Thiophene‐ and silarylene‐containing polyesters. Resonance effect on conductivity after polarization in an external electric field

Polyesters were synthesized by direct polycondensation of thiophene‐2,5‐dicarboxylic acid and five different silarylene‐containing diphenols using a tosyl chloride/pyridine/N,N‐dimethylformamide system as a condensing agent. Polymers were obtained in good yields and were characterized using Fourier transform infrared and NMR (¹H, ¹³C, 135‐DEPT and ²⁹Si) spectroscopy and elemental analysis. All polymers were completely soluble in aprotic organic polar solvents such as dimethylformamide, dimethylsulfoxide and N‐methyl‐2‐pyrrolidone. The range of effective mass of the polymers (m/z) was 1 × 10⁵–2 × 10⁵, determined using electrospray ionization mass spectrometry. Asymmetry and steric hindrance prevented dense packing of the polymeric chains, showing glass transition temperatures between ? 78 and ? 51 °C and loss of thermal stability at 177–199 °C (10% weight loss). Additionally, the melting points of the polyesters were found to be in the range 62–67 °C. Because of this, the samples were semi‐solid at room temperature. The optical band gaps of the polymers were observed between 4.54 and 4.48 eV, corresponding in all cases to insulator behavior. The molecular structure of the samples was studied using X‐ray diffraction, showing a degree of order that was associated with two monoclinic lattices. Additionally, the conductivity was studied using a two‐point method with contacts on top of polymer films. Prior to the electrical measurement, the samples were polarized in an external electric field of 0.8 to 6.4 V cm^?1, and the alignment of the dipoles increased the electrical conductivity. Copyright © 2012 Society of Chemical Industry     

Comparative study between large-scale and small-scale electrochemical potentiokinetic reactivation performed on AISI 316L austenitic stainless steel

This work optimizes the application of electrochemical potentiokinetic reactivation (EPR) to assess the degree of sensitization (DOS) of AISI 316L and compares the large-scale and small-scale EPR with the aim of improving the study of the different zones of AISI 316L welded joints by using an electrochemical minicell. The optimized EPR allows to discriminate better than the standardized EPR among different DOS. Small-scale EPR shows greater sensitivity to assess the DOS than large-scale EPR: (i) at lower deformation levels; (ii) for shorter sensitization times; (iii) when localized microstructural regeneration is caused by the combined effect of deformation and subsequent sensitization.     

Typing artifacts in megamodeling

Model management is essential for coping with the complexity introduced by the increasing number and varied nature of artifacts involved in model-driven engineering-based projects. Global model management (GMM) addresses this issue by enabling the representation of artifacts, particularly transformation composition and execution, within a model called a megamodel. Type information about artifacts can be used for preventing type errors during execution. Built on our previous work, in this paper we present the core elements of a type system for GMM that improves its original typing approach and enables both typechecking and type inference on artifacts within a megamodel. This type system is able to deal with non-trivial situations such as the use of higher order transformations. We also present a prototypical implementation of such a type system.     

Determination of flonicamid and its metabolites in bell pepper using ultra-high-performance liquid chromatography coupled to high-resolution mass spectrometry (Orbitrap)

The development and validation of a method to determine flonicamid and its metabolites as TFNA (4-trifluoromethylnicotinic acid), TFNG (N-(4-trifluoromethylnicotinoyl) glycine) and TFNA-AM (4-trifluoromethylnicotinamide) in bell pepper samples by ultra-high-performance liquid chromatography coupled to Orbitrap mass spectrometry (UHPLC-Orbitrap-MS) was performed. A fast and simple extraction procedure with acidified acetonitrile and salts (magnesium sulfate and sodium chloride) was used. The methodology was validated, checking for specificity, recovery, precision, limits of detection (LODs) and limits of quantification (LOQs). The recoveries ranged from 84% to 98%, and precisions were lower than 17%. Finally, LODs ranged from 1 µg kg^–1 (flonicamid) to 6 µg kg^–1 (TFNA-AM), while LOQs ranged from 10 µg kg^–1 (flonicamid) to 30 µg kg^–1 (TFNA-AM). Bell pepper samples were analysed and concentrations up to 98 µg kg^–1 (flonicamid) were detected, although the sum of flonicamid and metabolites did not exceed the maximum residue limit (MRL) set by the European Union.     

An approach to calibrate incentives for continuity of supply in the Spanish electricity distribution system

This paper proposes an approach to calibrate incentives for continuity of supply in electricity distribution in Spain. This approach consists on the estimation of the impact of continuity of supply improvements on distribution network costs. For this purpose, distribution costs resulting from different continuity of supply requirements are computed by a reference network model (RNM). The results obtained from the RNM are used to estimate a cost-function that considers continuity of supply a cost driver for distribution costs. This methodology is applied to three Spanish areas of service (an urban one, a semi-urban one and a rural one) in such a way that differences in distribution costs caused by the characteristics of the area type can be taken into account. The analysis indicated that distribution costs are more sensitive to continuity of supply improvements in rural areas of service. It also demonstrated that the incentive for reducing number of service interruptions should be higher than the incentive for reducing duration of service interruptions. Finally, the current Spanish incentive scheme for continuity of supply was analyzed under the perspective of the proposed approach.     

An energy efficient middleware for an ad-hoc AAL wireless sensor network

DIA (Dispositivo Inteligente de Alarma, in Spanish) is an AAL (Ambient Assisted Living) system that allows to infer a potential dangerous action of an elderly person living alone at home. This inference is obtained by a specific sensorisation with sensor nodes (portables and fixes) and a reasoning layer embedded in a PC that learns of the users behaviour patterns and advices when actual one differs significantly of the normal patterns. In AAL systems, energy is a limited resource therefore sensor devices need to be properly managed to conserve energy. In this paper, we introduce the design and implementation of innovative and specific mechanisms at the sensory layer middleware which is capable of, first to discriminate spurious motion detections assuming that these signals do not resemble the patterns of real motion detections and, second to reduce the dynamics of messages by a sensor signal processing in order to compress the whole information in one single event. The middleware achieves power saving by modifying the raw information from sensors and adapting it to the predefined semantic of the reasoning layer. It manages the important task of data processing from sensors (raw information), and transfers the pre-processed information into the top layer of reasoning in a more energy efficient way. We also address the trade-off between reducing power consumption and reducing delay for incoming data. We present results from experiments using our implementation of these mechanisms at the middleware that comprises from node firmware to the PC driver. The number of messages of the proposed method with respect to the raw data is reduced by approximately 98.5%. The resources used in the PIR signal processing is reduced by approximately 85%. The resulting delay introduced is small (10–19 s) but system dynamics is slow enough to avoid contextualisation errors or reduction of system performance. We consider these results as very satisfactory.     

Characterization of lead zirconate titanate (53/47) films fabricated by a simplified sol–gel acetic-acid route

Lead zirconate titanate [PZT (53/47)] films (around 200 nm thick) were prepared by the sol–gel acetic-acid route, spin-coating onto Si/SiO₂/Pt substrates. A simple thermal annealing program rendered complete crystallization to the perovskite phase and full removal of the organic material. The 53/47 film composition was attained in the bulk, however, X-ray photoelectron spectroscopy detected a different titanium/zirconium ratio at the film surface. Hysteresis loops were measured using a film-tester constructed at our laboratory. The single-annealed films showed a high resistive leakage. A second annealing cycle led to a better film densification and a marked reduction in surface roughness, significantly enhancing the ferroelectric response. Ferroelectric domains were mapped by piezoresponse force measurements. The relatively-simple experimental procedure applied allowed the fabrication of good quality ferroelectric films.