Temperature dependence of second critical micelle concentration of dodecyldimethylbenzylammonium bromide in aqueous solution

The specific conductivity of dodecyldimethylbenzylammonium bromide (C12BBr) in aqueous solutions, in the temperature range of 15 to 40 °C, has been measured as a function of molality. The two breaks which were found on the conductivity against molality plots were attributed to the critical micelle concentration, cmc, and second critical micelle concentration, 2^nd cmc, respectively. The ratio of the slopes, S, of the three linear fragments on the plots, S2/S1 and S3/S1, was attributed to the degree of ionization of the micelles at cmc and 2^nd cmc respectively. It was shown that the values of the 2^nd cmc estimated above 27 °C are only apparent due to thermal disintegration of the micelles. In the temperature range of 15 to 27 °C, the values of the 2^nd cmc increase gradually and the plot of the 2^nd cmc against temperature is concave. The ratio of 2^nd cmc/cmc for C12BBr at 25 °C amounts to 15 and appears to be high compared to the literature values for other surfactants. For comparative purposes the cmc and 2^nd cmc values were also estimated conductometrically for decyldimethylbenzylammonium bromide (C10BBr) at 25 °C. The 2^nd cmc value for this surfactant is higher compared to the value for the C12 homologue by a factor of 2.6.The standard Gibbs free energies of micellization at cmc and at the 2^nd cmc were estimated from the experimental data for both surfactants at 25 °C.     

Selective extraction of benzoic acid from landfill leachate by solid-phase extraction and ion-exchange chromatography

In this work a simple method was described for selective extraction of benzoic acid from landfill leachate samples. The samples were submitted to solid-phase extraction (SPE) with XAD-4 resin as the stationary phase and ion-exchange chromatography (IEC) using the ion-exchange resin Amberlyst A-27. The instrumental analysis was performed by gas chromatography with mass spectrometric detection (GC-MSD). Benzoic acid was isolated, identified and quantified. The extraction process is rapid, simple and of low cost. It was also environmental friendly, that is, it was used a minimum amounts of hazardous organic solvents and produced also minimum quantities of residues.     

Rapid qualitative analysis of metallic alloys by electrospot chromatography

Summary Electrography and paper chromatography were combined to analyse rapidly metallic alloys in an almost non destructive technique. Using anodic dissolution the sample is applied on the start point of the chromatographic paper. Known ketones-HCl-water mixtures are usually used as solvents to analyse electrospots of different alloys and metal coatings and a separate electrospottest is recommended for Cr. Results of qualitative analysis of some steels, Cu–Ni, and Pb alloys are presented.     

Application of Graphite-Epoxy Composite Electrodes in Differential Pulse Anodic Stripping Voltammetry of Heavy Metals

An analytical study on the use of graphite-epoxy composite (GEC) electrodes for differential pulse anodic stripping voltammetry (DPASV) of heavy metals is presented. This study is accompanied by microscopic observations of the electrode surface before and after the stripping step in comparison to glassy carbon electrode. GEC electrodes show much better accumulation properties and consequently acceptable behaviour which makes them suitable as working electrodes in the DPASV of heavy metals. Lead determination in real water samples in a batch system as well as some preliminary results in a flow-through system are presented. The detection limits in batch measurements were 100ppb for Cd, 10pb for lead and 50ppb for copper. The detection limit for lead in the flow-through system was similar to that in the batch. The results obtained show that these low cost and easy to prepare materials can be of interest in future research concerning stripping techniques of heavy metals and other analytes.     

Molecular-level control of the photoluminescence from PPV nanostructured films

The fabrication of varied molecular architectures in layer-by-layer (LbL) films is exploited to control the photoluminescence (PL) of poly(p-phenylene vinylene) (PPV) in an unprecedented way. This was achieved by controlling the F?rster energy transfer between PPV layers (donors) and layers of a commercial azodye, Brilliant Yellow (BY) (acceptors). Energy transfer was controlled by inserting spacer layers of inert polymers between PPV and BY layers and by photoaligning the BY molecules via trans-cis-trans isomerization. The PPV/BY LbL films displayed polarized PL whose intensity could be varied almost continuously by changing the time of photoalignment, which was carried out by impinging a linearly polarized laser light simultaneously to the PL experiments. For PPV/BY films with no spacer layers, PL was completely quenched, but its intensity increased with the number of spacing layers. Further increase in PL was obtained by photoaligning the BY molecules perpendicularly to the PPV molecules. This minimizes energy transfer, since F?rster processes are directional, dipole-dependent resonant transfers. Energy transfer is also controlled by imparting a preferential orientation of the PPV chains on PPV/BY LbL films deposited onto flexible Teflon substrates that may be stretched.     

Determination of aflatoxins in peanuts by matrix solid-phase dispersion and liquid chromatography

A new method based on matrix solid-phase dispersion (MSPD) extraction was studied to determine aflatoxin B1, B2, G1 and G2 from peanuts. Optimization of different parameters, such as type of solid supports for matrix dispersion and elution solvents were carried out. The method used 2 g of peanut sample, 2 g of C18 bonded silica as MSPD sorbent and acetonitrile as eluting solvent. Recoveries of each aflatoxin spiked to peanut samples at 2.5 ng/g (5 ng/g for aflatoxin G2) level were between 78 and 86% with relative standard deviations ranging from 4 to 7%. The limits of quantification ranged from 0.125 to 2.5 ng/g for the four studied aflatoxins using liquid chromatography (LC) with fluorescence detection. In addition, LC coupled to mass spectrometry with an electrospray interface was used for confirmation of aflatoxins present in real samples. Eleven peanut samples from different countries were analyzed by the proposed method and by using an enzyme-linked immunosorbent assay (ELISA). ELISA test is a good screening method for investigation of these mycotoxins in peanut samples.     

Particle-size distribution of polycyclic aromatic hydrocarbons in urban air in southern Spain

The size distribution of polycyclic aromatic hydrocarbons (PAH) was determined for airborne particles from a large city with high vehicular traffic. The analytical method was optimised and validated using NIST standard reference material (SRM 1649a Urban Dust). The 16 priority PAH listed in the US-EPA were Soxhlet-extracted from filtered particulate matter and then fractionated using on-column chromatography. The aromatic fraction was quantified by gas chromatography-mass spectrometry. Real samples of particles collected in Seville (Spain) were analysed using the validated method. Values for the total concentration of PAH in the air, as well as the concentrations of each PAH in six particle-size ranges were obtained. Values of the PAH in TSP, PM₁₀, PM_2.5 and PM₁ were assessed.     

A simple and fast micromethod for the analysis of polychlorinated biphenyls in air by sorbent enrichment and ultrasound-assisted solvent extraction

A combination of sorbent enrichment and ultrasound-assisted solvent extraction has been used to determine polychlorinated biphenyls in air. Analytes were sampled by pumping a known volume of air through a porous polymer (Tenax TA). The enriched adsorbent was transferred into a glass vial, and ultrasound-assisted extraction of the analytes was then performed in n-hexane. Quantification was carried out by using gas chromatography coupled to tandem mass spectrometry. Breakthrough volume of the sampling step was studied, indicating that 10 m³ of air could be processed without losses of the most volatile compounds. Good recoveries (75–96%) were obtained, and limits of detection at the sub ng m^–3 were achieved for all the analytes. The proposed method is very simple and fast, avoiding the use of large solvent volumes and time-consuming preconcentration steps.