Dispersive micro solid-phase extraction using multiwalled carbon nanotubes combined with portable total-reflection X-ray fluorescence spectrometry for the determination of trace amounts of Pb and Cd in water samples

In this paper the combination of dispersive micro solid-phase extraction (DMSPE), using multiwalled carbon nanotubes (MWCNTs) as solid sorbents, with total-reflection X-ray fluorescence spectrometry (TXRF) is proposed for preconcentration and determination of lead and cadmium ions in water samples. The proposed sample preparation is quite simple and economic. After the sorption processes of the metals on the MWCNTs, the aqueous sample is separated by centrifugation and the metal loaded MWCNTs are suspended using a small volume of an internal standard solution and analyzed directly by TXRF. Parameters affecting the extraction process (complexing agent, pH of the aqueous sample, amount of MWCNTs) and TXRF analysis (volume of the deposited suspension on the reflector, drying mode, and instrumental parameters) have been carefully evaluated to test the real capability of the developed methodology for the determination of Cd and Pb at trace levels. For both elements the linear range is observed up to 50 ng mL(-1). Under optimized conditions detection limits are 1.0 ng mL(-1) and 2.1 ng mL(-1) for Cd(II) and Pb(II) ions, respectively. Both of the examined elements can be determined with quantitative recoveries (ca. 100%) and with an adequate precision (RSD = 6.0% and 10.5% for Cd(II) and Pb(II), respectively). Our results give insight into the possibilities of the combination of DMSPE and TXRF for trace metal determination in different types of environmental waters (sea, river and waste water).This work was supported by the Spanish National Research Program (Project ref. CGL2010-22168-C03-01) and the Bilateral Agreement (Lifelong Learning Program/Erasmus) for the Academic year 2012 – 2013 between the University of Silesia (Poland) and the University of Girona (Spain). Karina Kocot is grateful for the financial support of the UPGOW project, cofinanced by the European Union within the European Social FundPeer Reviewe