Solvent free esterification reactions using Lewis acids in solid phase catalysis

A clean, efficient and fast method for esterification reactions for sterically (biodiesels) or otherwise inactive (aromatic) precursors was developed, using catalysts supported in a solid phase under solvent free conditions, and whose reactions can be promoted by MW irradiation. (c) 2006 Elsevier B.V. All rights reserved.

Label-free DNA detection based on modified conducting polypyrrole films at microelectrodes

A label-free electrochemical detection method for DNA hybridization based on electrostatic modulation of the ion-exchange kinetics of a polypyrrole film deposited at microelectrodes is reported. Synthetic single-stranded 27-mer oligonucleotides (probe) have been immobilized at 2,5-bis(2-thienyl)-N-(3-phosphorylpropyl)pyrrole film formed by electropolymerization on the previously formed polypyrrole layer. The 27- or 18-mer target oligonucleotides were monitored via the electrochemically driven anion exchange of the inner polypyrrole film. The performance of the miniaturized DNA biosensor system was studied in respect to selectivity, sensitivity, reproducibility, and regeneration of the sensor. Control experiments were performed with a noncomplementary target of 27-mer DNA and 12 base-pair mismatched 18-mer sequences, respectively, and did not show any unspecific binding. Under optimized experimental conditions, the label-free electrochemical biosensor enabled the detection limits of 0.16 and 3.5 fmol for the 18- and 2 7-mer DNA strand, respectively. Furthermore, we demonstrate reusability of the electrochemical DNA biosensor after successful recovery of up to 100% of the original signal by regenerating the DNA label-free electrode with 50 mM HCl at room temperature.

Simplified multiresidue method for the determination of organophosphorus insecticides in olive oil

A simple and rapid method for the determination of 13 organophosphorus insecticides and their metabolites in olive oil by GC is described. The pesticide was extracted from oil with acetonitrile and no cleanup was needed. GC-nitrogen-phosphorus detection response factors of pesticides were affected by solvents and coextractive substances. Pesticides in hexane showed on average higher response factors. Standards were prepared in the residue-free oil extract solubilized in hexane to handle effects of matrix and solvent. The low amount of coextractive substances does not decrease the column efficiency, even after a few hundred analyses. Recovery at three fortification levels (ca. 0.1, 1.0 and 3.0 mg/kg) ranged from 74 to 118%, With coefficients of variation ranging from 1 to 16.

The effect of microwave annealing on the electrical characteristics of lanthanum doped bismuth titanate films obtained by the polymeric precursor method

Lanthanum doped bismuth titanate thin films (Bi3.25La0.75Ti3O12-BLT) were produced by the polymeric precursor method and crystallized in a domestic microwave oven and in conventional furnace. Using platinum coated silicon substrates configuration, ferroelectric properties of the films were determined with remanent polarization P-r and a coercive field E-c of 3.9 mu C/cm(2) and 70 kV/cm for the film annealed in the microwave oven and 20 mu C/cm(2) and 52 kV/cm for the film annealed in conventional furnace, respectively. The films annealed in conventional furnace exhibited excellent retention-free characteristics at low infant periods indicating that BLT thin films can be a promise material for use in nonvolatile memories. on the other hand, the pinning of domains wall causes a strong decay at low infant periods for the films annealed in the microwave furnace which makes undesireable the application for future FeRAMS memories. (c) 2005 Elsevier B.V. All rights reserved.

A new method for the selective quantitation of cyanogenic glycosides by membrane introduction mass spectrometry

A new method is described for the rapid, sensitive, virtually interference-free, and selective quantitation of cyanogenic glycosides in aqueous extracts using membrane introduction mass spectrometry (MIMS). Selective monitoring, by either conventional MIMS or cryotrap-MIMS, not of HCN but of the co-released ketones (acetone and butan-2-one), when performed for both the crude cassava extracts and the linamarase-NaOH-hydrolyzed extracts, is found to offer an advantageous alternative to classic spectrophotometric methods based on HCN analysis for the selective quantitation of the two cyanogenic glycosides linamarin and lotaustralin expressed as both the free HCN content and the total cyanogenic potential (total HCN).

Effect of thermal treatment temperature on the crystallinity and morphology of LiTaO3 thin films prepared from polymeric precursor method

Lithium tantalate thin films (LiTaO3) with (50:50) stoichiometry were prepared by spin coating method using a polymeric organic solution. The films were deposited on silicon (100) substrates with 4 layers. The substrates were previously cleaned and then the solution of lithium tantalate was deposited by adjusting the speed at 5000 rpm. The thin films deposited were thermally treated from 350 to 600degreesC for 3 hours in order to study the influence of the thermal treatment temperature on the crystallinity, microstructure, grain size and roughness of the final film. X-ray diffraction (XRD) results showed that the films are polycrystalline and secondary phases free. The thickness of films was observed by scanning electron microscopy (SEM). The atomic force microscopy (AFM) studies showed that the grain size and roughness are strongly influenced by thermal treatment.

Barium strontium titanate nanocrystalline thin films prepared by soft chemical method

Barium strontium titanate (Ba0.65Sr0.35TiO3) nanocrystalline thin films, which were produced by the soft chemical method, were crystallized at low temperature using a domestic microwave oven. A SiC susceptor were used to absorb the microwave energy and rapidly transfer the heat to the film. Low microwave power and short time have been used. The films obtained are crack-free, well-adhered, and fully crystallized. The microstructure displayed a polycrystalline nature with nanograin size. The metal-BST-metal structure of the thin films treated at 700 degrees C show food electric properties. The ferroelectric nature of the BST35 thin film was indicated by buttertly- shaped C-V curves. The capacitance-frequency curves reveal that the dielectric constant may reach a value up to 800 at 100kHz. The dissipation factor was 0.01 at 100kHz. The charge storage density as function of applied voltage graph showed that the charge storage densities are suitable for use in trench type 64 Mb ( 1-5 mu C/cm(2) and 265 Mb (2-11 mu C/cm(2)) DRAMs. (C) 2007 Elsevier Ltd. All rights reserved.

Ferroelectric properties and leakage current characteristics of Bi3.25La0.75Ti3O12 thin films prepared by the polymeric precursor method

The ferroelectric properties and leakage current mechanisms of preferred oriented Bi3.25La0.75Ti3O12 (BLT) thin films deposited on La0.5Sr0.5CoO3 by the polymeric precursor method were investigated. These films showed excellent ferroelectric properties in terms of large remnant polarization (2P(r)) of 47.6 mu C/cm(2) and (2E(c)) of 55 kV/cm, fatigue-free characteristics up to 10(10) switching cycles, and a current density of 0.7 mu A/cm(2) at 10 kV/cm. X-ray diffraction and scanning electron microscope investigations indicate that the deposited films exhibit a dense, well-crystallized microstructure having random orientations and with a rather smooth surface morphology. The improved ferroelectric and leakage current characteristics can be ascribed to the platelike grains of the BLT films, which make the domain walls easier to be switched under external field.

Low temperature synthesis and electrical properties of PbTiO3 thin films prepared by the polymeric precursor method

Ferroelectric PbTiO3 thin films were successfully prepared on a Pt(111)Ti/SiO2/Si(100) substrate for the first time by spin coating, using the polymeric precursor method. X-ray diffraction patterns of the films indicate that they are polycrystalline in nature. This method allows low temperature (500 degrees C) synthesis and high electrical properties. The multilayer PbTiO3 thin films were granular in structure with a grain size of approximately 110-120 nm. A 380-nm-thick film was obtained by carrying out four cycles of the spin-coating/heating process. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) analyses showed the surface of these thin films to be smooth, dense and crack-free with low surface roughness (=3.4 nm). At room temperature and at a frequency of 100 kHz, the dielectric constant and the dissipation factor were, respectively, 570 and 0.016. The C-V characteristics of perovskite thin film prepared at low temperature show normal ferrolectric behavior. The remanent polarization and coercive field for the films deposited were 13.62 mu C/cm(2) and 121.43 kV/cm, respectively. The high electrical property values are attributed to the excellent microstrutural quality and chemical homogeneity of thin films obtained by the polymeric precursor method. (C) 2000 Elsevier B.V. S.A. All rights reserved.

Dielectric and fatigue properties of Pb(Zr0.53Ti0.47)O-3 thin films prepared from oxide precursors method

Fatigue is an important problem to be considered if a ferroelectric film is used for non-volatile memory devices. In this phenomena, the remanent polarization and coercive field properties degrades in cycles which increase in hysteresis loops. The reasons have been attributed to different mechanisms such as a large voltage applied on ferroelectric film in every reading process in Ferroelectric Random Access Memory (FeRAM) or memories for digital storage in computer, grain size effects and others. The aim of this work is to investigate the influence of the crystallization kinetics on dielectric and ferroelectric properties of the Pb(Zr0.53Ti0.47)O-3 thin films prepared by an alternative chemical method. Films were crystallized in air on Pt/Ti/SiO2/Si substrates at 700 degrees C for 1 hour, in conventional thermal annealing (CTA), and at 700 degrees C for 1 min and 700 degrees C 5 min, using a rapid thermal annealing (RTA) process. Final films were crack free and presented an average of 750 nm in thickness. Dielectric properties were studied in the frequency range of 100 Hz - 1 MHz. All films showed a dielectric dispersion at low frequency. Ferroelectric properties were measured from hysteresis loops at 10 kHz. The obtained remanent polarization (P-r) and coercive field (E-c) were 3.7 mu C/cm(2) and 71.9 kV/cm respectively for film crystallized by CTA while in films crystallized by RTA these parameters were essentially the same. In the fatigue process, the P, value decreased to 14% from the initial value after 1.3 x 10(9) switching cycles, for film by CTA, while for film crystallized by RTA for 5 min, P, decreased to 47% from initial value after 1.7 x 10(9) switching cycles.

Are Working Memory Measures Free of Socioeconomic Influence?

Purpose: This study evaluated the impact of socioeconomic factors on children's performance on tests of working memory and vocabulary.Method: Twenty Brazilian children, aged 6 and 7 years, from low-income families, completed tests of working memory ( verbal short-term memory and verbal complex span) and vocabulary ( expressive and receptive). A further group of Brazilian children from families of higher socioeconomic status matched for age, gender, and nonverbal ability also participated in the study.Results: Children from the low socioeconomic group obtained significantly lower scores on measures of expressive and receptive vocabulary than their higher income peers but no significant group differences were found on the working memory measures.Conclusion: Measures of working memory provide assessments of cognitive abilities that appear to be impervious to substantial differences in socioeconomic background. As these measures are highly sensitive to language ability and learning in general, they appear to provide useful methods for diagnosing specific learning difficulties that are independent of environmental opportunity.

Superparamagnetic Ni:SiO2-C nanocomposites films synthesized by a polymeric precursor method

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Mechanistic approach to predict real machining time for milling free-form geometries applying high feed rate

An accurate estimate of machining time is very important for predicting delivery time, manufacturing costs, and also to help production process planning. Most commercial CAM software systems estimate the machining time in milling operations simply by dividing the entire tool path length by the programmed feed rate. This time estimate differs drastically from the real process time because the feed rate is not always constant due to machine and computer numerical controlled (CNC) limitations. This study presents a practical mechanistic method for milling time estimation when machining free-form geometries. The method considers a variable called machine response time (MRT) which characterizes the real CNC machine's capacity to move in high feed rates in free-form geometries. MRT is a global performance feature which can be obtained for any type of CNC machine configuration by carrying out a simple test. For validating the methodology, a workpiece was used to generate NC programs for five different types of CNC machines. A practical industrial case study was also carried out to validate the method. The results indicated that MRT, and consequently, the real machining time, depends on the CNC machine's potential: furthermore, the greater MRT, the larger the difference between predicted milling time and real milling time. The proposed method achieved an error range from 0.3% to 12% of the real machining time, whereas the CAM estimation achieved from 211% to 1244% error. The MRT-based process is also suggested as an instrument for helping in machine tool benchmarking.

Luminescence properties of Eu(3+)- and Mg(2+)-doped LiTaO(3) obtained via the polymeric precursor method

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Strain behavior of lanthanum modified BiFeO3 thin films prepared via soft chemical method

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)