Accurate iron quantification in colloids and nanocomposites by a simple UV-Vis protocol.

The selection and comparative study is reported of calibration curves to quantify iron by a simple UV-Vis protocol based on the formation of iron (III) chloride complexes. The reliability of each calibration curve was evaluated using statistical and analytical parameters. The robustness of each calibration curve using superparamagnetic iron oxide nanoparticles (SPIONs) of different sizes and surface functionalization is demonstrated . We have also evaluated the effect of the particle coating and estimated the minimum time to ensure the full oxidation of iron (II) to (III) in sample solutions. Results from UV-Vis are comparable with those obtained from ICP-OES and from other spectroscopic techniques to quantify the iron. We advocate the proposed protocol as a simple and non-expensive route to determine accurately the iron content in colloidal and nanocomposite iron-based materials. Graphical abstract.

From Silver Plates to Spherical Nanoparticles: Snapshots of Microwave-Assisted Polyol Synthesis.

The fabrication of silver nanoparticles (Ag NPs) with different sizes by microwave (MW)-assisted synthesis is presented. The fast heating of the MW technique, combined with the possibility to thermally quench the reactions, enabled us to capture snapshots of nucleation and growth processes difficult to accomplish in other techniques. The Ag NPs were synthesized using poly(vinylpyrrolidone) (PVP) through a polyol approach. The effects of the reaction time, the reaction temperatures, and the silver precursor concentration were investigated. The influence of agitation, the PVP concentration, and the initial conditions of the silver precursor was also studied. It is found that at very short reaction times and at low temperatures, polyhedral plates are formed with sizes ca. 300 nm and large polydispersity. However, by increasing the time or the temperature, a size and shape refinement is observed resulting in 10 nm spherical NPs with low polydispersity. Mechanistic insights are provided based on the observations extracted from transmission electron microscopy (TEM) and ultraviolet-visible spectroscopy (UV-vis). A formation mechanism starting from kinetically favored silver polyhedral plates to thermodynamically favored spherical nanoparticles is proposed. Understanding these effects allowed us to control the particle size and the tuning of Ag NPs on-demand. Moreover, the reproducibility and scalability of the process and the long-term stability of the NPs in aqueous solutions are demonstrated. Finally, we provide a recommendation regarding the use of fresh PVP as a capping and stabilizing agent.

Fast and Simple Microwave Synthesis of TiO2/Au Nanoparticles for Gas-Phase Photocatalytic Hydrogen Generation.

The fabrication of small anatase titanium dioxide (TiO2) nanoparticles (NPs) attached to larger anisotropic gold (Au) morphologies by a very fast and simple two-step microwave-assisted synthesis is presented. The TiO2/Au NPs are synthesized using polyvinylpyrrolidone (PVP) as reducing, capping and stabilizing agent through a polyol approach. To optimize the contact between the titania and the gold and facilitate electron transfer, the PVP is removed by calcination at mild temperatures. The nanocatalysts activity is then evaluated in the photocatalytic production of hydrogen from water/ethanol mixtures in gas-phase at ambient temperature. A maximum value of 5.3 mmol·[Formula: see text]h-1 (7.4 mmol·[Formula: see text]h-1) of hydrogen is recorded for the system with larger gold particles at an optimum calcination temperature of 450°C. Herein we demonstrate that TiO2-based photocatalysts with high Au loading and large Au particle size (≈50 nm) NPs have photocatalytic activity.