A Practical Application of Solid-phase Extraction Using a Syringe Filled with Sorbent for the Determination of Lead...

In this study, at first the synthesis of 3-chloro-2-hydroxypropyl methacrylate-ethylene glycole dimethacrylate co-polymer beads and its modification with tris(2-aminoethyl) amine is described. Characterization of the polymer was done by FTIR and SEM. The functional co-polymer was filled in a disposable pipet tip and tightly connected to a 50-mL syringe for the separation and the enrichment of lead and cadmium prior to their determination by flame atomic absorption spectrometry. The sample and then the eluate were subsequently drawn and discharged to retain and desorb lead and cadmium by means of the syringe, respectively. Both analytes were quantitatively retained at pH 4 and eluted using 3.0 mol L^-1 of HNO₃ at flow rates of approximately 10 mL min^-1. Under the optimum conditions, the enrichment factors of up to 50-fold both elements could be obtained by drawing and discharging 250 mL (5 × 50 mL) of the sample, and then 5 mL of the eluent. The recoveries were >90%. The limits of detection (3σ; N = 10 of blank) for Pb and Cd were 0.0034 and 0.0016 mg L^-1 for a 50-fold enrichment, respectively. The analyte concentrations in a certified waste water reference agreed within the certified values in the 95% confidence range.