The hydrolysis of alpha tricalcium phosphate (α-TCP) impacts the reaction kinetics and the resulting injectability of minimally invasive cements, cohesion and mechanical properties. Real-time tracking will provide greater insight to the reaction kinetics and an important comparison with the evolution of mechanical properties. A range of spectroscopic methods have been chosen to determine the changes with hydrolysis of β-TCP and compared to X-ray diffraction. FTIR spectroscopy (DRIFT, ATR), Raman spectroscopy and X-ray diffraction were employed to for real-time assessment of the reaction kinetics. Nanosized β-TCP was chosen for a faster reaction time and a mixture with 5% β-TCP also included seeing the effect of a seed. Powders were mixed with water, attened and the reaction followed over time. To minimize the exposure of irradiation, short analysis times were chosen with XRD over the range of 25°-35° and a different probing location was chosen with micro Raman spectroscopy. FTIR-ATR analyzed through the window thus ensuring constant water content in the reaction mixture. Results reveal the advantages with each technique for quick analysis, ease of providing reproducible analysis conditions and the ability to identify changes during hydrolysis. X-ray diffraction showed good phase evolution and could detect early changes in the reaction. All spectra required further analysis by peak deconvolution with the easiest detection by micro Raman spectroscopy. Irradiation was found to remove water and prevent the reaction from reaching completion. The testing conditions are discussed in relation to larger β-TCP particles that react over a longer period of time and reproducible reaction conditions for a comparison between cements.