Two synthetic goethites of varying crystal size distributions were analyzed by BET, conventional TEM, cryo-TEM, atomic resolution STEM and HRTEM, and electron tomography in order to determine the effects of crystal size, shape, and atomic scale surface roughness on their adsorption capacities. The two samples were determined by BET to have very different site densities based on Cr adsorption experiments. Model specific surface areas generated from TEM observations showed that, based on size and shape, there should be little difference in their adsorption capacities. Electron tomography revealed that both samples crystallized with an asymmetric {101} tablet habit. STEM and HRTEM images showed a significant increase in atomic-scale surface roughness of the larger goethite. This difference in roughness was quantified based on measurements of relative abundances of crystal faces {101} and {201} for the two goethites, and a reactive surface site density was calculated for each goethite. Singly coordinated sites on face {210} are 2.5 more dense than on face {101}, and the larger goethite showed an average total of 36% {210} as compared to 14% for the smaller goethite. This difference explains the considerably larger adsorption capacitiy of the larger goethite vs the smaller sample and points toward the necessity of knowing the atomic scale surface structure in predicting mineral adsorption processes.

Iron oxyhydroxides, such as goethite and ferrihydrite, are highly abundant and ubiquitous minerals in geochemical environments. Because of their small particle sizes, their surface reactivity is high towards adsorption of anions and cations of environmental relevance. For this reason these minerals are extensively studied in environmental geochemistry, and also are very important for environmental and industrial applications. In the present work, we report the synthesis and characterization of goethite and ferrihydrite of controlled particle sizes. It has been shown that surface reactivity of these minerals is highly dependent on crystal sizes, even after normalizing by specific surface area. In order to investigate the reasons for this changing reactivity it is necessary to work with reproducible particle sizes of these minerals. We investigated here the experimental conditions to synthesize goethite samples of four different specific surface areas: ca. 40, 60, 80 and 100 m 2 g -1 , through the controlled speed of hydroxide addition during hydrolysis of acid Fe(III) solutions. In the case of 2-line ferrihydrite, samples with two different particle sizes were prepared by changing the aging time under the pH conditions of synthesis (pH = 7.5). The synthesized minerals were identified and characterized by: X-ray diffraction, N 2 adsorption BET specific surface area, transmission electron microscopy, attenuated total reflectance Fourier transform infrared spectroscopy, and maximum Cr(VI) adsorption.Keywords: synthesis, iron oxides, specific surface area, goethite, ferrihydrite, particle size. Resumen

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An important target of photoelectrocatalysis (PEC) technology is the development of semiconductor-based photoelectrodes capable of absorbing solar energy (visible light) and promoting oxidation and reduction reactions. Bismuth oxyhalide-based materials BiOX (X = Cl, Br, and I) meet these requirements. Their crystalline structure, optical and electronic properties, and photocatalytic activity under visible light mean that these materials can be coupled to other semiconductors to develop novel heterostructures for photoelectrochemical degradation systems. This review provides a general overview of controlled BiOX powder synthesis methods, and discusses the optical and structural features of BiOX-based materials, focusing on heterojunction photoanodes. In addition, it summarizes the most recent applications in this field, particularly photoelectrochemical performance, experimental conditions and degradation efficiencies reported for some organic pollutants (e.g., pharmaceuticals, organic dyes, phenolic derivatives, etc.). Finally, as this review seeks to serve as a guide for the characteristics and various properties of these interesting semiconductors, it discusses future PEC-related challenges to explore.

Lead ion in drinking water is one of the most dangerous metals. It affects several systems, such as the nervous, gastrointestinal, reproductive, renal, and cardiovascular systems. Adsorption process is used as a technology that can solve this problem through suitable composites. The adsorption of lead (Pb(II)) on graphene oxide (GO) and on two goethite (α-FeOOH)/reduced graphene oxide (rGO) composites (composite 1: 0.10 g GO: 22.22 g α-FeOOH and composite 2: 0.10 g GO: 5.56 g α-FeOOH), in aqueous medium, was studied. The GO was synthesized from a commercial pencil lead. Composites 1 and 2 were prepared from GO and ferrous sulfate. The GO and both composites were characterized by using scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM), Raman spectroscopy, X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and dynamic light scattering (DLS). The adsorption capacity of Pb(II) on the GO and both composites was evaluated through adsorption isotherms. Composite 1 presented a significant agglomeration of α-FeOOH nanorods on the reduced graphene oxide layers. Meanwhile, composite 2 exhibited a more uniform distribution of nanorods. The adsorption of Pb(II) on the three adsorbents fits the Langmuir isotherm, with an adsorption capacity of 277.78 mg/g for composite 2200 mg/g for GO and 138.89 mg/g for composite 1. Composite 2 emerged as a highly efficient alternative to purify water contaminated with Pb(II).