Synthesis, spectral assignment and application of a recently synthesized macrocyclic ionophore to simultaneous pre-concentration and determination of ultra traces of copper and lead by solid phase extraction-flame atomic absorption spectrometry.

Ethyl(2-ethylamino)thiophenol-2,6-pyridinedicarboxylate (ETPD) was synthesized from the reaction of disodium pyridine-2,6-dicarboxylate with 1,2-dibromoethane in methanol, followed by treatment with 2-aminothiophenol. The spectral characterization of ETPD is described in detail. This electron-donating agent was successfully utilized for simultaneous enrichment of ultra trace levels of copper and lead in a wide variety of samples. By passing the aqueous solutions through octadecylsilyl bonded phase membrane disks impregnated with 12 mg of ETPD at flow rates of 45 mL min(-1), Cu and Pb were selectively trapped on the disk surface over the pH range 3.0 to 7.0, whereas most other ions were negligibly retained. Numerous chemical parameters affecting sorption and subsequent elution were also investigated. The target ions were stripped from the disk surfaces by reverse flow, at rates of 12 mL min(-1), and were immediately introduced to the nebulizer of an atomic absorption spectrometer. This inexpensive and off-line method offers enrichment factors of 400 and 300 and detection limits of 2.5 and 0.2 μg L(-1) for copper and lead, respectively. The potential applicability of the method was confirmed by its reliable use in quantification of these elements in some real water samples, industrial effluents, three tea samples and peppers, as well as by comparison with graphite furnace atomic absorption spectrometric determinations.