Development and the Implementation of High-Temperature Reliable Heaters in Plasma Spray Technology

Many problems have been encountered during development of reliable high-temperature heaters by means of atmospheric plasma spray and procedures commonly adopted in thermal spray technology, especially due to poor steel substrate corrosion resistance, notably affected by grit-blasting operations, but also deriving from contamination of insulating layers, dielectric arcs, and failures due to hot spots in the heating elements. While seeking the origin of these problems, a close scrutiny of every single step of the preparation process and analyses of the coatings were carried out using laser confocal scanning microscopy, optical and electronic microscopy, fluorescence analysis, X-ray diffraction, and ancillary techniques. The electrical properties of both alumina layers and metal strips prepared with Ni, NiCr, NiAl commercial powders for the heating elements were studied and cross-related to the failures in the heaters. The article reports the main results of these investigations, delineates the innovations introduced to overcome or circumvent the problems, and underlines the distinct characteristics of new heaters, whose reliability has been proven up to now with temperatures of up to 600 °C in air.     

Characterization of lignite low-severity depolymerization products

Oils and asphaltenes derived from direct extraction and several mild depolymerization processes have been studied. The asphaltenes have been fractionated by column adsorption chromatography (with deactivated silica gel) and benzene, THF and MeOH were used in sequence as eluothropic series. Clear chemical separation between one aromatic and two polar fractions has been obtained, giving high percentages recovery. The fractions have been characterized by VPO, FT-IR, ¹H-NMR and elemental analysis. Several structural parameters of oils have been calculated. These oils can be assimilated to equivalent average hydrocarbons having between 10 and 20 carbon atoms and an aromatic carbon percentage oscillating between 47 and 66%. In general, the degree of substitution in aromatic rings is low and the presence of phenolic groups is limited. The majority of the carbons are aromatic and these rings show low degrees of condensation.     

New ionization chambers for beta and X-radiation

Two new ionization chambers were designed, constructed and tested in beta and X-radiation fields. They have a circular form, a sensitive volume of 0.6 cm³ and collecting electrodes of graphite and aluminium. The short- and long-term stability checks and the lack of current leakage indicate that the present performance of the chambers is comparable to that expected from secondary standards. The differential energy dependence of both chambers permits effective-energy determination of unknown X-radiation fields. The chambers display applicability for ⁹⁰Sr + ⁹⁰Y radiation detection.     

Room-Temperature Degradation of t-Zr(Pr)O2 in an Aqueous Suspension Revealed by Perturbed Angular Correlations

This paper deals with the phase stability of an aqueous suspension of tetragonal Zr_0.9Pr_0.1O₂ (20 wt%/vol%) at room temperature as a function of the aging time. The suspension is investigated in situ using the highly localized Perturbed Angular Correlations technique. The results indicate that an almost fully reversible degradation process toward monoclinic zirconia takes place through a first-order reaction of rate constant k =0.7 day⁻¹. Two successive diffusion mechanisms are observed that are interpreted as OH⁻ ions' migration in the grain surface and then, as proton defects' diffusion into the bulk.     

Antioxidant activity and phenolic contents of Olea europaea L. leaves sprayed with different copper formulations

Olive trees (Olea europaea L. Cv. Cobrançosa) from the northeast of Portugal were sprayed with three different copper formulations [bordeaux mixture (copper sulphate + calcium hydroxide − 20% Cu), copper hydroxide (40% Cu) and copper oxychloride (50% Cu)] to control olive fungal diseases. The residues of copper in olive leaves, harvested at different times, were evaluated by atomic absorption spectrometry. At all the collection times, treated olive leaves had significantly higher copper contents, compared to the control. The different copper amounts in pesticide formulations lowered the leaves contents in total phenols and hence their antioxidant properties. Olive leaves sprayed with copper oxychloride possessed the highest copper levels and the lowest content in phenols, which influenced its antioxidant activity (higher EC₅₀ values for reducing power, scavenging effect on DPPH radicals and inhibition of erythrocyte hemolysis). Leaves without copper residues proved to be a good natural source of antioxidants, giving values comparable to the reference compounds.     

Activity and thermal stability of antioxidants by differential scanning calorimetry and electron spin resonance spectroscopy

Heat flux differential scanning calorimetry (DSC) and electron spin resonance spectroscopy (ESR) were used to assess the activity and the thermal stability of antioxidants in four vegetable oils. Sunflower oil (SO) and high oleic sunflower oil (HOSO), both rich in diunsaturated fatty acids (FA), low trans oil (LT) and partially hydrogenated palm oil (PHPO), both containing monounsaturated FA, were analyzed by isothermal heat flux DSC, with or without 300 mg/kg of antioxidant: ascorbyl palmitate (AP), α-tocopherol (αT), δ-tocopherol (δT) and propyl gallate (PG). DSC experiments showed that δT is the most effective antioxidant for SO and PG for the less unsaturated oils. SO and PHPO were also analyzed by ESR at 120 and 145 °C, respectively. ESR results confirm the strongest antioxidant activity of δT and PG for SO and PHPO, respectively. Therefore, the present study demonstrates that DSC and ESR are valuable technologies to study activity and stability of antioxidants at high temperature. Moreover, experiments performed in the presence of the spin-trap N-tert-butyl-α-phenylnitrone (PBN), suggest that δT delay lipid oxidation through a different reaction mechanism when compared to αT. A different mechanism between tocopherols isomers in delaying lipid oxidation has been hypotized.     

Effects of Lysine and Methionine Fortification on Dough and Bread Characteristics

Wheat flour from the Hermosillo Hard Red Spring cultivar in Sonora, Mexico was fortified with various levels of lysine and methionine. The effects of added amino acids on the rheological properties were measured by the Brabender Farinograph and the Chopin Alveograph. Nutritional characteristics were measured by Protein Efficiency Ratio (PER). Dough development and stability times were not significantly different between control and fortified flours. Water absorption and Alveograph results indicated differences between samples. PERs were significantly improved by fortification. Overall bread acceptability was not significantly different from unfortified samples.     

Determination of flavonoids in a Citrus fruit extract by LC–DAD and LC–MS

Flavonoids are a group of polyphenolic compounds with health-related properties. Citrus fruits are rich in flavonoids and their extracts are being used as functional ingredients for several industrial products. A new high performance liquid chromatography technique with an UV photodiode-array detector was used to analyze flavonoids of an extract of Citrus species. To our knowledge this is the first study that reports isoquercitrin presence at a level of 77.3 mg/100 g in a sample made of Citrus fruits; four other flavonoids were quantified as rutin (326.59 mg/100 g), naringin (338.36 mg/100 g), quercetin (96.35 mg/100 g) and naringenin (2.35 mg/100 g). Identification was confirmed by a liquid chromatography mass spectrometer system. Method validation was achieved, providing an analytical technique that can be used to detect trace amounts of these compounds in Citrus extracts with an extremely rapid sample preparation.     

Chemical stability of some poly(amide imide) type polymers

The stability of some heterocyclic poly(amide imide)s in acidic and alkaline medium was compared to the structurally related polyimide and poly(amide imide)s without other heterocyclic groups. All the polymers have high stability in acidic medium. The introduction of additional heterocycles such as 1,3,4-0xadiazole or phenylquinoxaline into the macromolecular chain of a poly(amide imide) increases substantially the resistance to alkaline medium. Polyamides containing imide rings only in the side chain are more stable to hydrolysis than related polyamide having imide units in the main chain.