IR spectroscopic analysis of polymorphism in C13H14N4O

IR analysis is used here to investigate the changes in N-N, N-H, CO modes of thermally treated diphenyl carbazide (DPC) during the variation of temperature from room temperature up to ≈160°C. Polymorphism in DPC compound has been studied here by detecting the changes in some IR spectroscopic parameters (e.g., mode shift, band contour) during the elevation of temperature. Also, DSC, X-ray, NMR and atomic mass spectra are used as confirming tools for what is obtained by IR. All of the vibrations of DPC were found to be due to ionic fundamentals 3311 cm(-1), 3097 cm(-1), 3052 cm(-1), 1677 cm(-1), 1602 cm(-1), 1492 cm(-1), 1306 cm(-1), 1252 cm(-1), 887 cm(-1) and 755 cm(-1). The results revealed for the first time that the thermally treated DPC traverse four different phase transformations at 50°C, 90°C, 125°C and 140°C. The crystal structure was found to be amorphous, monoclinic, tetragonal, orthorhombic and amorphous within a temperature range (30°C-160°C). X-ray diffraction patterns support the results obtained by IR and DSC.