Injectable smart hydrogels have been investigated as matrices for controlled release of drugs. The attractiveness of these systems is due to their unique sol-gel phase transition in the body, modification-ability and biocompatibility. This study presents a comprehensive investigation of the thermo-reversible and rheological properties of amphiphilic poloxamers P-407 and P-188 F127. Careful experiments have been performed on aqueous solutions with concentrations of poloxamer ranging from 0.1 to 40 wt. %. The rheological behaviour has been evaluated by oscillatory tests at different temperatures, while micellisation and gelation have been investigated by FT-Raman and thermo-gravimetric and calorimetry thermal analysis techniques. The formulations expressed clear temperature and concentration dependencies with higher concentrations exhibiting higher viscosity values, longer water retention times and lower thermal gelation temperatures. The thermal reversibility and shear thinning properties of the formulation were confirmed and showed good correlation with published literature obtained by other characterisation methods.Elucidation of structural changes under different temperatures (and shear rates) will be conducted by real-time in-line Raman, fluorescence spectroscopy and light scattering techniques.