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In the present work, the usefulness of ultrasonic power as a dispersion and mixing tool to accelerate the adsorption of Safranin O (SO), methylene blue (MB), Pb(2+) ions and Cr(3+) ions onto the novel composite Fe3O4-NPs-AC adsorbent was investigated. This new material was extensively characterized and analyzed by different techniques such as XRD, FESEM, Raman spectroscopy and FT-IR. Central composite design (CCD) based on designed runs revealed that adsorbent mass, sonication time, MB concentration, SO concentration, Pb(2+) ion and Cr(3+) ion concentration and some of their interactions have significant contributions to the target compounds removal percentages. A combination of response surface methodology and Design-Expert software was used to qualify and estimate the influence and magnitude of each terms contribution to the response. An optimization study using the following investigated increments of the effective variables, adsorbent mass (0.01-0.03 g), sonication time (2-6 min), initial dye concentration (5-25 mg L(-1)), and initial metal ion concentration (20-60 mg L(-1)), revealed that fixing the experimental variables at 0.025 g of Mn-Fe3O4-NPs-AC, with a 3 min sonication time, and 20 mg L(-1) of MB, 10 mg L(-1) of SO, 38 mg L(-1) of Pb(2+) ions and 42 mg L(-1) of Cr(3+) ions at room temperature lead to the achievement of the best characteristics and performance. Conduction of 32 experiments according to the limitations of CCD and a subsequent analysis of variance (ANOVA) gave useful information about the significant and also approximate contributions of each term (main and interaction of variables) in an empirical equation for the expected response. The results indicate that the R(2) values are more than 0.988 and the adjusted R(2) values are in reasonable agreement with R(2). Under the optimal conditions, the MB, SO, Pb(2+) ion and Cr(3+) ion removal efficiencies reached 99.54%, 98.87%, 80.25% and 99.54% after 3 min, while their equilibrium data with high performance can be represented by Langmuir isotherms and a pseudo second-order kinetic model. The maximum adsorption capacities for the single component system, 229.4 mg g(-1) for MB, 159.7 mg g(-1) for SO, 139.5 mg g(-1) for Pb(2+) ions and 267.4 mg g(-1) for Cr(3+) ions, support the high efficiency of Mn-Fe3O4-NPs-AC as a new adsorbent.

This review (with 151 refs) focuses on recent progress that has been made in magnetic nanoparticle-based solid phase extraction (SPE), pre-concentration and speciation of heavy metal ions. In addition, it discusses applications to complex real samples such as environmental, food, and biological matrices. The introduction addresses current obstacles and limitations associated with established SPE approaches and discusses the present state of the art in different formats of off-line and on-line SPE. The next section covers magnetized inorganic nanomaterials for use in SPE, with subsections on magnetic silica, magnetic alumina and titania, and on magnetic layered double oxides. A further section treats magnetized carbonaceous nanomaterials for use in SPE, with subsections on magnetic graphene and/or graphene oxides, magnetic carbon nanotubes and magnetic carbon nitrides. We then discuss the progress made in SPE based on the use of magnetized organic polymers (mainly non-imprinted and ion-imprinted polymer). This is followed by shorter sections on the use of magnetized metal organic frameworks, magnetized ionic liquids and magnetized biosorbents. All sections include discussions of the nanomaterials in terms of selectivity, sorption capacity, mechanisms of sorption and common routes for material synthesis. A concluding section addresses actual challenges and discusses perspective routes towards further improvements. Graphical abstract An overview on booster nanomaterials (ionic liquids, inorganic, organic and biological materials, and metal-organic frameworks) for use in magnetic nanoparticle-based solid-phase extraction of heavy metal ions.

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