A MoS42−-intercalated magnetic FeMgAl layered double hydroxide (Fe3O4@MoS42−-FeMgAl LDH) nanocomposite was synthesised via hydrothermal assisted exfoliation. The material was applied as the adsorbent for extraction, preconcentration and removal of cadmium ions (Cd2+) and lead ions Pb2+ from wastewater and river water. The structural properties and morphologies of the adsorbent were determined by transmission electron microscopy (TEM), scanning electron microscopy coupled with energy dispersive spectroscopy (SEM/EDS), Fourier transform infrared spectroscopy (FTIR), zeta potential and X-ray diffraction (XRD). The parameters influencing preconcentration and the adsorptive removal process were optimised using the central composite design (CCD) method. The concentration of Cd2+ and Pb2+ in the samples was determined using inductively coupled plasma optical emission spectrometry (ICP-OES). The preconcentration method developed in the study was ultrasound-assisted magnetic solid phase extraction (UA-MSPE). Under optimum conditions, linearity was 0.1-800 µg/L with a correlation of determination (R2) of 0.9987. The uncertainty of the slope and the uncertainty of the intercept were both lower than the uncertainty of the calibration indicating good precision, selection of standards closest to a blank and wide range. Precision expressed as %RSD for both intra-day (n = 27) and inter-day (n = 9) were found to be 3.3 % and 7.0 % respectively. The limit of detection (n = 10) and limit of quantification (n = 10) of the UA-MSPE/ICP-OES were 0.03 µg/L and 0.10 µg/L. The developed method was applied for real sample analysis. Herein, influent wastewater was reported as 1.77 ± 0.14 and 6.53 ± 0.33 ug/L for Cd2+ and Pb2+, respectively while the effluent was reported at 0.96 ± 0.07 and 2.57 ± 0.13 ug/L, respectively. River water samples were found to be 0.45 ± 0.01 and 1.23 ± 0.04 ug/L, respectively proving that the adsorbent is capable of preconcentrating the target analytes.
Read full abstract