A series of side chain liquid crystalline copolymers having different spacer lengths, copolymer compositions, and chromophore types were synthesized and characterized both in the bulk and at the gas-water interface. Liquid crystalline properties were identified by differential scanning calorimetry (DSC), optical microscopy, and X-ray diffraction (XRD). Copolymer with spacer lengths 4, 5, 10, and 11 showed smectic A (S-A) phases with a batonnet texture. The liquid crystalline (LC) phase stabilized as the spacer increased. Copolymers with different compositions were investigated both as monolayers and transferred films. The isotherms suggest nanodomain formation at time gas-water interface in copolymers with high nitrobiphenyl (NBP) content.