This paper deals with the characterization of styrene-butadiene-styrene (SBS) block copolymers at molecular level through different techniques. SBS molecular weight distributions (MWD) were measured by Gel Permeation chromatography (GPC) in tetrahydrofuran (THF) solvent and using a calibration curve based on mono-dispersed polystyrene standards; afterwards, the relative molecular weights obtained by GPC were adjusted using a correction factor based on Mark-Houwink-Sakurada parameters for SBS in THF. Quantitative characterization of polybutadiene (PB) structures in SBS was made by solid-state C-13 Nuclear Magnetic Resonance (NMR). A novel method using Fourier transform infrared spectroscopy (FTIR) has been developed for characterizing the SBS composition. This method covers the determination of composition in SBS ranging from 20 to 75 wt% of polybutadiene (PB) and was performed based on a FTIR calibration curve, which was prepared using mixtures of polystyrene (PS) and polybutadiene (PB) of known compositions.