Three new aromatic polyazomethines have been synthesized by solution polycondensation reactions of terephthalic dialdehyde with fluorine containing aromatic diamines. The polymers were obtained in high yields. The investigation of these polymers by means of matrix-assisted laser desorption ionizationtime-of-flightmass spectrometry (MALDITOFMS) proved the initial members of the four theoretical possible series of the corresponding oligomers with 210 repeating units per molecule.