FTIR, FT-Raman, and X-ray diffraction techniques were used to determine chain segregations and lamellar structures of the mixed binary n-paraffins with different chain lengths. The results of three different techniques, infrared spectroscopic studies of crystal field splitting, the Raman longitudinal acoustic mode, and the SAXS long period measurements were compared one another to understand the crystallization mechanism of separated or mixed n- paraffin lamellae.