Hierarchically Structured Zeolite Bodies: Assembling Micro‐, Meso‐, and Macroporosity Levels in Complex Materials with Enhanced Properties

Engineering levels of porosity in hierarchical zeolites is a vibrant area of research with remarkable application potential. To gain practical relevance, the superior properties observed for the as‐synthesized powders have to be preserved when they are shaped into suitable technical geometries. Herein, mechanically stable millimeter‐sized bodies are prepared by granulation of mesoporous ZSM‐5 zeolite powders using an attapulgite clay binder. Alkaline treatment of conventional zeolite granules is demonstrated to be unsuitable for this purpose. Multiple techniques are applied to characterize mesoporous zeolite granules with respect to their conventional zeolite counterparts, thus establishing the impact of binder inclusion and granulation on their respective properties. The intrinsic structure and acidity of the zeolite are retained post‐structuring. Gas adsorption and mercury porosimetry confirm the presence of interconnected micro‐, meso‐, and macropores. A wide range of imaging techniques permits visualization of the particle properties, phase distribution, and consequent origins of the distinct levels of porosity within the zeolite granules. The superior adsorption properties of the hierarchical ZSM‐5 zeolite granules are demonstrated using cyclohexane, toluene, and isopropyl alcohol as probe molecules.     

The Influence of Different Processing Stages on Particle Size,Microstructure, and Appearance of Dark Chocolate

The effect of different process stages on microstructural and visual properties of dark chocolate was studied. Samples were obtained at each phase of the manufacture process: mixing, prerefining, refining, conching, and tempering. A laser light diffraction technique and environmental scanning electron microscopy (ESEM) were used to study the particle size distribution (PSD) and to analyze modifications in the network structure. Moreover, colorimetric analyses (L*, h°, and C*) were performed on all samples. Each stage influenced in stronger way the microstructural characteristic of products and above all the PSD. Sauter diameter (D [3.2]) decreased from 5.44 μm of mixed chocolate sample to 3.83 μm, of the refined one. ESEM analysis also revealed wide variations in the network structure of samples during the process, with an increase of the aggregation and contact point between particles from mixing to refining stage. Samples obtained from the conching and tempering were characterized by small PS, and a less dense aggregate structure. From color results, samples with the finest particles, having larger specific surface area and the smallest diameter, appeared lighter and more saturated than those with coarse particles.     

Effects of olive paste fast preheating on the quality of extra virgin olive oil during storage

The olive paste obtained after crushing was fast preheated under different time/temperature conditions and then malaxed in an industrial oil mill (600 kg Frantoio/Leccino olive blend). Legal parameters (peroxides, free acidity and sensory panel), oil yield, total phenolic content, oxidative stability and phenolic profile were monitored during 12 months of storage of the virgin olive oil (VOO) kept in closed bottles in the dark. A fast preheating not longer than 72 s at 38 °C without malaxation lead to an extra VOO with a shelf-life of at least 12-months, similarly to the traditional EVOO obtained with malaxation. A fast preheating not longer than 72 s at 38 °C followed by 10 min malaxation lead to an EVOO with a ‘mild’ sensory profile and a shelf life of at least 12-months. Thus, the use of a specific designed fast preheater instead or before (a shortened) malaxation allows to obtain an EVOO with a low bitter/pungent attribute from olives which are rich of (sometimes unpleasant) phenolic compounds with the aim to meet the preference of targeted groups of consumers. Time and temperature of fast preheating are the critical parameters of the process.     

In situ synchrotron X-ray micro-tomography study of pitting corrosion in stainless steel

Pitting corrosion of stainless steel has been investigated with high-resolution in situ X-ray microtomography. The growth of pits at the tip of stainless steel pins has been observed with 3D microtomography under different conditions of applied current and cell potential. The results demonstrate how pits evolve in stainless steel, forming a characteristic “lacy” cover of perforated metal. In addition, it is shown how the shape of pits becomes modified by MnS inclusions.     

δ18O of Ethanol in Wine and Spirits for Authentication Purposes

Since 1986 the European Union has established official isotopic analysis methods for detecting the illegal addition of sugar and water to wine and to enable geographical traceability. In this paper we investigate the possibility of using analysis of the ¹⁸O/¹⁶O stable isotope ratio (expressed as δ¹⁸O) of ethanol to improve detection of the watering of wine and to determine the origin of ethanol. Sixty‐nine authentic wine samples from all over Italy, 59 spirits from fruit and cereals, 5 chemically synthesized ethanols, one concentrated and rectified must, one beet and one cane sugar, one fresh must, and 6 waters with increasing δ¹⁸O values were considered. Ethanol was recovered by distillation, using a Cadiot spinning band column, following the official OIV methods. The residual water was trapped by storing the distillate for at least 24 h on a molecular sieve. The ¹⁸O/¹⁶O ratio was measured using a pyrolyser interfaced with an isotope ratio mass spectrometer. The δ^‐18O of ethanol is significantly related to the δ¹⁸O of the fermentation water and can be considered as a reliable internal reference. The values ranged from +24‰ to +36‰ in wine (years 2008 to 2012), +10‰ to +26‰ in fruit and cereal distillates, and from –2‰ to +12‰ in synthetic ethanol. The method was shown to be effective in improving detection of the watering of wine and determining the origin of ethanol (from grapes, other fruit, or synthesis), but not in detecting the addition of cane or beet sugar to wine.     

Radical Scavenging,Total Antioxidant Capacity,and Antiproliferative Activity of Phenolic Extracts from Extra Virgin Olive Oil by Cultivar ‘Frantoio’

The beneficial health effects of extra virgin olive oil are due to both its high content of monounsaturated fatty acids and its high content of phenolic compounds, which have recently attracted research interest. In this context, the aim of this work was to examine the in vitro antioxidant and antiproliferative activities of the phenolic extract obtained from extra virgin olive oil from O. europea cultivar ‘Frantoio’ (samples 1–4), one of the main varieties cultivated in Italy. The total phenolic content was determined by Folin–Ciocalteu method and instead the phenolic profile was obtained by HPLC coupled to a diode array detector and mass spectrometry. Extra virgin olive oil extracts exhibited high antioxidant activity through different mechanisms of action and these activities are related to the phenolic content. Sample 3 demonstrated the strongest free radical scavenging activity with IC₅₀ value of 56.5 μg/mL. The reducing ability measured with FRAP assay revealed that samples ranged from 91.3 to 156 μM Fe(II)/g. The same interesting trend was observed with Trolox equivalent antioxidant capacity value. Moreover, the virgin olive oils showed a good oxidative stability ranging between 19 to 32 h. Antiproliferative activity evaluated by SRB assay revealed that phenolic extracts from the cultivar ‘Frantoio’ showed a strong antiproliferative activity against CORL-23 cell line with an IC₅₀ value of 14.5 and 55.9 μg/mL for samples 3 and 1, respectively, and these results are comparable to the positive control vinblastine. Overall, these results showed that extra virgin olive oils from the cultivar ‘Frantoio’, may represent an interesting source of phenolic compounds as functional components that could be consumed in diets and/or used for the elaboration of functional food and pharmaceutical industries.     

Diode Laser Cure of Serigraphic Ink

Laser polymerization of serigraphic ink was performed by diode laser (DL). Experimental tests were carried out by depositing a commercial solvent-based ink on a polyvinylchloride (PVC) sheet. Ink cure was obtained using a 940 nm emission wavelength DL with an almost rectangular spot. We considered different values for laser power, scanning rate and focalization distance and several behaviors were observed depending on the laser fluence, from the uncured ink state to substrate warpage and degradation. Both ink thickness measurement and scratch tests were conducted on laser-processed samples. Analysis of experimental results shows that the full cure can occur within an extremely short time and at very low power values.     

Highly porous polycaprolactone-45S5 Bioglass® scaffolds for bone tissue engineering

Highly porous biocompatible composites made of polycaprolactone (PCL) and 45S5 Bioglass® (BG) were prepared by a solid–liquid phase separation method (SLPS). The composites were obtained with BG weight contents varying in the range 0–50%, using either dimethylcarbonate (DMC) or dioxane (DIOX) as solvent, and ethanol as extracting medium. The porosity of the scaffolds was estimated to be about 88–92%. Mechanical properties showed a dependence on the amount of BG in the composites, but also on the kind of solvent used for preparation, composites prepared with DIOX showing enhanced stress at deformation with respect to composites prepared with DMC (stress at 60% of deformation being as high as 214 ± 17 kPa for DIOX-prepared composites and 98 ± 24 kPa for DMC-prepared ones, with 50 wt/wt_PCL% of glass), as well as higher elastic modulus (whose value was 251 ± 32 kPa for DIOX-prepared scaffolds and 156 ± 36 kPa for DMC-prepared ones, always with 50 wt/wt_PCL% of glass). The ability of the composites to induce precipitation of hydroxyapatite was positively evaluated by means of immersion in simulated body fluid and the best results were achieved with high glass amounts (50 wt/wt_PCL%). In vitro tests of cytotoxicity and osteoblast proliferation showed that, even if the scaffolds are to be considered non-cytotoxic, cells suffer from the scarce wettability of the composites.