The solid-state transition mechanisms of ammonium nitrate IV, III, and II were studied by measuring samples simultaneously by Raman spectrometry and differential scanning calorimetry (DSC). The Raman instruments were a Fourier transform Raman spectrophotometer and triple monochromator Raman spectrophotometer with charge-coupled-device (CCD) detector. The spectral data of the transitions were collected simultaneously with the calorimetric data in the temperature-scanning mode of the calorimeter and then isothermally between transitions. The phase transition from phase IV to phase III occurred through an intermediate phase II*, whose lifetime was seven minutes maximum when the onset temperature of the reaction was close to the phase-transition IV → II onset temperature. It is concluded that there is always an intermediate phase II* between IV and III. Simultaneous Raman measurements are shown to be an effective tool for interpreting complex DSC curves.
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