Development and validation of an intrinsic dissolution method for nimodipine polymorphs

The polymorphs of nimodipine, Modification I (Mod I), the metastable racemate, and Modification II (Mod II), the stable conglomerate, were evaluated by means of the intrinsic dissolution procedure. For this purpose, a hydro alcoholic solution (ethanol:water, 50:50, v/v) was selected as the dissolution medium, maintained at 37±0.5°C. Different rotation speeds were tested (50, 75 and 100 rpm) and the lower one was chosen for the test validation. Although the sample initially characterized as polymorph Mod I presented higher intrinsic dissolution rates in all the conditions tested, no statistical differences were noticed between the two polymorphs. This result can be attributed to the partial solution-mediated phase transformation from Mod I to Mod II, detected through X-ray powder diffraction and differential scanning calorimetry. Also, reliable intrinsic dissolution rate data were acquired for the polymorph Mod II. The dissolution method was validated, being considered stable, specific, linear, sensible, accurate and precise.      

Parametric, external and self-excitation of a tower under turbulent wind flow

In this paper the analysis of a self-excited tower under turbulent wind flow is carried out. The structure is considered as a one dof nonlinear system, and the implications of this modeling are deeply discussed. The stationary wind is responsible for self-excitation, while the turbulent part provides both parametric and external excitations. The simultaneous presence of those excitations is taken into account in a specific resonance condition. The periodic and quasi-periodic solutions are studied by means of a perturbation method and the effects of the turbulence on the dynamics of the structure are analyzed.     

On the nonlinear effects of the mean wind force on the galloping onset in shallow cables

Nonlinear Dynamics - The critical aeroelastic behavior of horizontal, suspended, and shallow cables is analyzed via a continuous model accounting for both external and internal damping....     

Structural relaxation of an unentangled polymer in terms of a simple phenomenological approach

The enthalpy relaxation mechanism of a low molecular weight synthesis of polymethylmethacrylate was investigated by means of calorimetric experiments. The data were analyzed in terms of a kinetic approach treating nonlinearity in a different manner with respect to the Tool-Narayanaswamy-Moynihan model. The relaxation isotherms recorded at four different temperatures were well reproduced by this approach that, however, failed in describing the relaxation asymmetry towards the equilibrium after opposite temperature jumps. A modification of the model was proposed with an additional free parameter accounting for the stretching of the relaxation function. In this way all the experimental data were reproduced fairly well.     

Coordination Number of Ternary Mixtures of Spheres†

This paper presents an experimental study of the coordination number of ternary mixtures of particles of sizes 24.4 : 11.6 : 6.4 (mm) by the use of the liquid bridge technique. It generates detailed information about the distributed coordination numbers corresponding to different types of contacts between small, medium and large components. The analysis is focused on the mean coordination numbers corresponding to these contacts. The results indicate that these partial mean coordination numbers vary with the volume fractions of the components while the overall mean coordination number is essentially a constant and independent of particle size distribution.     

Determination of simple bromophenols in marine fishes by reverse-phase high performance liquid chromatography (RP-HPLC)

Brominated phenols 2- and 4-bromophenol (2-BP and 4-BP); 2,4- and 2,6-dibromophenol (2,4-DBP and 2,6-DBP) and 2,4,6-tribromophenol (2,4,6-TBP) have been identified as key flavor compounds found in seafoods. Depending on their concentrations, they were responsible for marine or ocean flavor (shrimp/crab/fish/sea salt-like) or for phenolic/iodine/iodoform-like off-flavor. In this work a new analytical methodology was developed to determine, simultaneously, such bromophenols in fish meats, based on reversed-phased high-performance liquid chromatographic separation (RP-HPLC). The separation of bromophenols was made onto a Lichrospher 100 RP-18 column using water:acetonitrile gradient at a flow rate of 1.0 mL min⁻¹, using absorbance detection at 286 nm, were the 2-BP, 4-BP, 2,4- and 2,6-DBP show significant absorbtivity values and at 297 nm for 2,4,6-TBP. They were separated in 20 min with a good chromatographic resolution (Rs) for the isomeric compounds: 2- and 4-BP, Rs = 1.23; 2,4- and 2,6-DBP, Rs = 1.63. The calibration curves were linear in the bromophenols concentration range of 200.0-1000 ng mL⁻¹. Under optimized conditions, the detection limit of the HPLC method was 127 ng mL⁻¹ for 2-BP; 179 ng mL⁻¹ for 4-BP; 89.0 ng mL⁻¹ for 2,4-DBP; 269 ng mL⁻¹ for 2,6-DBP and 232 ng mL⁻¹ for 2,4,6-TBP. This method has been applied in determination of bromophenols, isolated by combined steam distillation-solvent extraction with 2 mL of pentane/diethyl ether (6:4), from Brazilian fishes samples, collected on the Atlantic coast of Bahia (13°01′S and 38°31′W), Brazil. The concentration range determined were 0.20 ng g⁻¹ (2-BP) to 299 ng g⁻¹ (2,4,6-TBP). The method proposed here is rapid and suitable for simultaneous quantification of simple bromophenols in fish meat. As long as we know, it is the first analytical methodology, using RP-HPLC/UV, which was developed to determine simple bromophenols in fish meat.     

3D model of rigid block with a rectangular base subject to pulse-type excitation

A model of 3D rigid body with a rectangular base, able to rock around a side or a vertex of the base is developed. Eccentricity of the center of mass with respect to the geometrical center of the body is also considered. The equations of motion are obtained through the general balance principle. A one-sine pulse base excitation is applied to the body in different directions. The analyses are conducted with the aim to highlight the role of the period, the amplitude and the direction of the external excitation. In significant ranges of the previous parameters, the results obtained with a bi-dimensional model, that does not consider the 3D rocking motions on a vertex of the base, are not in favor of safety. It is found, in fact, that in several conditions the overturning of the 3D block takes place for amplitudes of excitation smaller than those able to overturn the 3D block.