Various crystallite size estimation methods were used to analyze X-ray diffractograms of spherical cerium dioxide and titanium dioxide anatase nanoparticles aiming to evaluate their reliability and limitations. The microstructural parameters were estimated from several integral breadth methods such as Scherrer, Monshi, Williamson–Hall, and their variants: (i) uniform deformation model, (ii) uniform strain deformation model, and (iii) uniform deformation energy density model. We also employed the size–strain plot and Halder–Wagner method. For this purpose, an instrumental resolution function of an Al₂O₃ standard was used to subtract the instrumental broadening to estimate the crystallite sizes and strain, and the linear regression analysis was used to compare all the models based on the coefficient of determination. The Rietveld whole powder pattern decomposition method was introduced for comparison purposes, being the best candidate to fit the X-ray diffraction data of metal-oxide nanoparticles. Refined microstructural parameters were obtained using the anisotropic spherical harmonic size approach and correlated with the above estimation methods and transmission electron microscopy images. In addition, μ-Raman spectra were recorded for each material, estimating the mean crystallite size for comparison by means of a phonon confinement model.

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 (SiO₂), 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 (ζ) 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⁻¹. A nitrogen adsorption–desorption technique was used to determine the specific surface area and to study the porous structure. The functionalized γ-Fe₂O₃ Nps exhibited a Brunauer–Emmett–Teller (BET) specific surface area ranging from 74 to 214 m² g⁻¹ and revealed remarkable uptake capacities to remove Cu(II) and Pb(II) species from aqueous solutions.

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.