Determination of cadmium and lead in table salt by sequential multi-element flame atomic absorption spectrometry.
ABSTRACT In the present paper, a simultaneous pre-concentration procedure for the sequential determination of cadmium and lead in table salt samples using flame atomic absorption spectrometry is proposed. This method is based on the liquid-liquid extraction of cadmium(II) and lead(II) ions as dithizone complexes and direct aspiration of the organic phase for the spectrometer. The sequential determination of cadmium and lead is possible using a computer program. The optimization step was performed by a two-level fractional factorial design involving the variables: pH, dithizone mass, shaking time after addition of dithizone and shaking time after addition of solvent. In the studied levels these variables are not significant. The experimental conditions established propose a sample volume of 250mL and the extraction process using 4.0mL of methyl isobutyl ketone. This way, the procedure allows determination of cadmium and lead in table salt samples with a pre-concentration factor higher than 80, and detection limits of 0.3ngg(-1) for cadmium and 4.2ngg(-1) for lead. The precision expressed as relative standard deviation (n = 10) were 5.6 and 2.6% for cadmium concentration of 2 and 20ngg(-1), respectively, and of 3.2 and 1.1% for lead concentration of 20 and 200ngg(-1), respectively. Recoveries of cadmium and lead in several samples, measured by standard addition technique, proved also that this procedure is not affected by the matrix and can be applied satisfactorily for the determination of cadmium and lead in saline samples. The method was applied for the evaluation of the concentration of cadmium and lead in table salt samples consumed in Salvador City, Bahia, Brazil.
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ABSTRACT: A novel manganese dioxide (MnO2) resin is suitable for the determination and decontamination of lead isotopes (208Pb, 207Pb, 206Pb) in aqueous solutions at trace concentrations. This is desirable due to the toxic nature and high abundance of lead in the environment. Current techniques are both time consuming, expensive and not suitable for low-level lead decontamination. The MnO2 resin has been demonstrated to pre-concentrate with extraction efficiency above 90% for a range of pH values, and with a mean extraction of 92.5% from fresh waters at a flow rate of 100 ml min−1. The lead distribution coefficient is 1.3 × 104 (pH 7) with tolerance to calcium and sodium. Adsorption isotherms have been investigated and the resin shown to follow the Langmuir adsorption isotherm with a saturation point of 41.5 mg per g of MnO2 resin.Environmental Earth Sciences 10/2011; 67(3). DOI:10.1007/s12665-011-1509-7 · 1.77 Impact Factor
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ABSTRACT: In the present work, a slurry sampling flame atomic absorption spectrometric method to determine directly manganese and zinc in powdered chocolate samples is proposed. The optimization step was performed using univariate methodology involving the following factors: nature and concentration of the acid solution, sonication time, and particle size. The established conditions led to the use of a sample mass of 150 mg, 2.0 mol L− 1 nitric acid solution, sonication time of 15 min, and a slurry volume of 50 mL. This method allows the determination of manganese and zinc with detection limit of 52 and 61 ng g− 1, respectively, and a precision expressed as relative standard deviation (RSD) of 2.6% and 3.2% (both, n = 10) for contents of manganese and zinc of 52.4 and 100.0 μg g− 1, respectively. The proposed method was applied for determination of manganese and zinc in five powdered chocolate samples. In these, the manganese content varied from 42.8 to 52.7 and from 88.6 to 102.4 μg g− 1 of zinc. The analytical results were compared with the results obtained by analysis of these samples after digestion using open vessel and acid bomb digestion procedures and determination using FS-FAAS. The statistical comparison by t-test (95% confidence level) showed no significant difference between these results.Microchemical Journal 04/2006; 82(2-82):159-162. DOI:10.1016/j.microc.2006.01.008 · 3.58 Impact Factor