Vortex-assisted restricted access-based supramolecular solvent microextraction of trace Pb(II) ions with 4-(benzimidazolisonitrosoacetyl)biphenyl as a complexing agent before microsampling flame AAS analysis.

A new oxime compound, 4-(benzimidazolisonitrosoacetyl)biphenyl (BIBP) was synthesized and used as a complexing agent in this study to preconcentrate trace amounts of Pb(II) ions with vortex-assisted restricted access-based supramolecular solvent microextraction (RA/SUPRAS-LPME) method. The new complexing agent was characterized by a combination of elemental analyses, Proton Nuclear Magnetic Resonance (H- NMR), Carbon-13 Nuclear Magnetic Resonance (C NMR) and Fourier Transform Infrared spectroscopy (FT-IR) and techniques. Extraction of the complex which was formed at pH 8.0 was done by using a supramolecular solvent phase of tetrahydrofuran (THF) and 1-decanol. A microsampling flame atomic absorption spectrophotometer was used to measure the lead ion concentrations of the extract. The method optimized and the optimum experimental conditions were found as; pH = 8, amount of the ligand 2,25 mg, supramolecular solvent volume 50 μL, sample volume 20 mL and vortex time 3 min. The limit of detection (LOD), limit of quantification (LOQ) were calculated as 0.69 μg L and 2.29 μg L, respectively. Linear range was found between 15.1 μg L and 606 μg L. The developed method was applied to Pb(II) determination in real samples after evaluating the accuracy by using the TMDA-53.3 fortified environmental water sample as certified reference material.