Effect of Dehydration and Urea on Stability of Homosulfamine in Solid States

In the presence of urea in solid states, the stability of unpulverized homosulfamine hydrate (phase I; UHH) is significantly decreased whereas that of unpulverized homosulfamine anhydrate (UHA) is not. The stability of UHH is decreased slightly more by pulverization (PHH). The major objective of this study was to investigate the effects of urea, dehydration, and pulverization on the stability of homosulfamine in solid states. Binary mixtures of UHH and urea, PHH and urea, and UHA and urea in a ratio of 1:1 (wt/wt) were prepared as physical mixtures and were analyzed by scanning electron microscopy (SEM), powder X-ray diffraction (PXRD), and Fourier transform infrared (FTIR) spectroscopy to study their appearance and structural changes before and after storage. PXRD analysis revealed that physical mixtures comprising UHH and urea and PHH and urea have the same diffraction pattern as that of the mixture of UHA and urea after preparation. The dehydration rate of the crystal water of UHH was accelerated by the presence of urea in addition to pulverization. Moreover, the PXRD patterns of the physical mixtures of UHH/urea and PHH/urea were significantly altered during storage, whereas that of UHA/urea was not, which was consistent with the SEM and FTIR results. The particle shape and appearance of UHH varied significantly as a result of pulverization. The stability of homosulfamine was influenced not only by the presence of urea and dehydration but also by the surface state and particle size of the crystalline form.