| Summary: | A detailed study of the phase behavior of <i>n</i>-paraffin C<sub>23</sub>H<sub>48</sub> has been performed by means of real-time variable-temperature experiments with synchrotron radiation. Two detectors were employed for simultaneous analysis of the small-angle (SAXS) and wide-angle X-ray-scattering (WAXS) regions. This paraffin presents a very interesting phase behavior, involving two crystal polymorphs, three rotator phases and the liquid state. The Ostwald rule of stages is invoked to find similarities of the rotator phases with the eventual transient mesomorphic structure in the multistage model of polymer crystallization. That study is complemented by variable-temperature Raman experiments covering frequencies down to 150 cm<sup>−1</sup>. It was found that the low-frequency region is the most informative regarding the phase transitions, and specifically the intensity of the first overtone. From these analyses, several parameters are evaluated as function of temperature.
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