Instrumentation
All intstruments used enables measurement under an oxidation atmosphere (air 5N) or inert atmosphere (nitrogen 5N, argon 5N, helium 5,5N). Only the aforementioned gases are available in the laboratory.
Thermogravimmetric and differential thermal analysis combined with mass spectrometry (TG-DTA-MS)
For evolved gas analysis (EGA), a combination of a TG-DTA thermal analyser (Setaram Setsys Evolution, France; operating range of 25–1600 °C, eventually 1750 °C) with an OmniStarTM quadrupoule-type mass spectrometer (Pffeifer Vacuum, Germany) is used.
Differential scanning calorimeter (DSC)
A DSC 131 (Setaram, France) is used with the following operating ranges: (i) from -150 °C to 400 °C; (ii) from ambient temperature up to 600 °C (in oxidation atm.), eventually 700 °C ( in inert atm.). Isotherms or scanning rates slower than 5 °C/min in an oxidation atm. are limited to a temperature of 500 °C. It is recommended that DSC requirements are discussed with laboratory staff in advance.
Simultaneous thermogravimmetric and differential scanning calorimetry (TG-DSC)
Uniquely in the field of thermal analysis, TG-DSC is carried out using a Setaram Sensys Evo thermal analyser (France; operating range from -120 °C to 800 °C) equipped with a symmetrical balance and a Calvet 3D sensor.
Thermogravimetric analyser
TG-750 thermobalance (Stanton Redcroft, England) with an operating range of 25–800 °C.
Differential thermal analysis (DTA)
Custom-built apparatus with an operating range of 25–1100 °C.
Thermogravimetric analysis combined with fourier transform infrared spectroscopy (TGA-FTIR)
For evolved gas analysis (EGA), a combination of a Pyris 1 thermogravimetric analyser (Perkin Elmer, USA; operating range of 40–800 °C) and a Perkin Elmer Frontier infrared spectrometer is used.
Microbalances
- MYA 5 microbalance (Radwag, Poland): max load of 5000 mg; (sensitivity 0.001 mg)
- 4431 electronic microbalance (Sartorius, Germany) with two weight ranges available: (i) max. load of 13.999 mg (sensitivity 1 µg); (ii) max. load of 1.3999 mg (sensitivity 0.1 µg).
