This work presents a mechanistic study of the electrochemical synthesis of magnetite nanoparticles (NPs) based on the analysis of the electrochemical impedance spectroscopy (EIS) technique. After a discussion of the mechanisms reported in the literature, three models are devised and a prediction of their EIS spectra is presented. The approach consisted of the simulation of EIS spectra as a tool for assessing model validity, as EIS allows to characterize the relaxation of adsorbed intermediates. The comparison between the simulated impedance spectra and the experimental results shows that the mechanisms proposed to date do not explain all of the experimental results. Thus, a new model is proposed, in which up to three adsorbed intermediate species are involved. This model accounts for the number of loops found in experimental impedance data. The closest approximation of the features found in the experimental spectra by this proposed model suggests a better representation of the reaction mechanism within the evaluated potential range.

The standardization of secondary electrolytic conductivity cells requires the use of a certified reference material. The accepted certification method involves electrochemical impedance spectroscopy (EIS) to estimate the material’s solution resistance. This method normally assumes that the impedance’s imaginary component can be neglected; and hence, the measured impedance approximates the real impedance. Thus, a linear extrapolation of the impedance versus the period (inverse frequency) yields solution resistance. However, experimental impedance data usually do not exhibit a linear behavior over the spectra of frequency, which strongly suggest that the ideal capacitive assumption may not strictly apply. To account for the observed nonlinear behavior, we have proposed to introduce the concept of a constant phase element (CPE) to the analysis of impedance. This approach leads to the development of a relationship that improves the fitting of experimental data and improves the accuracy of the estimation, by establishing a critical frequency where extrapolation should be done. Finally, we are presenting simulated results to demonstrate how sizeable capacitive effects can influence the determination of solution resistance, and a final analysis to estimate the impact on constant cell or electrolytic conductivity values.

Geopolymers have been widely used for construction and building materials. Nevertheless, some other applications have been found from their ability to be ion exchanged. An example is the encapsulation of heavy metals, but some others involve the ion exchange of the aluminosilicate structure to form photoactive particles or to link copper ions. In this chapter, we summarize some of the properties which make aluminosilicate inorganic polymer (geopolymers) ion exchangeable: the synthesized temperature, its effect over their porosity and their stoichiometric nature. Also, the effects of ion exchanging a geopolymer with an NH4+Cl, (NH4)2TiO2(C2O4)2 and (CH3)4N+Br are presented. The geopolymer was characterized by FT-IR, XRD, BET and MAS NMR, showing how a 100% of replacement was achieved for NH4+Cl. On the contrary, the efficiency was reduced in (NH4)2TiO2(C2O4)2 and (CH3)4N+Br, effect ascribed to the fact of the molecular size that did not allow the counterions to reach the aluminum atoms in the geopolymer. Finally, the procedure followed to ion exchange a metakaolinite-based geopolymer is described, and the potential applications related are presented.

Biofuel production has increased significantly in several countries in recent decades. Different evaluation techniques are required for their characterization. The study measures the properties of the obtained biodiesel and a commercial diesel sample, using the techniques of open circuit potential, linear scanning voltammetry and electrochemical impedance spectroscopy. The transesterification reaction between sunflower oil and methanol was carried out with ultrasound as the energy source. The determination of triglyceride conversion to biodiesel is performed by high performance liquid chromatography (HPLC), obtaining up to 99.79% with a yield of 93.40% at a transesterification temperature of 50 ${}^{\circ }$C for 60 min with a methanol/oil molar ratio of 6:1. The potassium hydroxide catalyst concentration was 1.0 g catalyst/100 g oil. The biodiesel samples generally showed open circuit potential (OCP) values less than 790 mV and stabilization time less than 120 s, Linear sweep voltammograms (LSV) show no reaction peaks with current densities on the order of NanoAmpere, Electrochemical impedance spectroscopy (EIS) showed a capacitive system with impedances on the order of MΩ cm${}^2$ at low frequency; This information could help characterize biofuels and other similar materials.