Erythritol: crystal growth from the melt.
The structural changes occurring on erythritol as it is cooled from the melt to low temperature, and then heated up to the melting point have been investigated by differential scanning calorimetry (DSC), polarized light thermal microscopy (PLTM), X-ray powder diffraction (PXRD) and Fourier transform infrared spectroscopy (FTIR). By DSC, it was possible to set up the conditions to obtain an amorphous solid, a crystalline solid, or a mixture of both materials in different proportions. Two crystalline forms have been identified: a stable and a metastable one with melting points of 117 and 104 degrees C, respectively. The fusion curve decomposition of the stable form revealed the existence of three conformational structures. The main paths of the crystallization from the melt were followed by PLTM. The texture and colour changes allowed the characterization of the different phases and transitions in which they are involved on cooling as well as on heating processes. The type of crystallization front and its velocity were also followed by microscopic observation. These observations, together with the data provided by PXRD, allowed elucidating the transition of the metastable form into the stable one. The structural changes occurring upon the cooling and subsequent heating processes, namely those arising from intermolecular hydrogen bonds, were also accompanied by infrared spectroscopy. Particular attention was given to the spectral changes occurring in the OH stretching region.
Lopes Jesus
A J
AJ
Faculty of Pharmacy, University of Coimbra, 3004-295 Coimbra, Portugal. ajorge@qui.uc.pt
Nunes
Sandra C C
SC
Ramos Silva
M
M
Matos Beja
A
A
Redinha
J S
JS
D002152:Calorimetry, Differential Scanning; D002626:Chemistry, Pharmaceutical / Q000379:methods; D003460:Crystallization; D004896:Erythritol / Q000737:chemistry*; D005079:Excipients / Q000737:chemistry*; D006860:Hydrogen Bonding; D044367:Phase Transition; D017550:Spectroscopy, Fourier Transform Infrared; D044366:Transition Temperature; D014961:X-Ray Diffraction
D005079:Excipients; D004896:Erythritol