To Fourier Transform Infrared Spectrometers Coupling Thermal Analyzer

Importance of the Topic

Coupled thermal analysis and FT-IR enable simultaneous measurement of mass and heat flow changes with molecular fingerprinting of evolved gases. This synergy is critical for understanding decomposition, phase transitions and reaction mechanisms in polymers, pharmaceuticals, catalysts and advanced materials.

Study Objectives and Overview

This whitepaper presents concepts and applications of hyphenated thermal analysis to FT-IR using instruments from NETZSCH and Bruker. It reviews different coupling modes, gas cell designs, software integration and illustrates capabilities with case studies on dehydration, decomposition, catalysis and process optimization.

Methodology and Instrumentation

• Coupling modes: external gas cell, internal gas cell and direct PERSEUS integration without transfer line.
• Gas cells: low-volume long-path metal cells with optimized flow, heated to prevent condensation.
• Instrumentation: Bruker INVENIO, VERTEX, ALPHA II FT-IR spectrometers; NETZSCH TGAs (TG 209 F1/F3) and STAs (STA 449, STA 2500, DSC 204, DIL and TMA systems) and PERSEUS compact STA designs.
• Detectors: uncooled DLaTGS for routine high-throughput, LN2-cooled MCT for enhanced sensitivity.
• Software: NETZSCH Proteus and Bruker OPUS fully integrated for synchronized control, data exchange and combined evaluation.

Main Results and Discussion

• Citric acid monohydrate: 3-D FT-IR coupling resolved dehydration and decomposition steps, quantifying water and acid release and polymer backbone collapse.
• Aspirin: two-step mass loss attributed to hydrolysis and thermal degradation with detection of salicylic acid, phenol and CO2.
• Urea decomposition: three-stage release of NH3, HNCO and trihydroxytriazine confirmed by FT-IR and ATR-FT-IR residue analysis.
• Clay firing: analysis of energy release and evolved H2O, CO2, HF and SO2 to optimize ceramic porosity and emission control.
• Silicone synthesis: identification of cyclo-octamethyltetrasiloxane intermediate revealed incomplete polymerization in flawed batches.

Benefits and Practical Applications

• Real-time gas identification improves material characterization and failure analysis.
• Quantitative studies via PulseTA support calibration, adsorption and catalytic reaction monitoring.
• Enhanced QA/QC in pharmaceuticals, polymers and ceramics for residual solvents, impurities and process control.

Future Trends and Potential Uses

Further miniaturization and higher-throughput hyphenated systems, advanced IR detectors, expanded temperature and pressure ranges, integration of GC-MS and AI-driven spectral deconvolution will extend applications in materials science, environmental analysis and process monitoring.

Conclusion

Combining thermal analysis with FT-IR spectroscopy delivers comprehensive mechanistic insight and fingerprinting of evolved species, driving innovation in analytical chemistry, quality assurance and process optimization.

Reference

No specific literature references were provided; instrument and software manuals from NETZSCH and Bruker underpin this overview.