Reported here is the development of a novel evolved gas analysis technique: Sub-Ambient Thermal Volatilization Analysis (SATVA) and its application in characterizing key analyte species from conservation artifacts. In this work SATVA has been applied to the study of volatiles evolution processes occurring in number of model conservation artifacts. The evolution of volatile species from cured formaldehyde resin, leather and metallic artifacts has been studied by SATVA. The specific analytes making up the total quantity of evolved material in each case have been separated and identified using sub-ambient differential distillation and a combination of online mass spectrometry, gas phase IR spectroscopy and GC-MS. The data gathered has been used to provide information on both the degradation processes occurring within the artifacts and the environmental history of the artifacts themselves.