Effective and High-Throughput Analytical Methodology for the Determination of Lead and Cadmium in Water Samples by Disposable Pipette Extraction Coupled with High-Resolution Continuum Source Graphite Furnace Atomic Absorption Spectrometry (HR-CS GF AAS)

• Published in: Analytical letters 2019-09, Vol.52 (13), p.2133-2149
• Main Authors: Cadorim, Heloisa R., Schneider, Mauana, Hinz, Júlia, Luvizon, Fabiana, Dias, Adriana N., Carasek, Eduardo, Welz, Bernhard
• Format: Article
• Language: English
• Subjects: Absorption spectroscopy; Atomic absorption analysis; Cadmium; cork; disposable pipette tip extraction; Graphite; High resolution; high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS); Lead; Legislation; preconcentration; Quality control; Reference materials; Scanning electron microscopy; Scientific imaging; Spectrometry; Wastewater
• ISSN: 0003-2719; 1532-236X
• DOI: 10.1080/00032719.2019.1596117

A new procedure for the preconcentration of trace amounts of free Pb and Cd by disposable pipette extraction (DPX) is proposed herein. Recycled cork is used as a biosorbent and the procedure is completely free of organic solvents. The cork was reduced to a powder and characterized by scanning electron microscopy. Several parameters that influence the preconcentration of Pb and Cd with DPX-cork, such as the sample pH, number of extraction cycles, biosorbent mass, and percentage of acid in the desorption step, were studied. The tolerance of DPX-cork with respect to 10 potential interfering ions was also evaluated. Coupled with the high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) technique, the sample preparation method allowed the analytical limits required for quality control (according to the permitted limits established by legislation) to be obtained. The limits of detection for the extraction of a 3.5-mL water sample were 200 ng L −1 for Pb and 100 ng L −1 for Cd. The relative standard deviations were around 7.5% for Pb and 8.0% for Cd. The optimized method was successfully applied to the determination of Cd and Pb in two certified reference materials (water and wastewater) and five water samples (collected from a mangrove, a creek, and the sea).