In situ emulsification microextraction using a dicationic ionic liquid followed by magnetic assisted physisorption for determination of lead prior to micro-sampling flame atomic absorption spectrometry

• A dicationic ionic liquid was used as the extraction solvent, for the first time.
• A simple and efficient in situ emulsification microextraction method was developed.
• Magnetic assisted physisorption was used to collect the fine droplets of extraction solvent.
• Ammonium pyrrolidinedithiocarbamate was used for complexation of lead.
• Microsampling flame atomic absorption spectrometry was used to determine trace amounts of lead.

For the first time, a simple and efficient in situ emulsification microextraction method using a dicationic ionic liquid followed by magnetic assisted physisorption was presented to determine trace amounts of lead. In this method, 400 μL of 1.0 mol L−1 lithium bis (trifluoromethylsulfonyl) imide aqueous solution, Li[NTf2], was added into the sample solution containing 100 μL of 1.0 mol L−1 1,3-(propyl-1,3-diyl) bis (3-methylimidazolium) chloride, [pbmim]Cl2, to form a water immiscible ionic liquid, [pbmim][NTf2]2. This new in situ formed dicationic ionic liquid was applied as the acceptor phase to extract the lead-ammonium pyrrolidinedithiocarbamate (Pb-APDC) complexes from the sample solution. Subsequently, 30 mg of Fe3O4 magnetic nanoparticles (MNPs) were added into the sample solution to collect the fine droplets of [pbmim][NTf2]2, physisorptively. Finally, MNPs were eluted by acetonitrile, separated by an external magnetic field and the obtained eluent was subjected to micro-sampling flame atomic absorption spectrometry (FAAS) for further analysis. Comparing with other microextraction methods, no special devices and centrifugation step are required. Parameters influencing the extraction efficiency such as extraction time, pH, concentration of chelating agent, amount of MNPs and coexisting interferences were studied. Under the optimized conditions, this method showed high extraction recovery of 93% with low LOD of 0.7 μg L−1. Good linearity was obtained in the range of 2.5–150 μg L−1 with determination coefficient (r2) of 0.9921. Relative standard deviation (RSD%) for seven repeated measurements at the concentration of 10 μg L−1 was 4.1%. Finally, this method was successfully applied for determination of lead in some water and plant samples.

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