Effect of olive fruit freezing on oxidative stability of virgin olive oil

Several studies have suggested that the phenolic fraction plays an important role during storage and therefore in the shelf life of virgin olive oil. This investigation examines the effect of freezing olives (–18 °C) before processing into oil on the transfer of the phenolic compounds into the subsequent oil, and the consequential changes in oxidative stability. Oil samples obtained from frozen olives (24 h at –18 °C), crushed with and without preliminary thawing, were compared to a control sample; both oils were obtained using a two‐phase low‐scale mill. The oxidative stability in different samples was assessed in terms of primary and secondary oxidation products as measured by peroxide values and oxidative stability index times, respectively. The quality of the oil samples was also checked through the percentage of free acidity and the phenolic content. Phenols were determined by both spectrophotometric assays (total phenols and o‐diphenols) and HPLC‐DAD/MSD. The antiradical capacity of the phenolic fraction was determined by DPPH and ABTS spectrophotometric tests. These analyses showed that thawing of olives before oil extraction led to a significant loss of oxidative stability and phenols; in contrast, samples obtained from frozen olives that were not thawed before crushing showed qualitative characteristics similar to control samples.     

Micromechanical Characterization of Electrophoretic-Deposited Green Films

Low-load indentation experiments have been performed on electrophoretic-deposited films of SiC particles on a graphite substrate. Films with thicknesses between 60 and 300 µm prepared at two current intensities and subsequently dried under different humidities were indented with spherical indenters with nominal radii of 10, 50, and 150 µm. Force-displacement data were analyzed to determine contact pressure and elastic modulus versus depth results. The modulus and contact pressure behavior with depth exhibited opposite trends with indenter radius: the modulus increase was least for the 10 µm and greatest for the 150 µm, whereas the contact pressure was the inverse. The results may be rationalized by plotting modulus normalized to the ratio "contact radius/film thickness" ( a / t ), whereas the contact pressure results at small a / t could be normalized when plotted versus contact strain, i.e., contact radius divided by indenter radius ( a / R ). These approaches enabled the properties of the variously deposited films to be compared. Additional interesting microstructural and cracking behavior patterns are also reported.     

Microwave-assisted polyol synthesis of sub-micrometer Y2O3 and Yb-Y2O3 particles for laser source application

Sub-micrometer powder (100–150 nm diameter) of Yb-doped yttrium oxide was obtained, for the first time, by microwave-assisted polyol (diethylene glycol, DEG) method. This method is based on fast and homogeneous increase of temperature, due to the microwave heating, and on addition of the hydrolysing agent (water) at high temperature. This promotes a fast nucleation followed by a controlled growth of nuclei. Different procedures were used to process the as-synthesized powders. In some cases washing by ultrapure water was used to dissolve nitrate and DEG by-products, this treatment allowed the use of a lower calcination temperature (150–200 °C less) to obtain the crystalline phase. Analysis of the calcined powder showed different levels of structures: from nanocrystal (10–15 nm), to primary particles (100–150 nm), to micrometer soft aggregates (2–4 μm). The microwave-assisted polyol method resulted an easy way to dope yttria with the desired amount of Yb³⁺. This work was carried out in order to prepare particles to be used as rare-earth doped Y₂O₃ and YAG polycrystalline transparent ceramic for laser source applications.     

F-substituted hydroxyapatite nanopowders: Thermal stability,sintering behaviour and mechanical properties

Fluorine-substituted hydroxyapatites are considered promising materials for bone scaffolding. In this study a systematic investigation on F-half substituted hydroxyapatite (F-HAp, Ca₁₀(PO₄)₆OHF) obtained by precipitation is reported. Results on composition analysis, thermal behaviour, and sinterability are presented for a comparison with the respective pure hydroxyapatite. Samples were characterised by electron microscopy, induced coupled plasma-atomic emission spectroscopy, thermal analysis, infrared spectroscopy, N₂ adsorption measurements, X-ray diffraction and dilatometry. A semicrystalline F-substituted hydroxyapatite powder made up of needle-like nanoparticles was obtained. Notwithstanding that it was thermally stable up to 1300 °C, it was sintered at relatively low temperatures obtaining a very fine microstructure with a relevant nano-porosity, beneficial in view of cell adhesion and in-growth.Hardness, elastic modulus and toughness of produced samples were investigated by Vickers–Knoop microhardness testing. Significant improvements of the mechanical properties were observed for the F-substituted hydroxyapatite, in comparison with pure hydroxyapatite.     

Chromium (VI) removal by methylated biomass of Spirulina platensis: The effect of methylation process

Biosorption of heavy metals is an interesting approach to treat industrial wastewaters by an environmentally friendly system. Spirulina platensis biomass, an effective biosorbent for cations, cannot be used to adsorb chromate due to its negatively charged surface close to neutral conditions; therefore, methylation of biomass was performed to increase its adsorption capacity under these conditions. Batch adsorption tests carried out varying both Cr(VI) and methylated biomass concentrations showed that 2–4 g l^?1 of biosorbent were able to remove Cr(VI) with efficiency ≥80%, while higher Cr(VI) levels (43–50 mg l^?1) showed low removal efficiency. The model of Langmuir was shown to describe the adsorption phenomenon better than the Freundlich one. The values of the overall adsorption capacity of methylated biomass suggested that increased biosorbent availability does not necessarily correspond to larger amount of adsorbed metal. FT-IR spectra of dried and methylated biomass of S. platensis allowed us monitoring the efficiency of the methylation process through the analysis of CH and COO^? vibrational stretching modes, taken as diagnostic of this process.     

Rapid FTIR determination of water,phenolics and antioxidant activity of olive oil

A rapid Fourier transformed infrared (FTIR) attenuated total reflectance (ATR) spectroscopic method was applied to the determination of water content (WC), total phenol amount (TP) and antioxidant activity (ABTS ^{. +}) of virgin olive oils (VOO) and olive oils. Calibration models were constructed using partial least squares regression. Oil samples with WC ranging from 289 to 1402 mg water/kg oil, with TP from 46 to 877 mg gallic acid/kg oil and with ABTS ^{. +} from 0 to 5.7 mmol Trolox/kg oil were considered for chemometric analysis. Better results were obtained when selecting suitable spectral ranges; in particular, from 2260 to 1008 cm^?1 for WC, from 3610 to 816 cm^?1 for TP and from 3707 to 1105 cm^?1 for ABTS ^{. +}. Satisfactory LOD values by the FTIR‐chemometric methods were achieved: 9.4 (mg/kg oil) for WC; 12.5 (mg gallic acid/kg oil) for TP, and 0.76 (mmol Trolox/kg oil) for ABTS ^{. +}. The evaluation of the applicability of these analytical approaches was tested by use of validation sample sets (n = 16 for WC, n = 11 for TP and n = 14 for ABTS) with nearly quantitative recovery rates (99–114%). The FTIR–ATR method provided results that were comparable to conventional procedures. Practical applications : The presented method is based on ATR–FTIR in combination with multivariate calibration methodologies and permits a simultaneous evaluation of important quality parameters of VOO (WC, TP and ABTS ^{. +}). This approach represents an easy and convenient means for monitoring olive oil quality with the advantage of ease of operation, speed, no sample pretreatment and no consumption of solvents. The data obtained with this method are comparable to those obtained using the official reference method. Therefore, the technique is highly plausible as an alternative to the standard procedure for routine analysis or control at‐line of production processes.     

Application of a spectroscopic method to estimate the olive oil oxidative status

A rapid Fourier transformed infrared (FTIR) attenuated total reflectance (ATR) spectroscopic method coupled with partial least squares (PLS), was developed to estimate the oxidation degree of extra virgin olive oil (EVOO). The reference values of EVOO oxidation for the FTIR calibration were obtained by the specific absorptions at 232 and 270 nm, due to the presence of conjugated diene (CD) and conjugated triene (CT) groups, as monitored by the UV spectrophotometric determination. Specific washing procedures were applied to the EVOO to obtain EVOOP and EVOOTP samples, without phenolic compounds and without tocopherols and phenols, respectively. To obtain different oxidation degrees covering wide CD and CT ranges, EVOO, EVOOP, and EVOOTP samples were subjected to a forced oxidation at 60°C for 20 days and aliquots of the oils were daily analyzed. Regression of the FTIR/PLS‐predicted CD and CT of individual oxidized oils EVOO, EVOOP, EVOOTP, and all combined oils (EVOOALL) against UV–Visible reference values demonstrated the good quality of the models in terms of R² and RMSECV values. The results of the study indicated that a strong correlation existed between FTIR and UV–Visible peak intensities. Practical applications: The FTIR‐ATR method coupled with PLS elaboration was developed and applied to predict the oxidation degree of EVOO samples with considerable advantages in terms of simplicity, analysis time, and solvent consumption as compared to the standard method. Moreover, suitable adjustments of the equipment could permit a rapid control at‐line in oil sector.     

Theoretical and experimental studies of a new aniline derivative corrosion inhibitor for mild steel in acid medium

4-Chloro-N-(pyridin-2-ylmethyl)aniline (CPYA) was synthesized by a simple and inexpensive method and tested as a corrosion inhibitor in acid medium for mild steel by using gravimetric studies and electrochemical measurements. An average maximum efficiency of 96.0% was achieved at 4.59 mmol/L. Corrosion kinetic and thermodynamic parameters were also analyzed. Surface analyses (atomic force microscopy and scanning electron microscopy) show that protection is enabled by adsorption on the metal, forming a film. Quantum chemical calculations were performed to access information regarding the molecular structure in the corrosive medium and to support interpretation of the results obtained by experimental methods.     

Ferritic stainless steel welding with the A-TIG process

The main advantage of the TIG with flux process (A-TIG welding) is the possibility of obtaining greater penetration of the weld bead while employing the same welding parameters as conventional TIG welding. Various studies have shown the influence of active fluxes on the geometric characteristics of stainless steel austenitic welds. However, little is known about the influence of this process on the geometric and metallurgical characteristics of the weld beads in ferritic stainless steels. In this work, different types of flux are applied when welding ferritic stainless steel with the objective of verifying possible influences on the weld bead's profile, on its visual appearance, on the microstructure, on the hardness of the welded zone and on the impact resistance (Charpy test). The bead-on-plate welds were produced without using any addition metal. Six types of flux were used – one being an oxide produced in a laboratory (TiO₂) and five commercial fluxes. The results showed that use of the flux allows an increase in penetration with significant changes in the appearance of the weld bead. It was also confirmed that the microstructure and the hardness of the weld bead for the steel studied were not affected by the type of flux used, with the microstructure analysed under an optical microscope. The steel in the study showed a high degree of fragility at ambient temperature.     

Effects of Eltrombopag on In Vitro Macrophage Polarization in Pediatric Immune Thrombocytopenia

Immune Thrombocytopenia (ITP) is an autoimmune disease characterized by autoantibodies-mediated platelet destruction, a prevalence of M1 pro-inflammatory macrophage phenotype and an elevated T helper 1 and T helper 2 lymphocytes (Th1/Th2) ratio, resulting in impairment of inflammatory profile and immune response. Macrophages are immune cells, present as pro-inflammatory classically activated macrophages (M1) or as anti-inflammatory alternatively activated macrophages (M2). They have a key role in ITP, acting both as effector cells, phagocytizing platelets, and, as antigen presenting cells, stimulating auto-antibodies against platelets production. Eltrombopag (ELT) is a thrombopoietin receptor agonist licensed for chronic ITP to stimulate platelet production. Moreover, it improves T and B regulatory cells functions, suppresses T-cells activity, and inhibits monocytes activation. We analyzed the effect of ELT on macrophage phenotype polarization, proposing a new possible mechanism of action. We suggest it as a mediator of macrophage phenotype switch from the M1 pro-inflammatory type to the M2 anti-inflammatory one in paediatric patients with ITP, in order to reduce inflammatory state and restore the immune system function. Our results provide new insights into the therapy and the management of ITP, suggesting ELT also as immune-modulating drug.