We carried out a Raman study of a series of poly(L-lactide) (PLLA) samples annealed for different periods of time and therefore having different crystallin

We present an in-depth analysis of Raman spectra of novel block copolymers of methyl ethylene phosphate (MeOEP) with caprolactone (CL) and L-lactide (LA), recorded with the excitation wavelengths of 532 and 785 nm. The experimental peak positions, relative intensities and profiles of the poly(methyl ethylene phosphate) (PMeOEP), polycaprolactone (PCL) and poly(L-lactide) (PLA) bands in the spectra of the copolymers and in the spectra of the PMeOEP, PCL and PLA homopolymers turn out to be very similar. This clearly indicates the similarity between the conformational and phase compositions of PMeOEP, PCL and PLA parts in molecules of the copolymers and in the PMeOEP, PCL and PLA homopolymers. Experimental ratios of the peak intensities of PMeOEP bands at 737 and 2963 cm⁻¹ and the PCL bands at 1109, 1724 and 2918 cm⁻¹ can be used for the estimation of the PCL—b—PMeOEP copolymers chemical composition. Even though only one sample of the PMeOEP—b—PLA copolymers was experimentally studied in this work, we assume that the ratios of the peak intensities of PLA bands at 402, 874 and 1768 cm⁻¹ and the PMeOEP band at 737 cm⁻¹ can be used to characterize the copolymer chemical composition.