Arsenic and lead heavy metals are polluting agents still present in water bodies, including surface (lake, river) and underground waters; consequently, the development of new adsorbents is necessary to uptake these metals with high efficiency, quick and clean removal procedures. Magnetic nanoparticles, prepared with iron-oxides, are excellent candidates to achieve this goal due to their ecofriendly features, high catalytic response, specific surface area, and pulling magnetic response that favors an easy removal. In particular, nanomagnetite and maghemite are often found as the core and primary materials regarding magnetic nanoadsorbents. However, these phases show interesting distinct physical properties (especially in their surface magnetic properties) but are not often studied regarding correlations between the surface properties and adsorption applications, for instance. Thus, in this review, we summarize the main characteristics of the co-precipitation and thermal decomposition methods used to prepare the nano-iron-oxides, being the co-precipitation method most promising for scaling up processes. We specifically highlight the main differences between both nano-oxide species based on conventional techniques, such as X-ray diffraction, zero and in-field Mössbauer spectroscopy, X-ray photoelectron spectroscopy, X-ray absorption spectroscopy, and X-ray magnetic circular dichroism, the latter two techniques performed with synchrotron light. Therefore, we classify the most recent magnetic nanoadsorbents found in the literature for arsenic and lead removal, discussing in detail their advantages and limitations based on various physicochemical parameters, such as temperature, competitive and coexisting ion effects, i.e., considering the simultaneous adsorption removal (heavy metal–heavy metal competition and heavy metal–organic removal), initial concentration, magnetic adsorbent dose, adsorption mechanism based on pH and zeta potential, and real water adsorption experiments. We also discuss the regeneration/recycling properties, after-adsorption physicochemical properties, and the cost evaluation of these magnetic nanoadsorbents, which are important issues, but less discussed in the literature.

Applying a modified coprecipitation method, maghemite and anatase nanoparticles embedded in graphene oxide and multiwall carbon nanotube frameworks were prepared, and a detailed structural characterization is presented. Transmission electron images have revealed that the multiwall carbon nanotubes and graphene oxide act as substrates to reduce the nanoparticle agglomeration with narrow sizes of ca. 9–20 nm, in agreement with the results of the Rietveld refinement, which have also indicated their crystallite apparent size and shapes using the spherical harmonics approach. In structural studies of maghemite nanoparticles by Raman spectroscopy, it was found that the effect of optical density and laser power intensity plays a significant role. When no optical filter was located between the powder sample and the laser source, a transformation from the γ-Fe2O3 to the α-Fe2O3 phase was observed, as demonstrated by the disappearance of the characteristic broad Raman peak (A1g) of the γ-Fe2O3 phase when increasing the laser power. X-ray photoelectron spectroscopy has also brought insights into the functionalization mechanism, suggesting that the one-pot reduction of the graphene oxide is favored by the alkaline γ-Fe2O3 nanoparticle growth. The temperature dependence of the 57Fe Mössbauer spectra has indicated that the effective anisotropy constant of Fe oxide-based nanoparticles is similar to that of bulk maghemite, and magnetic relaxation of Fe3+ spins depends on particle sizes.

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Novel magnetic zeolite type 5A nanocomposites were synthesized by the co-precipitation method and applied to lead removal from aqueous ambient. Maghemite nanoparticles were mixed with zeolite and, by controlling its content, transmission electron microscopy results gave sizes of 5 to 15 nm and selected area electron diffraction patterns confirmed the presence of zeolite. The nanocomposites have high specific surface area with values up to 194 m2/g. Magnetization measurements proved superparamagnetic behavior with saturation values of ~35 emu/gFe. Kinetic adsorption experiments showed removal efficiencies of 99.9% and an enhanced equilibrium time of 5 min. The lead concentrations after adsorption experiments lay under the permissible levels of 10 μg L−1, according to the World Health Organization. The maximum adsorption capacity, estimated by Sips model, was 265 mg L−1 at 300 K. The removal efficiency was significantly improved in the range of pH > 6, as well as in the presence of cation interferents such as Ca(II), Cu(II), and Cd(II). The adsorption mechanism was explained with cation exchange between Pb(II), the zeolite framework, and the protonated maghemite surface. Besides, our system revealed recyclability even after seven regeneration cycles. Thus, our synthesized materials have remarkable adsorption properties for lead water remediation processes.

In this study, magnetic nanocomposites were developed and used as adsorbents for lead and copper from aqueous media. Structural, surface, magnetic and textural properties of functionalized maghemite nanoparticles synthesized by alkaline co-precipitation were studied. The surfaces of the iron oxide nanoparticles (Nps) were modified with different chemical agents such as fatty and amino acids, silica (SiO 2), mesoporous silica (SBA-15), hydroxyapatite, multiwall carbon nanotubes (MWCNTs) and ethylenediaminetetraacetic acid (EDTA), obtaining NPs with mean particle sizes ranging from 7 to 16 nm according to Rietveld refinement and TEM images analysis. The physicochemical surface properties of the functionalized materials were studied via zeta potential (z) and Fourier transform infrared (FTIR) spectroscopy. Mössbauer spectroscopy (MS) as a function of temperature and DC magnetometry were used to study the magnetic properties. The superparamagnetic relaxation was studied by MS. The resolved spectra at 20 K confirm the presence of nanomaghemite phase. Besides, the saturation magnetization varies from 12 to 62 emu g À1. A nitrogen adsorption-desorption technique was used to determine the specific surface area and to study the porous structure. The functionalized g-Fe 2 O 3 Nps exhibited a Brunauer-Emmett-Teller (BET) specific surface area ranging from 74 to 214 m 2 g À1 and revealed remarkable uptake capacities to remove Cu(II) and Pb(II) species from aqueous solutions.