Applications of TG-FTIR:
From Polymers to Pharmaceuticals, Foods, and Inorganic Materials

Yoshinobu Hosoi

Winter 2025 Volume 41, No. 1 , 19-24

TG-FTIR, which combines Simultaneous Thermal Analysis (STA) consisting of Thermogravimetry (TG) and Differential Thermal Analysis (DTA) with Fourier Transform Infrared Spectroscopy (FTIR), is an effective method for simultaneously obtaining information about the reactions occurring in a sample upon heating and the resulting reaction products. This paper presents several applications of TG-FTIR in the analysis of polymers, pharmaceuticals, foods, and inorganic materials. In fiber-reinforced plastics (FRPs), bisphenol A is evolved under thermal decomposition, while CO? is released during combustion. For other polymers, H?O and CO? were quantified during combustion. TG-FTIR was also applied to simulate the ceramic debinding process and identify polymer plasticizers. Additionally, TG-FTIR proved effective in analyzing dehydration in pharmaceuticals, thermal oxidation of edible oils, and reactions in inorganic materials such as gypsum dihydrate.

Highlights

  • TG-FTIR combines simultaneous thermal analysis with evolved gas analysis, allowing thermal events to be directly linked to the gases produced during heating.
  • The technique identifies and quantifies reaction products across diverse materials, including polymers, pharmaceuticals, edible oils, and inorganic compounds, providing insights unavailable from thermal analysis alone.
  • Applications range from polymer decomposition and ceramic debinding to pharmaceutical dehydration, food oxidation studies, and gypsum recycling reactions, demonstrating the versatility of TG-FTIR for materials characterization.

Summary

TG-FTIR integrates simultaneous thermogravimetric and differential thermal analysis with Fourier transform infrared spectroscopy to characterize both thermal behavior and the chemical identity of gases evolved during heating. Unlike thermal analysis alone, the combined technique reveals not only when mass loss or thermal events occur, but also the reactions responsible for them.

For polymer analysis, TG-FTIR distinguishes between thermal decomposition and combustion products, identifies resin chemistries through characteristic evolved compounds, and quantifies combustion products such as H₂O and CO₂. Stable FTIR signal intensity enables reliable gas quantification even when the furnace atmosphere changes during analysis. These measurements can be applied to estimate emissions from polymer combustion and to study decomposition mechanisms relevant to recycling and waste management.

The technique is also valuable for ceramic processing, where it can simulate debinding and show how inorganic fillers alter decomposition temperatures and reaction pathways. It can detect additives such as plasticizers by separating volatilization from polymer decomposition, providing detailed information about formulation components.

In pharmaceutical analysis, TG-FTIR confirms whether mass loss results from dehydration or solvent release, making it particularly useful for evaluating hydrates and supporting loss-on-drying studies. For edible oils, it enables real-time observation of thermal oxidation, identifying aldehydes, carbon dioxide, and other oxidation products while correlating chemical changes with thermal events.

Applications extend to inorganic materials such as gypsum, where TG-FTIR tracks dehydration, phase transformations, and high-temperature decomposition. It also clarifies reaction mechanisms during gypsum recycling by identifying the sequential evolution of CO₂ and SO₂, demonstrating its effectiveness for investigating complex solid-state reactions across a broad range of materials.

Frequently asked questions

TG and STA reveal when mass changes and thermal events occur but cannot identify the substances responsible for those changes. TG-FTIR adds evolved gas analysis, allowing reaction products to be identified in real time. This makes it possible to distinguish between processes such as dehydration, decomposition, oxidation, combustion, and additive volatilization while directly correlating chemical information with TG and DTA signals.

The technique identifies gases released during each stage of heating, allowing researchers to distinguish thermal decomposition products from combustion products. For example, epoxy-based fiber-reinforced plastics release bisphenol A during thermal decomposition, while carbon dioxide is produced during combustion of the carbonized residue. This information improves understanding of decomposition mechanisms, recycling processes, and combustion behavior.

Yes. TG-FTIR can quantify evolved gases by calibrating infrared absorption intensity against reference materials with known gas evolution. Because the optical path length remains constant and the signal is not significantly affected by changes in furnace atmosphere, the method provides stable quantitative measurements of gases such as H₂O and CO₂. This capability is useful for estimating emissions during polymer combustion and comparing combustion characteristics among different materials.

During ceramic debinding, organic binders decompose while ceramic powders remain. TG-FTIR shows how the presence of inorganic fillers influences decomposition temperature and changes the composition of evolved gases. These insights help optimize heating profiles, reduce defects during binder removal, and improve understanding of interactions between binders and ceramic materials.

Many additives evaporate or decompose at different temperatures than the base polymer. TG-FTIR identifies characteristic infrared spectra of evolved compounds, allowing plasticizers and other additives to be distinguished from decomposition products. In PVC formulations, for example, the plasticizer evolves before the polymer itself begins producing hydrogen chloride during decomposition, enabling clear separation of these processes.

Many pharmaceutical materials contain water or solvent molecules within their crystal structures. TG-FTIR confirms whether observed mass loss results from dehydration or solvent release by directly identifying the evolved species. This provides greater confidence in interpreting loss-on-drying measurements and evaluating hydrate stability during thermal analysis.

TG-FTIR monitors oxidation reactions as they occur during heating by identifying gases such as carbon dioxide and aldehydes while simultaneously recording thermal events and mass changes. Combined with complementary FTIR measurements of the oil itself, the technique provides insight into oxidation pathways, formation of degradation products, and chemical changes associated with thermal deterioration.

TG-FTIR distinguishes dehydration, phase transformations, and high-temperature decomposition by identifying the gases evolved at each stage. During gypsum heating, it detects water released during dehydration and sulfur dioxide generated during decomposition. When gypsum is reacted with carbon during recycling processes, TG-FTIR reveals the sequence of carbon dioxide and sulfur dioxide evolution, helping clarify the underlying reaction mechanisms.

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