A combined thermogravimetry/differential scanning calorimetry device (TG/DSC) was coupled to single photon ionisation mass spectrometry (SPI-MS) for evolved gas analysis (EGA). Single photon ionisation (SPI) was performed with a new type of VUV light source, the so called electron beam pumped rare gas excimer lamp (EBEL). SPI does not fragment molecules upon the ionisation process. Thus the molecular mass signature of the evolving gases
from thermal composition of carbonaceous material can be directly on-line recorded. In this work the thermo-analytical data
and the SPI-MS information on the released organics is presented and discussed for various samples. Namely biomass (soft and
hard wood), fossil fuel (crude oil and coal) as well as a complex polymer (ABS) are investigated. The general potential of
hyphenating thermal analysis and soft photo ionisation mass spectrometry (EBEL-SPI-MS) for fundamental and applied research
and material analysis is discussed.