Perovskite has gained significant interest in the past few years, due to its superior light harvesting abilities.  Photovoltaic devices using perovskite as the light harvesting material, have presented an extremely steep rise in efficiency, in an exceptionally short amount of time, when compared to equivalent PV devices.  Efficiencies have risen from 3.8%, up to a certified 20.1% in just 6 years [1].  Although these cells are not yet stabilized, they are still showing promising potential to surpass commercial silicon equivalents.  The main attraction of these devices is the fabrication cost, which are magnitudes smaller than silicon.  They are produced via wet chemistry, and can be easily incorporated into standard thin-film architecture, as well as continuous (roll-to-roll and sheet-to-sheet) manufacturing [2].A perovskite, usually CH3NH3PbI3 or CH3NH3PbCl3 is deposited onto a substrate, normally on top of a TiO2 scaffold layer.  Crystallization of this perovskite is paramount to the performance of the device, with many methods being applied to achieve this.  Annealing the precursor material at a suitable temperature removes any unwanted precursor material, and also crystallises the perovskite layer.  Many parameters can influence this crystallization such as; solvent, substrate preparation, concentration, drying, and annealing conditions.  In this work, evolved gas analysis is utilised to study the annealing process used in scalable deposition techniques like bar coating, and screen printing.    Evolved gas analysis is achieved by the ‘hyphenation’ of two or more analytical instruments (Fig 1.), in this case, an STA (Simultaneous Thermal Analyzer), FTIR (Fourier Transform Infrared Spectroscopy), and a GC-MS (Gas Chromatography – Mass Spectrometry).  Samples are heated in the STA, with any evolved species being transferred directly to the FTIR, and then the GCMS, via a heated transfer line, allowing the gases to be analysed in real time.  Therefore this hyphenation uncovers results and insights, which are not possible with individual techniques.  So far using these methods we have investigated: Annealing of the TiO2 precursor ‘pastes’ used as a scaffold layer, finding ideal sintering times, and whether all organic material had been removed. Annealing conditions for a variety of perovskite solutions, and analysed previously annealed films to determine if any residual solvent was present.