Spectroscopic method of zigzag chain molecules length determination from Raman spectra was developed. The method is based on measuring Raman lines frequencies, corresponding to acoustical modes and different optical modes of chain molecules. The excitation of Raman spectra was produced by continuous argon laser or by pulsed radiation from copper vapor laser. Raman spectra of hydrocarbon and fluorocarbon zigzag structure molecules have been studied. The investigations have been fulfilled for following substances: C n H 2n+2 (n=6, 7, 10), C n F 2n+1 Br (n=6,7,8, 10, 14), C n F 2n+2 , C n H 2n O 2 (n=4, 5, 8, 10, 11, 13, 15, 18). The frequency dependence of some Raman modes on the length of zigzag molecule has been observed. The theory, explaining this dependence, is developed. The obtained results allow estimating fluorocarbon and hydrocarbon molecules length from the Raman spectra parameters.