Preconcentration and determination of copper in tobacco leaves samples by using a minicolumn of sisal fiber (Agave sisalana) loaded with Alizarin fluorine blue by FAAS.

In the present study, a minicolumn of sisal fiber loaded with alizarin fluorine blue is proposed as a preconcentration system for copper determination in tobacco leaf samples by flame atomic absorption spectrometry. During the optimization procedure, a two level full factorial design (2(4)) was used at the preliminary evaluation of four factors, involving the following variables: sampling flow rate, elution flow rate, buffer concentration and pH. Regarding the studied levels, this design has shown that buffer concentration and pH were significant factors. The experimental conditions established in the optimization step were: pH=4.75, buffer concentration of 0.005 mol L(-1) for elution with HCl 1.0 mol L(-1) this system allows the determination of copper content with a detection limit (LD) of 0.018 µg L(-1) and a quantification limit (LQ) of 0.061 µg L(-1) precision expressed as relative standard deviation (R.S.D.) of 4.65 and 5.07%, utilizing concentration of 10 and 2.0 µg L(-1), respectively, and a preconcentration factor of 75, for a sample volume of 50.0 mL. Accuracy was confirmed by copper determination in the standard reference material, NIST SRM 1570 a trace element units in Spinach Leaves and by spike tests with recovery levels ranging from 93 to 100%; the procedure was applied for copper determination in tobacco leaf samples collected in Cruz das Almas City, Bahia, Brazil. The achieved concentrations of the three samples analyzed varied from 0.15 to 0.52 µg g(-1).

Direct determination of iron and manganese in wine using the reference element technique and fast sequential multi-element flame atomic absorption spectrometry.

A procedure is proposed for the direct determination of manganese and iron in wine employing fast sequential flame atomic absorption spectrometry and the reference element technique to correct for matrix effects. Cobalt, silver, nickel and indium have been tested as reference elements. The results demonstrated that cobalt and indium at a concentration of 2 and 10mgL(-1) were efficient for quantification of manganese and iron, respectively. Under these conditions, manganese and iron could be determined with quantification limits of 27 and 40microg L(-1), respectively. The proposed method was applied to the determination of manganese and iron in 16 wine samples. The content of manganese varied from 0.78 to 2.89mgL(-1) and that of iron from 0.88 to 9.22mgL(-1). The analytical results were compared with those obtained by inductively coupled plasma optical emission spectrometry after complete mineralization using acid digestion. The statistical comparison by a t-test (95% confidence level) showed no significant difference between the results.

Review of procedures involving separation and preconcentration for the determination of cadmium using spectrometric techniques.

Spectrometric techniques for the analysis of trace cadmium have developed rapidly due to the increasing need for accurate measurements at extremely low levels of this element in diverse matrices. This review covers separation and preconcentration procedures, such as electrochemical deposition, precipitation, coprecipitation, solid phase extraction, liquid-liquid extraction (LLE) and cloud point extraction (CPE), and consider the features of the their application with several spectrometric techniques.

An on-line pre-concentration system for determination of cadmium in drinking water using FAAS.

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).