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.     

On the Robustness of Gaussian Elimination with Partial Pivoting

It has been recently shown that large growth factors might occur in Gaussian Elimination with Partial Pivoting (GEPP) also when solving some plausibly natural systems. In this note we argue that this potential problem could be easily solved, with much smaller risk of failure, by very small (and low cost) modifications of the basic algorithm, thus confirming its inherent robustness. To this end, we first propose an informal model with the goal of providing further support to the comprehension of the stability properties of GEPP. We then report the results of numerical experiments that confirm the viewpoint embedded in the model. Basing on the previous observations, we finally propose a simple scheme that could be turned into (even more) accurate software for the solution of linear systems.     

2-Aryl-7,7-dimethyl-5,6,7,8-tetrahydrothieno[3,2-c]azepin-4-ones from 5,5-dimethyl-1,3-cyclohexanedione

A novel synthesis of substituted thieno[3,2-c]azepinones is described. This new approach uses 5,5-dimethyl-1,3-cyclohexanedione (dimedone) as the starting material. Oxime intermediates are obtained in three steps from the aforementioned diketone. Using these intermediates, the title compounds are synthesized in moderate yields.     

Copper(II) complexes with a flexible oxamato ligand

We report on a convenient synthesis of the ligand precursor, diethylethylene-1,2-bis(oxamate), (Et₂H₂oeo, 1), and show how a partial and preferential hydrolysis of the ester group can give rise to the dianionic ligand, (H₂oeo)²⁻. Reaction of this ligand with Cu(II) affords the neutral dimeric species, [Cu₂(H₂oeo)₂], which has a low aqueous solubility. We describe the crystal structure of the hydrate Cu₂(H₂oeo)₂(H₂O)₄ (2) and report magnetic studies that show a weak exchange interaction in the solid. Under more basic conditions and in the presence of Cu(II) ions, we are able to avoid amide cleavage and yet deprotonate the amide group, resulting in the formation of the highly soluble [Cu(Hoeo)₂]⁴⁻ complex anion. The structure of (NBu₄)₄[Cu(Hoeo)₂](H₂O)₄ (3) is described and compared with the recently reported anhydrous phase.     

Solvent-free synthesis of nitrones in a ball-mill

Various C-aryl and C-alkyl-nitrones were synthesized within 0.5–2 h via condensation of an equimolar amount of aldehydes and N-substituted-hydroxylamines under solvent-free conditions in a ball-mill apparatus. Reactions can be performed without the need of excluding air and moisture and yields the expected products with no need for further purification. The study has been complemented by Differential Scanning Calorimetry (DSC) and solid-state ¹³C MAS nuclear magnetic resonance experiments. We have also studied the temperature profile during the reaction. A comparative study with the corresponding solvent-free microwave activated reaction showed the superiority of the ball-milling method; 31 examples are described, including the synthesis of the anti-aging agent C-phenyl-N-tert-butyl nitrone (PBN) and one of its analogues C-2-pyridyl-N-tert-butylnitrone (2-PyBN).     

Adsorption behaviour of cadmium on L-methionine immobilized on controlled pore glass

The adsorption behaviour of Cd onto the relative non-polar L-methionine was studied. To this end, L-met was immobilized on controlled pore glass (CPG), incorporated in a microcolumn and inserted in a flow injection system for Cd preconcentration from aqueous solutions. Binding constant of the system was calculated and it turned to be of 1.99, with sites capacity of n = 3.12. The ratio of Cd moles bound to L-met moles was calculated and it was 0.03:1 at pH 9.0. On-line breakthrough curves were used to study the effect of pH, analyte concentration and influent flow rate on Cd retention. A complementary pH study was added with a titration curve. Transient peak areas revealed that Cd stripping from the column occurred instantaneously. The system achieves an enrichment factor of 130, reaching a detection limit of 0.63 ng L^{− 1} when 10 mL of the solution were passed through the column. The method was successfully applied to Cd determination in the standard reference material (SRM), QC METAL LL2 metals in natural water, as a validation study.     

Diffusion coefficients across polycarbonate microporous membranes

Summary Apparent ionic diffusion coefficients across polycarbonate membranes bathed by two electrolyte solutions have been studied from Nernst-Planck equation using the assumption of constant electric field. From these diffusion coefficients we have also determined the cation transport numbers across the membranes. Six different membranes and two electrolytes (LiCl and MgCl₂) have been considered, at the temperature of 20°C and for concentrations in the range (10⁻⁴÷10⁻¹) mol l⁻¹.

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Riassunto Sono stati studiati coefficienti apparenti di diffusione ionica attraverso membrane di policarbonato magnate da due soluzioni di elettroliti a partire dall’equazione di Nernst-Planck usando l’assunto di campo elettrico costante. Da questi coefficienti di diffusione abbiamo anche determinato il numero di trasporto di cationi attraverso le membrane. Si sono considerate sei diverse membrane e due elettroliti (LiCl e MgCl₂), alla temperatura di 20°C e per concentrazioni nell’intervallo (10⁻³÷10⁺¹) mol l⁻¹.

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Резюме Используя предположения о постоянном электрическом поле, на основе уравнения Нернста-Планка исследуются ионные коэффициенты диффузии через поликарбанатные мембраны, омываемые двумя электролитическими растворами. Из этих коэффициентов диффузии мы также определяем транспорт катионов через эти мембраны. Были рассмотрены шесть различных мембран и два электролита (LiCl и MgCl₂) при температуре 20°C и для концентраций в области (10⁻⁴÷ ÷10⁻¹) моль·л⁻¹.

     

Electronic speckle pattern interferometry analysis of tensile tests of semihard copper sheets

Uniaxial tension tests of semihard copper sheets were studied by means of electronic spekle pattern interferometry (ESPI). The setup allowed the authors to analyze in detail the transitions from elastic to plastic behavior and from homogeneous to inhomogeneous plastic deformation. In agreement with the conventional definition of the yield point for copper fully plastic behavior starded at permanent strains close to 0.005. The strain-hardening coefficient was very low at the early stage of plastic flow (“easy glide”), increasing progressively until values on the order of 0.13 to 0.14 were reached at maximum load. A this point, the appearance of unequally spaced fringes signaled the beginning of inhomogeneous deformation. With ESPI, this occurrence may thus serve as a criterion to establish the forming limit of the material.