Thermogravimetric Analysis Combined with Calorimetry and Gas-Chromatography/Mass Spectrometry

• Subject Area: Molecular Chemistry
• Term: Funded in 2023
• Project identifier: Deutsche Forschungsgemeinschaft (DFG) - Project number 530331787

In the present application, the procurement of a combined thermogravimetric analysis/differential scanning calorimeter (TGA-DSC) coupled to gas chromatography/mass spectrometry (GC/MS) for the simultaneous investigation and characterization of ionic liquids (ILs) is kindly requested. The system will be installed in the Chair of Inorganic and General Chemistry at the Friedrich-Alexander-Universität Erlangen-Nürnberg (FAU) and represents a central infrastructure component of the newly established Collaborative Research Center SFB 1452 “Catalysis at Liquid Interfaces” (CLINT). In close collaboration with working groups from chemistry, physics, theory, chemical engineering, and material science, the instrument will enable the characterization of the thermal and thermodynamic properties of task-specific (TS) ILs. The newly developed and synthesized ILs are of vital importance for interface-enhanced “Supported Ionic Liquid Processes” (ie-SILP) and “Solid Catalysts with Ionic Liquid Layer” (SCILL) systems in connection with (electro-)catalytic processes at gas/liquid and liquid/solid interfaces within CLINT. The focus is on the idea of using the anisotropic reaction environment at the interface to tailor active sites with unique reactivity. Thus, the device will play a central role in studying interface-enhanced SILP and SCILL, concepts that use custom-tailored ILs to control (electro-)catalytic reactions in which interface-enhanced molecular complexes generate the catalytic properties. Several specific requirements for the device result from the envisioned application areas. Custom-tailored TS-ILs with different thermal and chemical properties must be developed, synthesized, and fully characterized with regard to their thermal stability and sub¬stance properties; thus, leading the way to potential applications. Accordingly, we will have to install an apparatus that allows for the simultaneous thermal analysis (STA) combined with gas-chromatography and mass spectrometry (STA-GC-MS), which combines four standard characterization methods (DSC, TGA, GC, and MS) in a single instru¬ment. With only one sample required, the results of the thermal analyses are exceptionally comparable due to perfectly identical measuring conditions, such as atmosphere, gas flow rate, vapor pressure, heating rate, and thermal contact with the sensor. Thus, it is less time-consuming and reduces the expenses for high-cost materials and elaborate syntheses. Due to wider operating temperature windows (–150 to 1600 °C) of STA instruments – compared to common TGA instruments – temperature-sensitive samples can be examined regarding their thermal properties. Additionally, the in-situ attached GC-MS unit can clearly separate and detect the complex product and pyrolysis mixtures, providing insights into the constitution of the reaction and decomposition products. This gives access to a variety of information on material properties, composition, and stability.

• DFG Programme: Major Research Instrumentation
• Major Instrumentation: Thermogravimetric Analysis Combined with Calorimetry and Gas-Chromatography/Mass Spectrometry
• Instrumentation Group: 8650 Spezielle Kalorimeter
• Applicant Institution: Friedrich-Alexander-Universität Erlangen-Nürnberg
• Leader: Professor Dr. Karsten Meyer