beta-ZnMoO4 microcrystals synthesized by the surfactant-assisted hydrothermal method: Growth process and photoluminescence properties

In this communication, we investigate the effect of different surfactants: cetyltrimethylammonium bromide (CTAB), sodium dodecyl sulfate (SDS) and polyvinylpyrrolidone (PVP-K40) on the growth process of zinc molybdate (beta-ZnMoO4) microcrystals synthesized under hydrothermal conditions at 140 degrees C for 8 h. These microcrystals were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and photoluminescence (PL) measurements. XRD patterns proved that these crystals are monophasic and present a wolframite-type monoclinic structure. FE-SEM images revealed that the surfactants modified the crystal shapes, suggesting the occurrence of distinct crystal growth processes. The CTAB cationic surfactant promotes the hindrance of small nuclei that leads to the formation of rectangle-like crystals, SDS anionic surfactant induces a growth of irregular hexagons with several porous due to considerable size effect of counter-ions on the crystal facets, PVP-K40 non-ionic surfactant allows a reduction in size and thickness of plate-like crystals, while without surfactants have the formation of irregular plate-like crystals. Finally, the PL properties of beta-ZnMoO4 microcrystals were explained by means of different shape/size, surface defects and order-disorder into lattice. (C) 2011 Elsevier B.V. All rights reserved.

History and Epistemology of Science in the Classroom: The Synthesis of Quinine as a Proposal

The history of the quinine synthesis can be used as a case study to emphasize that science is influenced by social and historical processes. The first efforts toward the synthesis of this substance, which until recently was the only treatment for malaria, were by Perkin in 1856 when, trying to obtain quinine,,. he synthesized mauveine. Since then, the quest for the total synthesis of quinine involved several characters in a web of controversies. A major step in this process was made in 1918 by Rabe and Kindler, who proposed the synthesis of quinine from quinotoxine. Twenty-six years later, after obtaining the total synthesis of quinotoxine, Woodward and Doering announced the total synthesis of quinine. However, the lack of experimental details about Rabe and Kindler's process, associated with Woodward and Doering's failure to reproduce it, raised a series of doubts about the synthesis. Stork and colleagues questioned the veracity of the experimental data and even the scientific reputation of the involved researchers. Doubts remained alive until 2008, when Williams and Smith reported, not without reservations, the reproducibility of Rabe and Kindler's protocol. The scientific knowledge as a social and historical development, its legitimating process, and the absence of neutrality in science constitute aspects that can be discussed from this case study, providing significant contributions to science education, in particular, to the initial or continued training of chemistry teachers.

Effects of synthesis conditions on the nanostructre of CexZr1-xO2 mesoporous ceramics.

CexZr1-xO2 (0.5 ≤ x ≤ 0.9) were synthesized with Zr and Ce chloride precursors, using the triblock copolymer Pluronic P123 and HCl (2 mol/L). The pH adjustment was performed in two ways: synthesis A used 11.4 mL of a NH4OH solution added at once to the initial mixture, composed by metal precursors and template in HCl; synthesis B was done by dripping slowly until the change of pH value (between 3 and 6). In this work, CexZr1-xO2 samples synthesized by these two processes are compared. The effects of pH values in materials characteristics were also evaluated. These samples were analysed by X-Ray Diffraction (XRD) with Rietveld refinement, and Nitrogen Adsorption/Desorption. In both processes, the studied materials presented two crystalline phases of CexZr1-xO2 solid solution: cubic and tetragonal. The synthesis A also presented a tetragonal phase of ZrO2. The average crystallite size and the Brunauer- Emmett-Teller (BET) surface area are bigger in process A. Both processes give samples with a mesoporous structure.

Magnetic Properties of γ - Fe2O3 Nanoparticles at the Verge of Nucleation Process.

A low-energy new method based in a one-step synthesis at room temperature produces very small maghemite nanopar ticles. The fast neutralization reaction (co-precipitation) of a ferric solution (FeCl3 aqueous) in a basic medium (NH4OH concentrated) produces an intermediate phase, presumably two-line ferrihydrite, that in oxidizing conditions is transformed to maghemite nanopar ticles. That “primordial soup” is characterized by small atom arrangements that are the base for maghemite tiny crystals. The final product of the reaction was characterized by X-ray diffraction, high-resolution transmission electron microscopy, X-ray absorption fine structure, Mössbauer spectroscopy, and magnetometry.

Electrochemically prepared polypyrrole-2-carboxylic acid films: synthesis protocols and studies on biosensors

The process for obtaining polypyrrole-2-carboxylic acid (PPY-2-COOH) films in acetonitrile was investigated using cyclic voltammetry, electrochemical quartz crystal microgravimetry (EQCM), and infrared spectroscopy (FTIR). Different potential ranges were applied during cyclic voltammetry experiments with the aim of obtaining films without and with the presence of controlled amounts of water added in acetonitrile. The FTIR spectra of the films have evidenced that cations and anions from the electrolyte solution were incorporated into the PPY-2-COOH structure, with a preferential adsorption of cations. After chemically immobilizing polyphenoloxidase (tyrosinase, PPO), PPY-2-COOH/PPO films were build for amperometric detection of catechol, establishing a linear limit of concentrations ranging from 5.0 x 10-4 to 2.5 x 10-2 mol L-1.