Estudo de espalhamento Raman em cristais de nitrato de monoglicina submetidos a altas pressões.

Abstract

In this work monoglycine nitrate crystals (MGN) were prepared by slow evaporation technique at room temperature and characterization by X-ray diffraction, thermogravimetry, differential thermal analysis, differential scanning calorimetry and Raman scattering at room temperature and under high pressures. After six days, it was possible obtain various crystals of good crystalline quality. The solution was acidic with pH 2,6. From the XRD pattern of the material and the Rietveld analysis, it was found that at room temperature MGN crystallizes in orthorhombic space group (P212121) with four molecules per unit cell. The thermal analysis showed that the material undergoes fusion around 148 ° C and there is no thermal event that features phase transition. In addition, thermal analysis showed that the crystal is stable up to 115 ° C. From the Raman spectroscopy with the hydrostatic pressure on the MGN crystal, it was found that the material undergoes two phase transitions in the pressure ranges of 1.1-1.6 GPa and 4.0-4.6 GPa. These changes are mainly related to lattice modes. The first transition was justified by the disappearance of a band and the appearance of two new bands related to the lattice modes. Moreover, changes in the slop of dω/dP it was also observed for these bands. The second phase transition showed, as main change, the appearance of a strong band at 55 cm-1. No change related to internal modes with increasing pressure was observed, except for the first transition in which a splitting of ν(CCN) was evidenced. These changes can be related to the size of glycine molecule compared to larger amino acid molecules, in which structural phase transitions are followed by molecular conformations. Finally, the results show that the nitrate anions play an important role on the stability of the monoglycine nitrate crystal.