Accurate determination of hexanal in beef bouillons by headspace solid‐phase microextraction gas‐chromatography mass‐spectrometry

Lipid oxidation has great impact on the quality of food products through flavor and taste deterioration, reduction in nutritive value, and potential toxicity of the oxidized food components. Flavor and taste deterioration can be easily perceived and it represents one of the major causes of consumer complaints in the food industry. The deterioration of sensory properties is due to the decomposition products of hydroperoxides that easily isomerize and degrade into volatile compounds. Volatile products are responsible for flavor and taste deterioration. In this study, we present the development of the solid‐phase microextraction gas chromatography‐mass spectrometry (SPME‐GC‐MS) technique to quantify low amounts (μg/g range) of secondary oxidation products, i.e. hexanal. The optimization of SPME parameters is a difficult task because of the possibility of further formation of volatile products during analysis. Different parameters such as type of fiber, exposure time of the fiber to the sample headspace and the optimal temperature of absorption have also been investigated. The complete validation of the method was achieved by the determination of linearity, limits of detection and quantification and repeatability. We demonstrated that the SPME method is a valuable tool for the quantification of low amounts of secondary oxidation products such as hexanal. Therefore, this technique can be used to detect early formation of volatiles.     

Nitriding aluminum alloys by N-multicharged ions implantation: Correlation between surface strengthening and microstructure modifications

This paper deals with the surface strengthening of aluminum alloys by means of a new process allowing multi-charged nitrogen ion implantation. X-ray photoelectron spectroscopy, grazing-incidence X-ray diffraction and atomic force microscopy were used to study microstructural changes involved by implantation. This microstructural study revealed the formation of AlN and AlONγ due to the low nitrogen concentration gradient obtained with multi-charged implantation. Nanoindentation and wear tests were performed to evaluate the mechanical properties of implanted surfaces. A significant improvement of wear resistance was observed as a consequence of the nitride protective layer formation. The observed surface hardening is attributed to both AlONγ and AlN formations and to the precipitation-induced stress.     

Size Effects in Thin Face-Centered Cubic Metals for Different Complex Forming Loadings

Influence of the size effects on the mechanical behavior of face-centered cubic metals was studied for complex loadings close to microforming ones. The effect of a reduction in thickness (t) over grain size (d) ratio on the mechanical behavior for high-purity nickel and copper is investigated for three different loadings by tensile and Nakazima tests (plane strain conditions and balanced biaxial expansion). Experimental results highlight a strong degradation of the mechanical properties of Cu and Ni when the t/d ratio is reduced below a critical value, independently of the strain path. However, this effect occurs if the equivalent plastic strain is larger than a critical level which is strain path dependent and related to the stress triaxiality. The current study reveals that plastic anisotropy is also affected by size effects. An excellent correlation is obtained between the t/d ratio and the thickness reduction, through the mean normal plastic anisotropy parameter which is widely used to estimate sheet formability. A size effect map based on forming limit diagrams is proposed to depict the optimal conditions of microforming.     

Arsenic removal with iron(II) and iron(III) in waters with high silicate and phosphate concentrations

Arsenic removal by passive treatment, in which naturally present Fe(II) is oxidized by aeration and the forming iron(III) (hydr)oxides precipitate with adsorbed arsenic, is the simplest conceivable water treatment option. However, competing anions and low iron concentrations often require additional iron. Application of Fe(II) instead of the usually applied Fe(III) is shown to be advantageous, as oxidation of Fe(II) by dissolved oxygen causes partial oxidation of As(III) and iron(III) (hydr)oxides formed from Fe(II) have higher sorption capacities. In simulated groundwater (8.2 mM HCO3(-), 2.5 mM Ca2+, 1.6 mM Mg2+, 30 mg/L Si, 3 mg/L P, 500 ppb As(III), or As(V), pH 7.0 +/- 0.1), addition of Fe(II) clearly leads to better As removal than Fe(III). Multiple additions of Fe(II) further improved the removal of As(II). A competitive coprecipitation model that considers As(III) oxidation explains the observed results and allows the estimation of arsenic removal under different conditions. Lowering 500 microg/L As(III) to below 50 microg/L As(tot) in filtered water required > 80 mg/L Fe(III), 50-55 mg/L Fe(II) in one single addition, and 20-25 mg/L in multiple additions. With As(V), 10-12 mg/L Fe(II) and 15-18 mg/L Fe(III) was required. In the absence of Si and P, removal efficiencies for Fe(II) and Fe(III) were similar: 30-40 mg/L was required for As(II), and 2.0-2.5 mg/L was required for As(V). In a field study with 22 tubewells in Bangladesh, passive treatment efficiently removed phosphate, but iron contents were generally too low for efficient arsenic removal.     

Fabrication and electroosmotic flow measurements in micro- and nanofluidic channels

An easy method for fabricating micro- and nanofluidic channels, entirely made of a thermally grown silicon dioxide is presented. The nanochannels are up to 1-mm long and have widths and heights down to 200 nm, whereas the microfluidic channels are 20-μm wide and 4.8-μm high. The nanochannels are created at the interface of two silicon wafers. Their fabrication is based on the expansion of growing silicon dioxide and the corresponding reduction in channel cross-section. The embedded silicon dioxide channels were released and are partially freestanding. The transparent and hydrophilic silicon dioxide channel system could be spontaneously filled with aqueous, fluorescent solution. The electrical resistances of the micro- and nanofluidic channel segments were calculated and the found values were confirmed by current measurements. Electrical field strengths up to 600 V/cm were reached within the nanochannels when applying a potential of only 10 V. Electroosmotic flow (EOF) measurements through micro- and nanofluidic channel systems resulted in electroosmotic mobilities in the same order of those encountered in regular, fused silica capillaries.     

Hepatic failure and liver cell damage in acute Wilson''s disease involve CD95 (APO-1/Fas) mediated apoptosis

We gave auditory examples of two semantic categories through headphones to 100 surgical patients anaesthetized with propofol and enflurane. This presentation was made during certain stages of the procedure, potentially associated with arousal, and during steady-state anaesthesia. Postoperative review using category generation tests showed successful priming in a pre-induction group but no evidence of implicit memory in the anaesthetized groups. These results suggest that timing an auditory input to coincide with surgical stimulation does not increase the probability of retrieval of information by this type of testing.     

Virtual enantiomers as the solution of optical activity's deterministic offset problem

Deterministic offsets have remained one of optical activity's most intractable problems. To the extent that the mechanisms by which they are produced do not depend on the chiroptical properties of the sample, they can be eliminated by the subtraction of measurements done on both enantiomers. We show that it is possible to create, by purely optical means, by the sole use of half-wave retarders, the optical antipode of a chiral molecule, to measure the chiroptical properties of the molecule and of its optically generated antipode, and to recover, by subtracting the measurements, the offset-free data of the enantiomer which is physically present. We moreover show that it is possible to do the measurements in a way that eliminates offsets that might occur through the influence of the differing chiroptical properties of the two antipodes. The procedure can be repeated, and by doing so, an almost arbitrarily high precision can be reached. The method is demonstrated by offset-free Raman optical activity back-scattering spectra measured in the so-called scattered circular polarization mode, one of optical activity's so far largely unsolved measurement problems. Such measurements can now be done with 2 mg of substance, in throw-away capillary cells, and on compounds sealed in cylindrical vials.     

Study of the local atomic strain field in a Zr-doped TiAl intermetallic alloy by EXAFS and ab initio FLAPW calculations

The mechanical properties of gamma-TiAl-based intermetallic alloys are strongly influenced by Ti d-Ti d and Al p-Ti d hybridizations. These directional bonds supply good mechanical properties at high temperature but they are also associated with a low ductility at room temperature. Small amounts (about 3%) of additional elements can improve this behaviour noticeably and modify the mechanical properties. In the present case, the addition of zirconium in the gamma-TiAl-based alloys has been reported to increase their ductility at low temperature. Beyond the modifications of the directional bonds which come directly from the band structure, the different atomic volumes of the solute atoms induce local deformation fields which interact with the dislocations. We present ab initio calculations (FLAPW method) compared with an EXAFS study which the aim is to determine the site preference of zirconium in the TiAl lattice and the deformation fields around the solute atoms.