Hyphenated techniques are highly effective instrument configurations for characterizing the evolved gaseous (EGA) species released from a sample during controlled thermal treatment.
By combining thermogravimetry (TGA/STA/SDT) with spectroscopy (FT-IR), gas chromatography and spectrometric (GC/MS) methods, hyphenation offers detailed insights into chemical composition, thermal behavior, reaction pathways and decomposition mechanisms arriving at the footprint of your sample.
The versatility of your instruments makes them valuable across multiple scientific and industrial domains.
Here are our top five applications used in material characterization:
1. New Material Composition, Reverse Engineering
Information obtained from the study of thermal stability, decomposition kinetics and degassing of materials such as polymers, compounds and electronics is fundamental for developing new materials with properties that present improvements compared to the previous ones.
EGA with REDshift hyphenation allows the composition of the material to be identified, reverse engineered and the purity or impurity of the material to be revealed, allowing the precise detection of contaminants. Controlling thermal properties can provide valuable information on the behavior of the material during processing and use.
Application Example: Thermal Degradation Analysis of Polyvinylpyrrolidone (PVP)
The evolved gas analysis with REDshift hyphenation can be effectively applied to investigate the thermal degradation of polymers such as polyvinylpyrrolidone (PVP) using a TG-FTIR system. With our interface we checked that vinyl pyrrolidone is the main volatile product formed during the decomposition process, indicating that the dominant mechanism involves depolymerization of the polymer backbone into its monomer units. Other concurrent reactions leading to the formation of oligomers are also evident.
2. Polymer Analysis
Hyphenated techniques enable detailed evaluation of polymer thermal stability and degradation mechanisms, supporting the optimization of processing conditions, prediction of shelf-life and verification of product safety.
Thermal analysis can provide information on crystalline, morphology and phase transitions, all of which strongly influence mechanical, rheological and physical properties. EGA further assists in volatilization behavior, promotes optimization of processing conditions, contaminants presence and decomposition pathways specific to polymeric materials.
Application Example: TG-GC/MS Analysis of Gaseous Emissions in 3D Printing
One possible application of TG-GCMS is analyzing the gases produced during a 3D printing process. Generally, when a high-performance polymer feedstock is thermally degraded under helium, three weight-loss steps are revealed, as well as the onset of pyrolysis at approximately 585 °C. The available MS Online and GC Separation modes in GC-MS can identify key gas evolution points at 315 °C and 605 °C. The evolved gases include linear nitrogen-containing hydrocarbons and aromatic compounds, such as phenols and biphenyl derivatives, which indicate an aramid-type polymer. The unpleasant emissions are mainly azoic compounds that are likely used as polymerization initiators.
Evaluating the thermal stability of active pharmaceutical ingredients and formulations under controlled temperature and environmental conditions allows for the prediction of storage stability, development of appropriate packaging solutions and definition of correct handling protocols.
Hyphenated techniques can also help detect polymorphic transitions, residual solvents, degradation products and interactions between excipients and active ingredients.
Application Example: Monitoring Polymorphism and Residual Solvents in Salbutamol Sulphate (SS)
It is possible to monitor polymorphic transitions and residual solvents, such as in the case of evolved gas analysis during thermal degradation of salbutamol sulphate (SS), a medicament widely used for the management of respiratory symptoms. The analysis is used to study the presence of water, ammonia, methanol, CO2, SO2 and other volatile organic compounds produced by the degradation of the sample molecule. The infrared spectra of the evolved gases from the thermogravimetric analysis (TG) of SS are obtained by coupling a thermogravimetric analyzer and a FT-IR spectrometer.
Evaluate the overall adulteration and identification of food processing or treatment methods applied to food products. These techniques support the study of thermal stability, shelf-life, phase transitions and degradation behavior, including the impact of packaging materials. They are also valuable for developing new formulations with tailored textural or functional properties.
In environmental fields, EGA supports the identification of volatile pollutants, characterization of organic fractions in soils or wastes and the assessment of thermal degradation behavior of environmental.
Application Example: Advanced Physico-Chemical Characterization of Chitosan by TGA-FTIR-GCMS
An advanced physio-chemical characterization of chitosan by means of TGA coupled on-line with FTIR and GCMS can be done. Chitosan, a commercially available linear polysaccharide primarily used as an antibacterial agent, as well as in functional coatings and drug delivery systems, has been studied to elucidate its interactions with water and its thermal stability. The analysis combines FTIR and GCMS of the exhausted gas, with the aim of detecting thermal events and identifying degradation products as a function of temperature.
In the energy sector, hyphenation enables the identification of degradation products and reaction intermediates in battery cathodes, anodes and electrolytes, providing essential information for improving safety and stability.
These techniques are also applied to the thermal decomposition of biofuels and energy-storage materials to optimize performance, conversion efficiency and environmental impact.
Application Example: Thermal Degradation Analysis of Solid Polymer Electrolytes by TG-IR-GC/MS
The TG-IR-GCMS analysis system allows for the analysis of a given amount of solid polymer electrolyte. Using solid-state electrolyte instead of the more conventional liquid electrolyte has advantages: higher performance, cyclability and safety. Using evolved gas analysis allows the user to understand the thermal degradation behaviour of the electrolyte and gain a better understanding of the components present in the electrolyte.
Hyphenated thermal analysis provides unique “thermal fingerprints” that support the identification of unknown materials across diverse domains. In forensic science, it is employed for:
The ability to correlate thermal events with chemical species evolution makes hyphenated techniques indispensable for advanced material identification and compliance testing.
