Abstract
A magnetic Fe3O4@MgAl-layered double hydroxide (MLDH) nanocomposite was successfully synthesized and applied as an effective adsorbent for preconcentration of trace As(III), Cd(II), Cr(III), Co(II), Ni(II), and Pb(II) ions from complex matrices. The quantification of the analytes was achieved using the inductively coupled plasma optical emission spectrometry (ICP-OES) technique. The nanocomposite was then characterized using BET, FTIR, SEM, and EDS. Due to its high adsorption surface area, compared to traditional metal oxide-based adsorbents, MLDH nanocomposite exhibited high extraction efficiency. Several experimental parameters controlling the preconcentration of the trace metals were optimized using response surface methodology based on central composite design. Under optimum conditions, the linearity ranged from 0.1 to 500 µg L−1 and the correlation of coefficients (R2) were higher than 0.999. The limits of detection (LODs) and quantification (LOQs) were 0.11–0.22 µg L−1 and 0.35–0.73 µg L−1, respectively. The intra-day (n = 10) and inter-day precisions (n = 5 working days) expressed in the form of percent relative standard deviations (%RSDs) were below 5%. The proposed method was successfully applied for the analysis of the As(III), Cd(II), Cr(III), Co(II), Ni(II), and Pb(II) ions in different environmental water samples.
Highlights
A magnetic Fe3O4@MgAl-layered double hydroxide (MLDH) nanocomposite was successfully synthesized and applied as an effective adsorbent for preconcentration of trace As(III), Cd(II), Cr(III), Co(II), Ni(II), and Pb(II) ions from complex matrices
Sample preparation methods such as dispersive liquid–liquid micro-extraction (DLLME)[15], solid-phase extraction (SPE)[16,17], dispersive solid-phase microextraction (DSPME), and dispersive magnetic solid-phase extraction (DMSPE)[18], among others have been used for preconcentration of trace metals
These findings suggested that the proposed method had the capability to extract, preconcentrate, and determine trace metals ions in real samples with complex matrices
Summary
A magnetic Fe3O4@MgAl-layered double hydroxide (MLDH) nanocomposite was successfully synthesized and applied as an effective adsorbent for preconcentration of trace As(III), Cd(II), Cr(III), Co(II), Ni(II), and Pb(II) ions from complex matrices. Owing to the low concentration of trace metals in various samples and the complexity of the sample matrices, there is a need for separation/preconcentration methods before ICP-OES determination This is because the preconcentration step improves the LOD/ LOQs, sensitivity, accuracy, and specificity of the analytical technique[14]. Dispersive magnetic solid-phase extraction (DMSPE) is classified as a miniaturized SPE technique because smaller amounts of adsorbents are needed compared to the traditional S PE19 Other advantages of this technique include being easy to carry out, effective, and safe sample preparation method[12]. In this method, the adsorbent is added to the aqueous sample without conditioning step, instead, the sample with the sorbent is dispersed using external forces. The adsorbent is recovered by an external magnet and the analytes are desorbed using an acid[12]
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