Field preconcentration of cadmium from seawater by using a minicolumn packed with Amberlite XAD-4/4-(2-pyridylazo) resorcinol and its flow-injection-flame atomic absorption spectrometric determination at the ng L(-1) Level.
A flow injection analysis-flame atomic absorption spectrometric method for the determination of cadmium in seawater was developed with the aim of yielding a sensitive assay with a low detection limit. The method employs a field flow preconcentration technique involving a minicolumn containing Amberlite XAD-4 impregnated with the complexing agent 4-(2-pyridylazo) resorcinol. A Plackett-Burman 2(7)x3/32 design for seven factors (sample pH, sample flow rate, eluent volume, eluent concentration, eluent flow rate, ethanol percentage in the eluent and minicolumn diameter) was carried out in order to find the significant variables affecting the field continuous preconcentration system (FCPS) and the flow injection elution manifold for cadmium determination in seawater samples by flame atomic absorption spectrometry. Cadmium can be preconcentrated with an enrichment factor of 1053 for a sample volume of 200 mL and a preconcentration time of 57 min. In these experimental conditions, the method provides a linear relationship between absorbance and cadmium concentration in the range from 22-1900 ng L(-1), with a detection limit (3SD) of 6 ng L(-1). The precision (expressed as relative standard deviation) for eleven independent determinations reached values of 8.9-0.8% in cadmium solutions of 50-700 ng L(-1). Analysis of certified reference materials (SLEW-3 and NASS-5) showed good agreement with the certified value. This procedure was applied to the determination of cadmium in seawater from Galicia (Spain).
Yebra
M C
MC
Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, University of Santiago de Compostela, 15782-Santiago de Compostela, Spain. qncayebi@usc.es
Salgado
J
J
Puig
L
L
Moreno-Cid
A
A
D002104:Cadmium / Q000032:analysis* / Q000737:chemistry; D002614:Chelating Agents / Q000737:chemistry; D017022:Flow Injection Analysis / Q000379:methods*; D012118:Resorcinols / Q000737:chemistry; D012623:Seawater / Q000737:chemistry*; D013030:Spain; D013054:Spectrophotometry, Atomic / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000032:analysis*
D002614:Chelating Agents; D012118:Resorcinols; D014874:Water Pollutants, Chemical; D002104:Cadmium; C028398:4-(2-pyridylazo)resorcinol