Lyotropic behavior of Gelucire 50/13 by XRD, Raman and IR spectroscopies according to hydration.

The present paper discuss the structural and vibrational properties of polyoxyethylene glycol glycerides (Gelucire 50/13) during the hydration with increasing water from 0% to 80%. The Gelucire 50/13 used as sustained release matrix forming agent in pharmaceutical applications and it was essentially studied by Small and Wide Angle X-ray Scattering (SWAXS), Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy according to the rate of hydration. The hydration behavior of this amphiphilic excipient has been investigated in the spectral range 4000-0cm-1 in Raman spectroscopy, and 4000-600cm-1 in FTIR. At increasing water contents Gelucire 50/13 forms successive bicontinuous to micellar supramolecular structures, and the vibrational changes were directly correlated with this conformational changes of the Gelucire structure. Overall, Raman and IR spectroscopy clearly demonstrated that the different functional groups studied could be characterized independently, allowing for the understanding of their role in Gelucire polymorphism.

Electron distribution on a tilted sample in the high pressure SEM.

The effect of the specimen inclination on the electron distribution at the specimen surface in an HPSEM was investigated by Monte Carlo simulation. A broadening of the electron profile versus the tilt angle was obtained and a relationship between the r(0.9) radius and this tilt angle is proposed. The plot of the electron distribution at the sample surface shows that the classical scattering profile in the standard conditions is modified so that an inclined truncated shape is obtained. This result confirms the difficulty to carry out X-ray microanalysis in low vacuum conditions.

Raman spectroscopy investigation of various saturated monoacid triglycerides.

A study of the vibrational behavior of five saturated monoacid triacylglycerides is performed by Raman spectroscopy at room temperature in the 3100-500 cm(-1) spectral range. The splitting of the CO stretching mode leads to conclude on the existence of two or three geometries of CO in the "knot" group OCO. The CO stretching mode seems to be a good tool for distinguishing the polymorphic forms of the studied triglycerides. The assignments of the different CH stretching modes are performed in the 1500-500 cm(-1) spectral range. The I(2845)/I(2880) (in the CH stretching spectral region) and I(1445)/I(1296) intensity ratios (between the maximal intensity I(1445) of the CH(2) scissoring mode and the maximal intensity I(1296) of the skeletal vibration of (CH(2))(n) in-phase twist) seem to depend on the type of polymorphic forms of these molecules.

The effect of beam diameter on the electron skirt in a high pressure scanning electron microscope.

Helium gas and air are commonly used in the high pressure scanning electron microscope (HPSEM). The presence of a gaseous environment in the specimen chamber modifies the electron beam profile. In order to fully understand the beam-gas interaction, we have investigated the beam-diameter effect for two gases (helium and air) by Monte Carlo simulation. In this calculation, we have assumed that the electron beam is Gaussian and we have explored the influence of the nature of the gas at low voltage. When the beam diameter varies between 1 and 100 nm, there is no influence on the beam profile for these two gases. The resolving power of the HPSEM is not affected by the beam-gas interaction. These theoretical results have been compared with experimental images obtained at low voltage under air and helium gases. The variation of image quality at low voltage has confirmed the interest of helium for use in a Field Emission Gun SEM (FEGSEM) in high pressure (or low vacuum) conditions.