Two-Dimensional Correlation Analysis of Temperature-Dependent FT-IR Spectra of Oleic Acid

ABSTRACT

In the present study, variable temperature FT-IR spectroscopic investigations were used to characterize the spectral changes in oleic acid during heating oleic acid in the temperature range from ?30°C to 22°C. In order to extract more information about the spectral variations taking place during the phase transition process, 2D correlation spectroscopy (2DCOS) was employed for the stretching (C?O) and rocking (CH₂) band of oleic acid. However, the interpretation of these spectral variations in the FT-IR spectra is not straightforward, because the absorption bands are heavily overlapped and change due to two processes: recrystallization of the γ-phase and melting of the oleic acid. Furthermore, the solid phase transition from the γ- to the α-phase was also observed between ?4°C and ?2°C. Thus, for a more detailed 2DCOS analysis, we have split up the spectral data set in the subsets recorded between ?30°C to ?16°C, ?16°C to 10°C, and 10°C to 22°C. In the corresponding synchronous and asynchronous 2D correlation plots, absorption bands that are characteristic of the crystalline and amorphous regions of oleic acid were separated.