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Miscibility, structure and property relationships were studied by different techniques for various polymer pairs. Four blends of polystyrene (PS), styrene-acrylonitrile copolymer (SAN), polycarbonate (PC) and polyphenylene oxide (PPO) [PS/PPO, PS/PC, PS/SAN and PPO/SAN] were investigated in the entire composition range. Glass transition temperatures were measured by DSC, mechanical properties were characterized by tensile test, methanol absorption was determined at 50 °C. The Flory-Huggins interaction parameter (χ) was derived from Hildebrand solubility parameters, and compared to χ-related quantities calculated from the experimental results. Good correlation was obtained between parameters derived from different methods used for the characterization of polymer/polymer interaction.