1. First SIM² - WORKSHOP Thermal analysis (TGA/DSC): practical aspects TGA – Thermogravimetric Analysis DSC – Differential Scanning Calorimetry Jacek Chwast jacek.chwast@ees.kuleuven.be Geo-Instituut 23.01.2013

2. Measurement conditions 2 Netzsch STA 409 PC Luxx®: -T [25 – 1000 °C] -heating rate 10 °C/min -N 2 atmosphere (60 ml/min) -alumina crucibles -simultaneous measurement of mass change (TG) and heat flow (DSC) -1 analysis (25  1000  25 °C) = 3 hrs furnace microbalance

3. Measurement conditions 3 Netzsch STA 409 PC Luxx®: -T [25 – 1000 °C] -heating rate 10 °C/min -N 2 atmosphere (60 ml/min) -alumina crucibles -simultaneous measurement of mass change (TG) and heat flow (DSC) -1 analysis (25  1000  25 °C) = 3 hrs furnace microbalance sample + reference

4. Thermal analysis (TGA/DSC) in a nutshell 4 Examples of thermal reactions resulting in mass change, measured by TG analysis: -loss of free water -loss of bound water -decomposition TG applications: -identification and quantification of sample components -thermal stability studies Examples of thermal reactions resulting in heat flow, measured by DSC analysis: -crystallization -melting -glass transitions DSC applications: -thermodynamic characterization of pure substances -quality control: sample purity -thermal stability studies TG analysis – mass (T)DSC analysis – heat flow (T)

5. Sample compatibility 5 Requirements: -no reaction with alumina crucible -no expansion or creep during thermal decomposition Compatible materials (KUL expertise): -clays and other geological materials -cements -slags Limitations: -polymers can be hazardous, as they can foam at high temperatures, -compatibility assessment is necessary for new materials

6. Evaluation of new materials 6 Compatibility assessment: by providing a reference to a thermal analysis or by burning the sample in a furnace at the conditions foreseen for the measurement: –sample composition –temperature range (max. 1000 °C) –inert atmosphere –alumina crucible

7. Sample preparation 7 1)Sample form: –fine powders –compact solids –films, fibers 2)Ensure good thermal contact between sample and heat flux-sensor: –powders: evenly distributed at the bottom of the sample crucible, gently tamped 3)Always use the same sample mass (~ 10-30 mg)

8. Software: NETZSCH Proteus® (Marsh procedure) Quantification of portlandite (Ca(OH) 2 ) content in cement Analysis of results 8 ~430°C: Ca(OH) 2 -> CaO + H 2 O↑

9. Software: NETZSCH Proteus® (Marsh procedure) Quantification of portlandite (Ca(OH) 2 ) content in cement Analysis of results 9 ~430°C: Ca(OH) 2 -> CaO + H 2 O↑ mass loss

10. Software: NETZSCH Proteus® (Marsh procedure) Quantification of portlandite (Ca(OH) 2 ) content in cement Analysis of results 10 ~430°C: Ca(OH) 2 -> CaO + H 2 O↑

11. Software: NETZSCH Proteus® (Marsh procedure) Quantification of portlandite (Ca(OH) 2 ) content in cement Analysis of results 11 ~430°C: Ca(OH) 2 -> CaO + H 2 O↑

12. Contact information and reservations 12 Contact / Training: Jacek Chwast jacek.chwast@ees.kuleuven.be tel. +32 16 3 27593 or +32 16 3 27580 Responsible professor: Jan Elsen TG /DSC instrument: Geo-Instituut Celestijnenlaan 200c Room 01.83 Reservations: - fill in the reservation list in the room 01.83

13. Thank you for your attention Questions? 13