being the most efficient adsorbent.

Determination of copper in airborne particulate matter using slurry sampling and chemical vapor generation atomic absorption spectrometry.

The present paper describes the development of a method for the determination of copper in airborne particulate matter using slurry sampling and chemical vapor generation atomic absorption spectrometry (CVG AAS). Chemometric tools were employed to characterize the influence of several factors on the generation of volatile copper species. First, a two-level full factorial design was performed that included the following chemical variables: hydrochloric acid concentration, tetrahydroborate concentration, sulfanilamide concentration and tetrahydroborate volume, using absorbance as the response. Under the established experimental conditions, the hydrochloric acid concentration had the greatest influence on the generation of volatile copper species. Subsequently, a Box-Behnken design was performed to determine the optimum conditions for these parameters. A second chemometric study employing a two-level full factorial design was performed to evaluate the following physical factors: tetrahydroborate flow rate, flame composition, alcohol volume and sample volume. The results of this study demonstrated that the tetrahydroborate flow rate was critical for the process. The chemometric experiments determined the following experimental conditions for the method: hydrochloric acid concentration, 0.208 M; tetrahydroborate concentration, 4.59%; sulfanilamide concentration, 0.79%; tetrahydroborate volume, 2.50 mL; tetrahydroborate flow rate, 6.50 mL min(-1); alcohol volume, 200 µL; and sample volume, 7.0 mL. Thus, this method, using a slurry volume of 500 µL and a final dilution of 7 mL, allowed for the determination of copper with limits of detection and quantification of 0.30 and 0.99 µg L(-1), respectively. Precisions, expressed as RSD%, of 4.6 and 2.8% were obtained using copper solutions at concentrations of 5.0 and 50.0 µg L(-1), respectively. The accuracy was evaluated by the analysis of a certified reference material of urban particulate matter. The copper concentration obtained was 570±63 mg kg(-1), and the certified value was 610±70 mg kg(-1). This method was applied for the determination of copper in airborne particulate matter samples collected in two Brazilian regions of Bahia State, Brazil. The copper contents found varied from 14.46 to 164.31 ng m(-3).

Analytical strategies for determination of cadmium in Brazilian vinegar samples using ET AAS.

This paper proposes two methods for determination of cadmium in vinegar employing electrothermal atomic absorption spectrometry. The optimization step was performed using two-level full factorial and Box-Behnken designs, being that a new multiple response function was established. Under experimental conditions of pyrolysis temperature of 640 °C and atomization temperature of 2000 °C, the direct method allows the analysis using the external calibration technique, with limit of quantification of 14 ng L(-1) and characteristic mass of 1.2 pg, having aluminium as chemical modifier. This method was applied in six samples of vinegar acquired from Salvador City, Brazil. The cadmium content varied from 20 to 890 ng L(-1). Other method was also proposed by digestion using nitric acid and hydrogen peroxide in reflux system employing cold finger, being cadmium determined by ETAAS. The results obtained with the complete digestion procedure were in agreement with those found by the direct method proposed herein.

Determination of mercury in phosphate fertilizers by cold vapor atomic absorption spectrometry.

In this paper, a method for the determination of mercury in phosphate fertilizers using slurry sampling and cold vapor atomic absorption spectrometry (CV QT AAS) is proposed. Because mercury (II) ions form strong complexes with phosphor compounds, the formation of metallic mercury vapor requires the presence of lanthanum chloride as a release agent. Thiourea increases the amount of mercury that is extracted from the solid sample to the liquid phase of the slurry. The method is established using two steps. First, the slurry is prepared using the sample, lanthanum chloride, hydrochloric acid solution and thiourea solution and is sonicated for 20 min. Afterward, mercury vapor is generated using an aliquot of the slurry in the presence of the hydrochloric acid solution and isoamylic alcohol with sodium tetrahydroborate solution as the reducing agent. The experimental conditions for slurry preparation were optimized using two-level full factorial design involving the factors: thiourea and lanthanum chloride concentrations and the duration of sonication. The method allows the determination of mercury by external calibration using aqueous standards with limits of detection and quantification of 2.4 and 8.2 µg kg(-1), respectively, and precision, expressed as relative standard deviation, of 6.36 and 5.81% for two phosphate fertilizer samples with mercury concentrations of 0.24 and 0.57 mg kg(-1), respectively. The accuracy was confirmed by the analysis of a certified reference material of phosphate fertilizer that was provided by the National Institute of Standards & Technology (NIST). The method was applied to determine mercury in six commercial samples of phosphate fertilizers. The mercury content varied from 33.97 to 209.28 µg kg(-1). These samples were also analyzed employing inductively coupled plasma mass spectrometry (ICP-MS). The ICP-MS results were consistent with the results from our proposed method.