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Jacek Chwast jacek.chwast@ees.kuleuven.be Geo- Instituut

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. Measurement conditions. Netzsch STA 409 PC Luxx® : T [25 – 1000 °C]

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Jacek Chwast jacek.chwast@ees.kuleuven.be Geo- Instituut

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

  2. Measurement conditions Netzsch STA 409 PC Luxx®: • T [25 – 1000 °C] • heating rate 10 °C/min • N2 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 furnace Netzsch STA 409 PC Luxx®: • T [25 – 1000 °C] • heating rate 10 °C/min • N2 atmosphere (60 ml/min) • alumina crucibles • simultaneous measurement of mass change (TG) and heat flow (DSC) • 1 analysis (25100025 °C) = 3 hrs sample + reference microbalance

  4. Thermal analysis (TGA/DSC) in a nutshell 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 TG analysis – mass (T) DSC analysis – heat flow (T) • Examples of thermal reactions resulting inheat flow, measured by DSC analysis: • crystallization • melting • glass transitions • DSC applications: • thermodynamic characterization of pure substances • quality control: sample purity • thermal stability studies

  5. Sample compatibility 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 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 • Sample form: • fine powders • compact solids • films, fibers • Ensure good thermal contact between sample and heat flux-sensor: • powders: evenly distributed at the bottomof the sample crucible, gently tamped • Always use the same sample mass (~ 10-30 mg)

  8. Analysis of results Software: NETZSCH Proteus®  (Marsh procedure) Quantification of portlandite (Ca(OH)2) content in cement ~430°C: Ca(OH)2 -> CaO + H2O↑

  9. Analysis of results Software: NETZSCH Proteus®  (Marsh procedure) Quantification of portlandite (Ca(OH)2) content in cement ~430°C: Ca(OH)2 -> CaO + H2O↑ mass loss

  10. Analysis of results Software: NETZSCH Proteus®  (Marsh procedure) Quantification of portlandite (Ca(OH)2) content in cement ~430°C: Ca(OH)2 -> CaO + H2O↑

  11. Analysis of results Software: NETZSCH Proteus®  (Marsh procedure) Quantification of portlandite (Ca(OH)2) content in cement ~430°C: Ca(OH)2 -> CaO + H2O↑

  12. Contact information and reservations 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?

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