Influence of the stirring speed and CaCl2 concentration on the nano‐object morphologies obtained via RAFT‐mediated aqueous emulsion polymerization in the presence of a water‐soluble macroRAFT agent

Aqueous emulsion polymerizations of styrene were performed in the presence of a macromolecular reversible addition‐fragmentation chain transfer (RAFT) agent (macroRAFT) composed of acrylic acid (AA) and poly(ethylene oxide) methyl ether acrylate (PEOA), end‐capped by a reactive dodecyl trithiocarbonate group (P(AA‐co‐PEOA)‐TTC). The influence of the stirring speed or the presence of different amounts of a divalent salt, CaCl₂, were investigated in this polymerization‐induced self‐assembly process, in which spherical and nonspherical nano‐objects were formed upon the synthesis of amphiphilic diblock copolymers in situ. It appeared that the addition of CaCl₂ led to the controlled formation of different nano‐objects such as spheres, fibers or vesicles, whereas an appropriate stirring speed was required for the formation of nanofibers. © 2011 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2011     

Determination of β-glucosidase activity in soils with a bioanalytical sensor modified with multiwalled carbon nanotubes

Soil microorganisms and enzymes are the primary mediators of soil biological processes, including organic matter degradation, mineralization, and nutrient recycling. They play an important role in maintaining soil ecosystem quality and functional diversity. Moreover, enzyme activities can provide an indication of quantitative changes in soil organic matter. β-Glucosidase (β-Glu) activity has been found to be sensitive to soil management and has been proposed as a soil quality indicator because it provides an early indication of changes in organic matter status and its turnover. The aims of the present study were to test and use a simple and convenient procedure for the assay of β-Glu activity in agricultural soil. The method described here is based on the enzymatic degradation of cellobiose by β-Glu present in the soil sample and the subsequent determination of glucose produced by the enzymatic reaction using screen-printed carbon electrodes modified with multiwalled carbon nanotubes (SPCE-CNT) equipped with coimmobilized glucose oxidase and horseradish peroxidase enzymes. The potential applied to the SPCE-CNT detection was −0.15 V versus a Ag/AgCl pseudo-reference electrode. A linear calibration curve was obtained in the range 2.7–11.3 mM with a correlation coefficient. In the present study, an easy and effective SPCE-CNT-modified electrode allowed an improved amperometric response to be achieved and this is attributed to the increased surface area upon electrode modification.     

Publisher’s note

Experimental Techniques -     

Can density functional theory (DFT) be used as an aid to a deeper understanding of tandem mass spectrometric fragmentation pathways?

Prediction of tandem mass spectrometric (MS/MS) fragmentation for non‐peptidic molecules based on structure is of immense interest to the mass spectrometrist. If a reliable approach to MS/MS prediction could be achieved its impact within the pharmaceutical industry could be immense. Many publications have stressed that the fragmentation of a molecular ion or protonated molecule is a complex process that depends on many parameters, making prediction difficult. Commercial prediction software relies on a collection of general heuristic rules of fragmentation, which involve cleaving every bond in the structure to produce a list of ‘expected’ masses which can be compared with the experimental data. These approaches do not take into account the thermodynamic or molecular orbital effects that impact on the molecule at the point of protonation which could influence the potential sites of bond cleavage based on the structural motif. A series of compounds have been studied by examining the experimentally derived high‐resolution MS/MS data and comparing it with the in silico modelling of the neutral and protonated structures. The effect that protonation at specific sites can have on the bond lengths has also been determined. We have calculated the thermodynamically most stable protonated species and have observed how that information can help predict the cleavage site for that ion. The data have shown that this use of in silico techniques could be a possible way to predict MS/MS spectra. Copyright © 2009 John Wiley & Sons, Ltd.     

State of the art of the sphere method, a unique characterization technique for non-linear crystals

We report the sphere method as a unique characterization technique for the complete study of non-linear optical properties for frequency conversion in new materials belonging to the uniaxial or biaxial optical class. It relies on the use of a single crystal with millimetre dimensions cut as a sphere, combined with a tuneable laser source. With the sphere method we perform direct measurements of phase-matching angles and associated conversion efficiencies for second harmonic, sum- and difference-frequency generation. Furthermore, we follow the orientation of the dielectric frame as a function of the wavelength for monoclinic and triclinic crystals. It also allows the determination of the magnitude of the principal refractive indices in biaxial crystals based on the study of the double refraction affect at the exit of a sphere. By combining the analysis of all these data simultaneously, we determine Sellmeier equations reliable over the whole transparency domain and we are able to get the non-zero elements of the second-order susceptibility tensor of uniaxial or biaxial crystals. Finally, the sphere method is completely self-sufficient for the study of biaxial crystals.     

A Survey of Calculator Usage in High Schools

This survey investigated the current status of calculator use in classrooms and schools. The results indicated that the prevailing policy in the sample of high schools is to allow the use of calculators during classroom learning activities and tests. Scientific calculators are more frequently used than graphing calculators in algebra I and geometry; whereas, graphing calculators are more frequently used in algebra II and precalculus/trigonometry. At the time of this survey, school policies regarding the use of graphing calculators with symbolic algebra capabilities were still not determined.     

Adsorption behaviour of cadmium on L-methionine immobilized on controlled pore glass

The adsorption behaviour of Cd onto the relative non-polar L-methionine was studied. To this end, L-met was immobilized on controlled pore glass (CPG), incorporated in a microcolumn and inserted in a flow injection system for Cd preconcentration from aqueous solutions. Binding constant of the system was calculated and it turned to be of 1.99, with sites capacity of n = 3.12. The ratio of Cd moles bound to L-met moles was calculated and it was 0.03:1 at pH 9.0. On-line breakthrough curves were used to study the effect of pH, analyte concentration and influent flow rate on Cd retention. A complementary pH study was added with a titration curve. Transient peak areas revealed that Cd stripping from the column occurred instantaneously. The system achieves an enrichment factor of 130, reaching a detection limit of 0.63 ng L^{− 1} when 10 mL of the solution were passed through the column. The method was successfully applied to Cd determination in the standard reference material (SRM), QC METAL LL2 metals in natural water, as a validation study.