Solvates of Indomethacin

Indomethacin is known to exhibit polymorphism and solvates, the different forms obtained do not exhibit the same solubility and their bioavailabilities are different. It is of a prime importance to identify the various polymorphic and solvated forms. This study was carried out by: DSC (different scanning calorimetry), TG (thermogravimetric analysis), X-ray diffraction and thermomicroscopy. Seven solvates, with acetone, benzene, dichloromethane, tetrahydrofurane, propanol, chloroform and diethylether, were isolated and studied. Their formulae have been determined by thermogravimetric analysis and their X-ray patterns on powder are presented, by DSC their behaviour after desolvation is recorded, the temperature and the enthalpy of fusion are measured and by this way the form obtained is deduced. This revised version was published online in July 2006 with corrections to the Cover Date.     

Etude du Systeme Ternaire Se-Te-Sn

This work is a part of the systematic study of the ternary based chalcogenides systems. The aim is to determine the phase equilibrium, and to determine the limits of the phase area. This is done in view to perfecting knowledge of elaboration conditions for new materials and to study of their physical properties. Few works have been devoted to the study of the ternary system Se-Te-Sn, only the cross section SnSe-SnTe has been studied [1] and [2]. The experimental study by DTA, DSC and X-ray diffraction on powder performed at room temperature, exhibits a miscibility gap in the liquid state which narrows as it goes through the Sn-Se binary system. Three cross sections behave as ‘quasi-binary‘ system and six ternary invariants have been exhibited: three ternary eutectics and three ternary quasi-peritectics. This revised version was published online in July 2006 with corrections to the Cover Date.     

Synthesis and Coordination Behavior of a New Hybrid Bidentate Ligand with Phosphine and Silylene Donors

This work describes the synthesis and coordination behavior of a new mixed-donor ligand PhC(NtBu)₂SiC₆H₄PPh₂ ( 1 ) containing both silylene and phosphine donor sites. Ligand 1 was synthesized from a reaction of ortho-lithiated diphenylphosphinobenzene (LiC₆H₄PPh₂) with chlorosilylene (PhC(NtBu)₂SiCl). Treatment of 1 with Se and GeCl₂ resulted in Si^IV compounds 2 and 3 by selective oxidation of the silylene donor. This strong σ-donor ligand induces dissociation of CuCl and PhBCl₂ leading to formation of ionic complexes 4 and 5 respectively. The reaction of 1 with ZnCl₂ and AlCl₃ resulted in the formation of chelate complexes 5 and 7 , respectively, while treatment with EtAlCl₂ and GaCl₃ forms monodentate complexes 8 and 9 . X-ray analysis of 4 showed that the copper is in the spiro center of the two five-membered rings. Moreover, the copper(I)chloride has not been oxidized but dissociates to Cu⁺ and [CuCl₂]⁻. All the compounds are well characterized by mass spectrometry, elemental analysis, NMR spectroscopy, and single-crystal X-ray diffraction studies.     

Thermoanalytical study of nimesulide and their recrystallization products obtained from solutions of several alcohols

Thermogravimetry, differential scanning calorimetry, and vibrational infrared spectroscopy were used to study nimesulide and its recrystallization products that were obtained from solutions of several alcohols. The thermoanalytical measurements were performed in both air and nitrogen atmospheres and the results suggest that, under the experimental conditions used in this paper, it was possible to obtain neither polymorphic nor pseudopolymorphic forms of this drug. In this investigation, quantum chemical approach methods were used to determine the molecular structures using the Becke three-parameter hybrid method and the Lee–Yang–Parr correlation functional. The performed molecular calculations were done with the Gaussian 09 routine and the theoretical calculation results were correlated with the experimental IR vibrational spectrum.     

Time-harmonic acoustic propagation in the presence of a shear flow

This work deals with the numerical simulation, by means of a finite element method, of the time-harmonic propagation of acoustic waves in a moving fluid, using the Galbrun equation instead of the classical linearized Euler equations. This work extends a previous study in the case of a uniform flow to the case of a shear flow. The additional difficulty comes from the interaction between the propagation of acoustic waves and the convection of vortices by the fluid. We have developed a numerical method based on the regularization of the equation which takes these two phenomena into account. Since it leads to a partially full matrix, we use an iterative algorithm to solve the linear system.     

A new differential thermal analysis setup for measuring high pressure phase transitions

A new setup has been recently developed in the toroidal opposed-anvil device ‘Conac 40’ to perform differential thermal analysis in a high pressure range (0–6 GPa). To evaluate the precision and the reliability of the setup, the high pressure melting curve of germanium and the transition points of α-iron have been investigated up to 5.3 GPa and compared with previous results.     

Detonation properties of dense methane-oxygen-diluent gaseous mixtures: application to ram accelerators

Using a 90mm-bore, 3.15 m long detonation tube, experimental detonation characteristics (detonability limits, detonation velocities and peak pressures) of stoichiometric methane-oxygen-diluent mixtures at an initial pressure up to 3.5 MPa have been experimentally investigated. A parametric study has been carried out as a function of both amount and nature of diluent, namely carbon dioxide, nitrogen and helium. The experimental results allowed the adjustment and validation of computations of the Chapman-Jouguet characteristics by means of a thermochemical code. These experimental data associated with validated computations provide a valuable tool, among others, for the choice of the most appropriate mixture composition in the superdetonative combustion mode for ram accelerator (ramac) experiments. The investigations were organized to determine the upper detonable areas of dense ternary mixtures, and to provide detonation velocity data in order to adjust a series of intermolecular parameters involved in the thermochemical code. Received 8 May 1997 / Accepted 15 December 1997