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Updated: Sep 20, 2025

Characterization, Quantification and Compound-specific Isotopic Analysis of Pyrogenic Carbon Using Benzene Polycarboxylic Acids BPCA
Published on: May 16, 2016
Vortex-assisted restricted access-based supramolecular solvent microextraction of trace Pb(II) ions with
Aslıhan Karatepe1, Mustafa Yemen1, Faruk Kayapa1
1Nevşehir Hacı Bektaş Veli University, Faculty of Arts and Science, Department of Chemistry, 50300, Nevşehir, Turkey.
Abstract:
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 (1H- NMR), Carbon-13 Nuclear Magnetic Resonance (13C 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-1 and 2.29 μg L-1, respectively. Linear range was found between 15.1 μg L-1 and 606 μg L-1. 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.
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