Lead is recognized worldwide as a poisonous metal. Thus, the determination of this element is often required in environmental, biological, food and geological samples. However, these analyses are difficult because such samples contain relatively low concentrations of lead, which fall below the detection limit of conventional analytical techniques such as flame atomic absorption spectrometry and inductively coupled plasma optical emission spectrometry. Several preconcentration procedures to determine lead have therefore been devised, involving separation techniques such as liquid-liquid extraction, solid phase extraction, coprecipitation and cloud point extraction. Citing 160 references, this paper offers a critical review of preconcentration procedures for determining lead using spectroanalytical techniques.
In the present paper, a minicolumn of polyurethane foam loaded with 4-(2-pyridylazo)-resorcinol (PAR) is proposed as pre-concentration system for cadmium determination in drinking water samples by flame atomic absorption spectrometry. The optimization step was performed using two-level full factorial design and Doehlert matrix, involving the variables: sampling flow rate, elution concentration, buffer concentration and pH. Using the established experimental conditions in the optimization step of: pH 8.2, sampling flow rate 8.5 mL min(-1), buffer concentration 0.05 mol L(-1) and elution concentration of 1.0 mol L(-1), this system allows the determination of cadmium with detection limit (LD) (3sigma/S) of 20.0 ng L(-1) and quantification limit (LQ) (10sigma/S) of 64 ng L(-1), precision expressed as relative standard deviation (R.S.D.) of 5.0 and 4.7% for cadmium concentration of 5.0 and 40.0 microg L(-1), respectively, and a pre-concentration factor of 158 for a sample volume of 20.0 mL. The accuracy was confirmed by cadmium determination in the standard reference material, NIST SRM 1643d trace elements in natural water. This procedure was applied for cadmium determination in drinking water samples collected from Salvador City, Bahia, Brazil. For five samples analyzed, the achieved concentrations varied from 0.31 to 0.86 microg L(-1).
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