Synthesis and acid digestion of biomorphic ceramics: determination of alkaline and alkaline earth ions

Ceramic and glass are some of the more recent engineering materials and those that are most resistant to environmental conditions. They belong to advanced materials in that they are being developed for the aerospace and electronics industries. In the last decade, a new class of ceramic materials has been the focus of particular attention. The materials were produced with natural, renewable resources (wood or wood-based products). In this work, we have synthesised a new biomorphic ceramic material from oak wood and Si infiltration. After the material characterization, we have optimized the dissolution of the sample by acid attack in an oven under microwave irradiation. Experimental designs were used as a multivariate strategy for the evaluation of the effects of varying several variables at the same time. The optimization was performed in two steps using factorial design for preliminary evaluation and a Draper-Lin design for determination of the critical experimental conditions. Five variables (time, power, volume of HNO3, volume H2SO4 and volume of HF) were considered as factors and as a response the concentration of different metal ions in the optimization process. Interactions between analytical factors and their optimal levels were investigated using a Draper-Lin design.     

High-temperature thermal behaviour of Cr-Doped LiMn<Subscript>2</Subscript>O<Subscript>4</Subscript> spinels synthesized by the sucrose-aided combustion method

Chromium doped spinels LiCr_YMn_2−YO₄ (0.2≤Y≤0.8) has been synthesized by the sucrose-aided combustion procedure. The thermal behaviour, phase homogeneity and structural characteristics of the samples were studied by thermal analysis, coupled mass spectrometry, and room-and high-temperature X-ray diffraction methods. It was found that the ‘as prepared’ samples contained residual organic impurities undetectable for X-ray diffraction, that burn out completely at 400°C. Samples treated between 400 and 750°C are single phase spinels, whose crystallites size increase from 10 to 50 nm on increasing the temperature. Cr-doping enhances the thermal stability of the spinels, which augments on increasing the Cr content Y. The enhanced thermal stability of the spinels has been accounted for based on the high excess stabilization energy of Cr³⁺ in octahedral ligand field.     

Retention of lysozyme activity by physical immobilization in nanocellulose aerogels and antibacterial effects

Aerogels prepared from aqueous dispersions of anionic and cationic cellulose nanofibrils (CNFs) were investigated as solid supports for enzymes and silver nanoparticles and to elicit a sustained antibacterial effect. The imparted stabilization in dry conditions was studied with aerogels that were cast after mixing the enzymes with CNFs followed by dehydration (freeze-drying). The activity of lysozyme immobilized in the given CNF system was analyzed upon storage in liquid and air media. In contrast with aqueous solutions of free, unbound enzyme, which lost activity after the first day, the enzyme immobilized physically in unmodified and cationic CNF presented better stability (activity for a longer time). However, the enzyme activity was reduced in the case of anionic CNF, which was prepared by TEMPO-mediated oxidation (TO-CNF). Both humidity and temperature reduced the stability of the enzyme immobilized in the respective CNF aerogel. The antibacterial activity of CNF aerogels carrying lysozyme was also tested against gram-negative and gram-positive bacteria. The results were compared with those obtained from CNF systems loaded with silver nanoparticles (AgNP) after in situ synthesis via UV reduction. Storage in cold or dry conditions preserved the activity and antibacterial performance of enzyme-loaded CNF aerogels. As expected, the lysozyme-containing aerogels showed lower inhibition than the AgNP-containing aerogel. In this latter case, the antibacterial activity depended on the concentration and size of the nanoparticles. Compared to unmodified CNF and TO-CNF, the aerogels prepared with cationic CNF, loaded with either lysozyme or AgNPs, showed remarkably better antibacterial activity. Similar experiments were conducted with horseradish peroxidase, which confirmed, to different degrees, the observations derived from the lysozyme systems. Overall, the results indicate that non-toxic and biodegradable CNF is a suitable support for bio-active materials and is effective in protecting and retaining enzymatic and antibacterial activities.     

Kinetic-fluorimetric determination of microamounts of cerium(IV) by means of sodium 4,8-diamino-1,5-dihydroxyanthraquinone-2,6-disulphonate

Summary A kinetic method for determination of traces of Ce(IV), based on the oxidation of sodium 4,8-diamino-1,5-dihydroxyanthraquinone-2, 6-disulphonate is described. The reaction is monitored by means of the fluorescence of the oxidation product ( _ex=525nm, _em=585 nm), and allows determination of 0.02–0.37 ppm Ce(IV). The proposed method has few interferences.

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Kinetisch-fluorimetrische Bestimmung von Mikromengen Cer(IV) mit Natnum-4,8-diamino-1,5-dihydroxyanthrachinon-2,6-disulfonat

Zusammenfassung Eine kinetische Methode zur Bestimmung von Spuren Cer(IV) mit Hilfe von Natrium-4,8-diamino-1,5-dihydroxyanthrachinon-2,6-disulfonat wurde beschrieben. Dabei wird ein fluoreszierendes Oxydationsprodukt gebildet, das bei 525 nm angeregt mit einer maximalen Emission bei 585 nm fluoresziert. Die Reaktion ermöglicht die Bestimmung von 0,02–0,37 ppm Cer(IV). Die vorgeschlagene Methode wird nur durch wenige Störungen eingeschränkt.

     

Conversion from n bands color space to HSI n color space

This paper presents the method to get the equations that transform a color space of n independent primary colors to the HIS _n color system (H: hue, S: saturation, I: intensity); n indicates the number of bands and the shape of the HIS _n space. For n = 3 the structure is a double triangular pyramid, for n 4 it is the structure of the double pyramid tetrangular, and so on.     

Magnetic and structural properties of mechanically alloyed Tb0.257−x Nd x Fe0.743 alloys, with x = 0 and 0.257

The alloys between a transition metal and a rare earth present magnetic and magneto optical properties of exceptional interest for the production of magnetic devices for information storage. In this work we report the magnetic and structural properties, obtained by Mössbauer spectrometry (MS) and X-ray diffraction (XRD), of Tb_0.257?x Nd _x Fe_0.743 alloys with x?=?0 and 0.257 prepared by mechanical alloying during 12, 24 and 48 h, to study the influence of the milling time in their magnetic and structural properties. The X-rays results show for all the samples that the α-Fe and an amorphous phase are always present. The first decreases and the second increases with the increase of the milling time. Mössbauer results show that the amorphous phase in samples with Nd is ferromagnetic and appears as a hyperfine field distribution and a broad doublet, and that as the milling time increases the paramagnetic contribution increases. For samples with Tb the amorphous phase is paramagnetic and appears as a broad doublet which increases with the milling time and for 48 h milling it appears an additional broad singlet.     

Scattering of a relativistic scalar particle by a cusp potential

We solve the Klein–Gordon equation in the presence of a spatially one-dimensional cusp potential. The scattering solutions are obtained in terms of Whittaker functions and the condition for the existence of transmission resonances is derived. We show the dependence of the zero-reflection condition on the shape of the potential. In the low-momentum limit, transmission resonances are associated with half-bound states. We express the condition for transmission resonances in terms of the phase shifts.     

Controlled release from a nanocarrier entrapped within a microcarrier

This study illustrates the entrapment of the dye molecule fluorescein sodium salt (FSS) by hydrogel nanoparticles, which are in turn confined inside a water-in-oil-in-water double-emulsion globule, and its subsequent release by the action of the competing agent hydrochloric acid (HCl). Thus, a "double carrier" concept is being introduced in which a nanoscale delivery vehicle is being transported by a microscale delivery vehicle in order to simultaneously take advantage of both systems. This may facilitate storage and handling while protecting the active substance and improving its action upon application.     

Production of palladium nanoparticles supported on multiwalled carbon nanotubes by gamma irradiation

Palladium nanoparticles were produced and supported on multiwalled carbon nanotubes (MWCNT) by gamma irradiation. A solution with a specific ratio of 2:1 of water-isopropanol was prepared and mixed with palladium chloride and the surfactant sodium dodecyl sulfate (SDS). The gamma radiolysis of water ultimately produces Pd metallic particles that serve as nucleation seeds. Isopropanol is used as an ion scavenger to balance the reaction, and the coalescence of the metal nanoparticles was controlled by the addition of SDS as a stabilizer. The size and distribution of nanoparticles on the carbon nanotubes (CNT) were studied at different surfactant concentrations and radiation doses. SEM, STEM and XPS were used for morphological, chemical and structural characterization of the nanostructure. Nanoparticles obtained for doses between 10 and 40 kGy, ranged in size 5-30 nm. The smaller nanoparticles were obtained at the higher doses and vice versa. Histograms of particle size distributions at different doses are presented.     

On-line preconcentration of mercury by sorption on an anion-exchange resin loaded with 1,5-bis[(2-pyridyl)-3-sulphophenyl methylene] thiocarbonohydrazide and determination by cold-vapour inductively coupled plasma atomic emission

1,5-Bis[(2-pyridyl)-3-sulphophenyl methylene] thiocarbonohydrazide (PSTH) immobilized on an anion-exchange resin (Dowex) has been used for the on-line preconcentration of mercury from biological samples and waters prior to its determination by inductively coupled plasma atomic emission spectroscopy. The metal was eluted from the column using a solution of 2 M HNO(3) and mixed on-line with SnCl(2). The optimum experimental conditions were evaluated for the continuous preconcentration of Hg, the direct generation of mercury vapour and the final determination of this element by ICP-AES. The enrichment, together with low blank levels of the optimized procedure, allow the simple determination of this toxic element at concentrations down to a few nanograms per milliliter. The proposed method has a linear calibration range 5-1000 ng ml(-1) of mercury, with a detection limit of 4 ng ml(-1) (S/N=3) and a sampling rate of 40 h(-1), investigated with a 9 ml sample volume. The precision of the method (evaluated as the relative standard deviation obtained after analyzing ten series of ten replicates) was +/-3.6% at the 10 ng ml(-1) level of Hg(II) and +/-1.3% at the 100 ng ml(-1) level. The accuracy of the method was examined by the analysis of certified reference materials.