Trace pollutants analysis in soil by a time-resolved laser-induced breakdown spectroscopy technique

The results of a joint experiment of IFAM-Pisa and ENEA-Frascati for the detection of traces of pollutants in soil by a time-resolved laser-induced spectroscopy technique are reported. Using samples of soil with known pollutants' concentration [Geochemical Exploration Reference (GXR) silicate from US Geological Survey], we were able to estimate the sensitivity of this Laser-Induced Breakdown Spectroscopy (LIBS) technique to be of the order of some parts per million for a vast class of metallic pollutants, including extremely dangerous soil pollutants such as copper, lead and chromium.ENEA guest with HC&M fellowship     

Effects of annealing on crystallinity and phase behaviour of PET/PC block copolymers

The effects of the annealing on the properties of PET/PC block copolymers, obtained by reactive blending in the presence of different catalysts and for different mixing times, have been studied. The annealing, performed in conditions that promote the crystallization, has been used to better understand the role of block length in determining the phase behaviour. The copolymers characterized by blocks with molecular weight larger than 8000 are able to reorganize towards more ordered domains. This rearrangement maintains the phase separation, as two crystalline phases are present before and after annealing, due to the immiscibility of long blocks. In copolymers characterized by blocks with molecular weight equal to about 2500, that is the higher limit for the miscibility in the amorphous state in PET/PC block copolymers studied in this work, the rearrangement of the chains during annealing causes a phase separation leading to two crystalline phases. Only in the copolymers with molecular weight of blocks lower than 1500, the very short block length hinders the crystallization: therefore, only in this case a phase separation does not take place after annealing.     

Underwater sediment analyses by laser induced breakdown spectroscopy and calibration procedure for fluctuating plasma parameters

Laser Induced Breakdown Spectroscopy (LIBS) was applied on sediments directly under water. The aim of the research was to develop a method for measuring the sediment elemental composition, including minor elements, which could be implemented in-situ. The plasma was generated by a double-pulse, Q-Switched Nd:YAG laser operated at 1064 nm. For signal detection, both ICCD and non-gated, compact detectors were used. The major difficulties in underwater sediment analyses are related to the natural and laser induced surface roughness, and to the sample softness. The latter is responsible for the formation of particle clouds above the surface, which scatter both the laser and plasma radiation, and often results in breakdown formation above the analyzed surface. In such cases, a broad sonoluminescence emission from water, formed during the gas bubble collapse was sometimes registered. Under optimized experimental conditions, even by using a non-gated detector and single shot acquisition, it was possible to detect several minor sediment constituents, such as titanium, barium, manganese and others. A crude estimation of the Limit of Detection (LODs) for these elements was performed by underwater measurements on certified soils/sediments. Due to strong shot-to-shot fluctuations in the plasma temperature, well correlated calibration curves, aimed for quantitative analyses, could only be obtained after applying an appropriate data processing procedure. The latter selects automatically only the spectra characterized by similar plasma parameters, which are related to their continuum spectral distribution. Application of such a procedure improves the measurement accuracy also in other surroundings and on samples different from the ones analyzed here.     

Dynamic-mechanical properties and melting points of some aliphatic and partially aromatic polyamides

Some aliphatic and partially aromatic polyamides have been prepared from hexamethylene diamine and the following dicarboxylic acids: deca-, octa-, hexa-methylenedicarboxylic, p-carboxymethylphenoxyacetic, p-carboxyethylphenoxyacetic, p-phenylenedipropionic, p-phenylenediacetic, p-carboxymethoxyphenoxyacetic, β(p-carboxymethyl)phenylpropionic.The dynamic-mechanical properties at 110 Hz have been measured between ?140° and about 200. Three relaxation processes α β and γ have been found: only the main transition α appreciably depends on chemical structure.The influences of the length of repeating unit and of in-chain substitution on melting points, crystallinity and the dynamic-mechanical α transition have been investigated. The results have been discussed in terms of chain flexibility, chain packing and intermolecular forces.     

Chemoenzymatic synthesis of both enantiomers of 3-hydroxy- and 3-amino-3-phenylpropanoic acid

Ethyl (S)-3-hydroxy-3-phenylpropionate (S)-2 was obtained by the asymmetric reduction of ethyl 3-phenyl-3-oxopropionate 1 with the yeast Saccharomyces cerevisiae (ATCC 9080). The kinetic resolution of racemic ethyl 2-acetoxy-3-phenyl-propionate rac-3 with the same microorganism, gave after hydrolysis ethyl (R)- and (S)-3-hydroxy-3-phenylpropionates (R)-2 and (S)-2 which were converted by a straightforward series of reactions to the enantiomers of 3-amino-3-phenyl-propionic acids (S)-6 and (R)-6. The asymmetric reduction and hydrolytic kinetic resolution were also tested with several other whole cell systems under a variety of conditions.     

A support for the identification of non-tryptic peptides based on low resolution tandem and sequential mass spectrometry data: The INSPIRE software

A simple software, to be used as an aid in the identification of non-tryptic peptides based on low resolution (3D-ion trap) tandem (MS/MS) and sequential (MS³) mass spectrometry data, is presented.     

Optofluidic droplet router

This contribution presents an optofluidic droplet router which is able to route and steer microdroplets using optically induced forces created solely by the bulk photovoltaic effect on a nonlinear substrate. The combination of microfluidic tools with the properties of a photorefractive crystal allows for the generation of dielectrophoretic forces that can be either repulsive, leading to virtual barriers, or attractive, creating virtual rails. The sign of these forces is solely determined by the electrical properties of the liquid medium under investigation. Moreover, the induced structures on the bottom of the microfluidic channel are optically reconfigurable, so that the same device can easily be adopted for different purposes. Appropriate droplet‐generating devices are fabricated by UV illumination of SU‐8 and polydimethylsiloxane replica molding of the master structures. The bottom of the channels is formed by an iron‐doped lithium niobate crystal, whose internal electric fields are induced by structured illumination patterns and exert dielectrophoretic forces on droplets in the microfluidic section.

     

Flexural,impact, rheological and physical characterizations of POM reinforced by carbon nanotubes and paraffin oil

The paraffin oil dispersion technique innovated in the recent years to synthesize bulk polymer nanocomposite materials has a uniform dispersion. This research work aims to study the effect of added carbon nanotubes (CNTs) on flexural, impact and rheology behaviors of polyoxymethylene (POM) reinforced by 0–0.03 wt% of CNT using paraffin oil dispersion technique. The wettability and lamellar thickness were measured and rheological performance investigated using a parallel plate rheometer. The flexural and impact mechanical properties were also evaluated. The fracture surfaces were then examined by microscopy. The results showed that the energy to break, flexural strength and modulus increased proportionally with the addition of the amount of CNT in the matrix. For the rheology behavior, the viscosity decreased at the low percentage of CNT and then increased with increase in the percentage weight ratio of CNT in the POM matrix. It was also noted that the water contact angle rose with the increase the CNT percentages. Copyright © 2016 John Wiley & Sons, Ltd.