Chromo‐Fluorogenic Detection of Nerve‐Agent Mimics Using Triggered Cyclization Reactions in Push–Pull Dyes

A family of azo and stilbene derivatives ( 1 , 2 , 3 , 4 , 5 , 6 , 7 , 8 , 9 ) are synthesized, and their chromo‐fluorogenic behavior in the presence of nerve‐agent simulants, diethylchlorophosphate (DCP), diisopropylfluorophosphate (DFP), and diethylcyanophosphate (DCNP) in acetonitrile and mixed solution of water/acetonitrile (3:1 v/v) buffered at pH 5.6 with MES, is investigated. The prepared compounds contain 2‐(2‐N,N‐dimethylaminophenyl)ethanol or 2‐[(2‐N,N‐dimethylamino)phenoxy]ethanol reactive groups, which are part of the conjugated π‐system of the dyes and are able to give acylation reactions with phosphonate substrates followed by a rapid intramolecular N‐alkylation. The nerve‐agent mimic‐triggered cyclization reaction transforms a dimethylamino group into a quaternary ammonium, inducing a change of the electronic properties of the delocalized systems that results in a hypsochromic shift of the absorption band of the dyes. Similar reactivity studies are also carried out with other “non‐toxic” organophosphorus compounds, but no changes in the UV/Vis spectra were observed. The emission behaviour of the reagents in acetonitrile and water–acetonitrile 3:1 v/v mixtures is also studied in the presence of nerve‐agent simulants and other organophosphorous derivatives. The reactivity between 1 , 2 , 3 , 4 , 5 , 6 , 7 , 8 , 9 and DCP, DCNP, or DFP in buffered water–acetonitrile 3:1 v/v solutions under pseudo first‐order kinetic conditions, using an excess of the corresponding simulant, are studied in order to determine the rate constants (k) and the half‐life times (t_1/2=ln2/k) for the reaction. The detection limits in water/acetonitrile 3:1 v/v are also determined for 1 , 2 , 3 , 4 , 5 , 6 , 7 , 8 , 9 and DCP, DCNP, and DFP. Finally, the chromogenic detection of nerve agent simulants both in solution and in gas phase are tested using silica gel containing adsorbed compounds 1 , 2 , 3 , 4 , or 5 with fine results.     

Study of matrix effects and spectral interferences in the determination of lead in sediments, sludges and soils by SR-ETAAS using slurry sampling

An interference-free, fast, and simple method is proposed for Pb determination in environmental solid samples combining slurry sampling and electrothermal atomic absorption spectrometry. Samples were ground to an adequate particle size and slurries were prepared by weighing from 0.05 g to 0.20 g of dry sediment, adding nitric acid, and a solution containing 0.1% Triton X-100. Ultrasonic agitation was employed for slurries homogenization. Analytical variables including acid pre-treatment conditions, particle size, slurry stability, temperature program of the graphite furnace, and type and concentration of the chemical modifier were studied. The undesirable effects of potential non-specific and spectral interferences on Pb signal were also taken into account. Continuum source and self-reversal methods for background correction were evaluated and compared. For calibration, synthetic acid solutions of Pb were employed. Calibration was linear within the range 1-30 μg L⁻¹ and 5-30 μg L⁻¹ when the 217.0 nm and 283.3 nm analytical lines were used. Correlation coefficients of 0.9992 and 0.9997 were obtained. Using optimized conditions, limits of detection (3σ) of 0.025 μg g⁻¹ and 0.1 μg g⁻¹ were achieved for the 217.0 nm and 283.3 nm analytical lines, respectively. The method was successfully applied to the determination of lead in soil, contaminated soil, municipal sludge, and sediment samples. The accuracy was assessed by the analysis of two certified reference materials: municipal sludge (QC MUNICIPAL SLUDGE A) and lake sediment (TRAP-LRM from IJS).     

Influence of the phase composition of the support on the catalytic activity of bimetallic catalysts

The influence of the nanocrystalline structure of an aluminum-zinc spinel support on the catalytic activity of bimetallic Pt-Sn catalysts in dehydrogenation of 2-methylbutane was studied. The formation of the spinel structure in solid-phase reactions of aluminum and zinc oxides was examined.     

Complementary split ring resonators for microstrip diplexer design

A new topology for the design of microstrip microwave diplexers, based on the use of quasi-lumped resonators, is presented. Specifically, the receiver (Rx) and transmitter (Tx) filters of the diplexer are implemented by etching complementary split ring resonators (CSRRs) in the ground plane as well as series capacitive gaps and shunt inductive strips in the upper metal level. By this means, narrowband microwave diplexers with transmission zeros can be synthesised, which allow for the improvement of Rx/Tx isolation. A prototype device operative in the 2.4-3.0 GHz frequency band is presented. Measured insertion losses are lower than 2 dB while the isolation between Rx/Tx channels is in the vicinity of 40 dB. Diplexer dimensions (29.8/spl times/16.3 mm), which are small on account of the semi-lumped resonators employed, and performance point to the practical application of these structures in communication transceiver front-ends.     

Airmed-cardio: a GSM and Internet services-based system for out-of-hospital follow-up of cardiac patients.

A platform built around three information entities (patient, health-care_agent, and central_station) was designed to enable patients with chronic heart disease (in stable condition; emergency situations were excluded deliberately) to complete specifically defined protocols for out-of-hospital follow-up and monitoring. The patients belonged to one of four specific risk groups: arterial hypertension, malignant arrhythmias, heart failure, and postinfarction rehabilitation. They were provided with portable recording equipment and a cellular phone that supported data transmission [electrocardiogram (ECG)] and wireless application protocol (WAP) (remaining parameters and ad hoc questionnaires). The central station was an automatized platform, with no human operator. The information received was organized chronologically in patient folders. The health-care_agents had continuous and secure access to the patient folders, through tools based on the world wide web and WAP, and to short messages sent by their patients. A pilot project was conducted with 89 patients (mean length of participation: 50.1 days). A total of 2168 ECGs (mean duration transmission = 2 min/30 s; network errors < 0.1%) and 4011 short messages (none lost, in 95% of cases 30 s < delay < 1 min) were transmitted; 6083 WAP sessions (mean duration = 3 min 11 s; network failures < 0.1%) were The functionality of the platform was also evaluated, analyzing the subjective component of usability, showing the evolution of patient acceptance over time.     

Study of the physicochemical properties of aminostyrene copolymers modified by plasma treatment

The change in the surface and mechanical properties of styrene-butyl methacrylate-aminostyrene terpolymer films by plasma treatment was investigated. It was found that treatment in a direct-current discharge enhanced the mechanical strength of the terpolymer surface, which can be associated with the crosslinking of linear macromolecules into a three-dimensional network structure. It was shown that the most substantial changes in the mechanical strength are achieved in the case of terpolymer film treatment at the anode.