Abstract
A new Fe 3O 4/polyaniline nanoparticle (PANI) material has been successfully developed as magnetic solid-phase extraction sorbent in dispersion mode for the determination of methylmercury (MeHg) in aqueous samples, via quantification by gas chromatography/mass spectrometry (GC–MS). The resultant core–shell magnetic solid-phase extraction nanoparticle (MSPE-NP) sorbent was characterized by scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDS) and Fourier transform-infrared (FTIR) spectroscopy. Fe 3O 4/PANI composites showed fibrous structure with diameters between 50 and 100 nm for fibers. The MSPE-NP process involved the dispersion of the Fe 3O 4/PANI nanoparticles in water samples with sonication, followed by magnetic aided retrieval of the sorbent and then, solvent (hexane) desorption of extracted MeHg for GC–MS analysis. The extraction, derivatization and adsorption conditions were optimized by selecting the appropriate extraction parameters including the amount of sorbent, extraction time, derivatizing reagent volume and extraction solvent. The calibration graph was linear in the concentration range of 0.5–300 ng mL −1 ( R 2 > 0.993) with detection limit of 0.1 ng mL −1 ( n = 3), while the repeatability was 4.1% ( n = 5). Enrichment factor was obtained as 91. Seawater sample was analyzed as real sample and good recoveries (>98%) were obtained at different spiked values.
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