Library · Materials, chemistry & fabrication

What Thermogravimetric Analysis (TGA/DSC) got wrong, from 12 theses

Summary written by a model from the records below: Thermogravimetric analysis and differential scanning calorimetry frequently encounter analytical failures caused by overlapping thermal transitions, unrepresentative heating rates, and unintended chemical decomposition. Researchers also face measurement errors from sample containment difficulties, rapid initial reaction kinetics, and secondary chemical interferences that obscure true material behavior. These records come from graduate theses, 2021 to 2026, each labeled with its degree where the repository states it, and each links to its thesis. They were extracted by language models reading the full text, so treat each as a lead to read, not a verdict.

12
theses
10
institutions
12
failure records
4
failure modes

Plus 8 problems the authors left open, listed at the end.

Failure modes, by theses reporting them

Select a mode to jump to its records.

Dynamic heating rates and transient phases distort thermal stability and kinetic measurements
4
4 theses · 4 institutions · 4 records
Complex decomposition pathways and matrix reactions undermine mass loss quantification
2
2 theses · 2 institutions · 2 records
Experimental calorimetry suffers from early heat loss, poor sample containment, and irreversibility
3
3 theses · 2 institutions · 3 records
Overlapping degradation and thermal transitions prevent resolution of distinct components
3
3 theses · 3 institutions · 3 records

Dynamic heating rates and transient phases distort thermal stability and kinetic measurements

4 theses · 4 institutions

Standard dynamic heating ramps in thermal analysis frequently overestimate degradation onset temperatures compared to slower isothermal conditions. In addition, degradation often initiates during the transient heating ramp before reaching target temperatures, while dynamic cooling cycles fail to capture realistic crystallization kinetics.

Considered and rejected

Considered and rejected: Rejected standard TGA fast ramp rates (5 °C/min) as primary metric for onset decomposition due to significant overestimation of thermal stability compared to GC-FID at 1 °C/min.

Developing novel magnetic ionic liquids and deep eutectic solvents, evaluating their solvation interactions, and utilizing them in microextractions · Iowa State · PhD

Considered and rejected

Considered and rejected: Rejected non-isothermal TGA onset temperature (Tonset) as a reliable metric of thermal stability due to high variance and overestimating isothermal stability by over 100 °C.

Pressurized Mixtures of Ionic Liquids as Process Solvents for Biomass · Virginia Tech · Doctorate

Tried and failed

isothermal kinetic parameter fitting applied to high-temperature thermal degradation. Outcome: worse than baseline. Reason: degradation initiates during the transient heating phase before reaching the target isothermal temperature

Heat transfer modelling, optimisation and monitoring of flashlamp- assisted automated tape placement. · Cranfield · PhD

Considered and rejected

Considered and rejected: Standard DSC heat/cool sintering window criterion rejected for Tb selection; replaced with isothermal crystallization kinetics halftime analysis because standard DSC uses unrealistic fixed dynamic cooling rates.

Additive manufacturing of carbon fiber reinforced thermoplastic polymer composites · Politecnico di Torino · PhD

Complex decomposition pathways and matrix reactions undermine mass loss quantification

2 theses · 2 institutions

Thermogravimetric mass loss measurements fail when reactive matrix elements cause interfering combustion reactions or when complex decomposition occurs under inert atmospheres. These ambiguous mass loss dynamics prevent reliable calibration of element content and obscure the diagnosis of amorphous phases.

Tried and failed

combustion thermogravimetric analysis for polymer quantification applied to silica and fluoropolymer composite matrices. Reason: interfering reactions from co-present silicon and fluorine during combustion skewed mass loss measurements

Structured gas-solid contactors for CO2 removal from air · Georgia Tech · PhD

Considered and rejected

Considered and rejected: Rejected relying on thermal gravimetric analysis (TGA) alone to explain TiOx darkness via carbon doping due to ambiguous sample mass decomposition dynamics.

Nanomaterials and Nanostructures for Full Spectrum Solar Energy Harvesting and Conversion · University at Buffalo · PhD

Experimental calorimetry suffers from early heat loss, poor sample containment, and irreversibility

3 theses · 2 institutions

Solution and differential scanning calorimetry fail when rapid flash reactions occur before sample placement or when samples vaporize inside poorly packed crucibles. Microcalorimetric characterization also suffers from averaging artifacts and errors when reactions lack thermodynamic reversibility, while standard laboratory mixing fails to replicate operational shear and heat release.

Tried and failed

differential scanning calorimetry applied to porous refractory insulating brick. Outcome: unstable. Reason: sample vaporization and low packing density within the crucible

Thermophysical and Molten Salt Corrosion Behavior of Structural Materials for Next-Generation Clean Energy Systems · Georgia Tech · PhD

Tried and failed

isothermal solution calorimetry applied to fast-reacting calcium-rich particulate materials. Outcome: too slow. Reason: Premature flash hydration occurred prior to sample placement in the calorimeter, missing initial heat release

Assessing supplementary cementitious materials for use in concrete : long-term and rapid testing · UT Austin · PhD

Considered and rejected

Considered and rejected: Rejected hand/Hobart mixing of cement paste for calorimetry calibration because it underpredicts the shearing action and heat release rate of ready-mix concrete aggregates.

Assessment of Mass Concrete Thermal Prediction and Failure Criteria: Novel Models, Evaluation Methods, and Case Studies · Georgia Tech · PhD

Overlapping degradation and thermal transitions prevent resolution of distinct components

3 theses · 3 institutions

Thermal analysis struggles to resolve target thermal events when degradation reactions overlap with melting points or when composite layers degrade across the same temperature ranges. Similarly, bulk calorimetric measurements cannot distinguish between thermal aging and mechanical wear because both mechanisms generate identical increases in sample crystallinity.

Tried and failed

differential scanning calorimetry and thermal analysis applied to measuring melting properties of organic solids. Outcome: no signal. Reason: thermal decomposition overlapped with melting at nearly identical temperatures

Crystallisation studies of glycine-based dipeptides: sequence-dependent solubility, cocrystal formation, and kinetics · Imperial · PhD

Tried and failed

thermogravimetric analysis for mass loading determination applied to composite films on polymeric substrates. Outcome: no signal. Reason: overlapping thermal degradation peaks between the active composite coating and the polymer substrate

Electrochemically Tunable Reduced Graphene Oxide Membranes for Ionic and Molecular Sieving · Johns Hopkins · Master's

Considered and rejected

Considered and rejected: Rejected using isolated single DSC/FSC bulk measurements for uranium forensics because thermal aging (e.g. 450°C), mechanical wear, and skiving gradients produce indistinguishable crystallinity increases (tens of J/g)

Pushing the plastic envelope: using physical measurements of polymers to infer uranium enrichment histories · MIT · PhD

Left open by the authors

Problems the authors named and did not get to.

Left open

Investigate structure-activity relationships and kinetics of cyclopropenimines for CO2 adsorption and desorption in solid and solution phases via standardized TGA. Blocker: Requires a wet chemistry lab, synthesis of cyclopropenimine derivatives, and a thermogravimetric analysis (TGA) instrument

Exploration of Carbonyl–Olefin Metathesis Reactions: Ring Opening, Ring Closing and Polymerization. Investigation of Cyclopropenimines for Carbon Dioxide Capture and Its Conjugate · Cornell · PhD

Left open

Quantify residual surfactant in extracted MSR via thermogravimetric analysis and measure silicon release during cryogel degradation. Blocker: Requires a wet laboratory, physical synthesized samples, and thermogravimetric analysis (TGA) equipment.

Biomaterials for acellular dental tissue regeneration · Imperial · PhD

Left open

Perform temperature-ramped TGA experiments using He and N2 purge gases to evaluate gas-phase diffusion and evaporation contributions. Blocker: Requires a physical thermogravimetric analysis (TGA) apparatus and laboratory access.

Thermal stability and solvent applications of protic ionic liquids · Imperial · PhD

Left open

Compare thermal behavior and water desorption free energy across different layered double hydroxides to correlate composition with water retention. Blocker: Requires synthesis of various layered double hydroxide materials and experimental thermal desorption characterization equipment.

Synthesis And Characterization Of Functional Materials Using Silica Colloidial Crystals, Their Inverse Replicas, And Layered Double Hydroxides · Penn · PhD

Left open

Test additional characterized GAC types with varying surface areas and oxygen/silicon contents to isolate mechanisms driving HF and SiF4 generation during PFAS thermal degradation. Blocker: Requires a wet chemistry lab, high-temperature combustion apparatus, FTIR gas cell, and specific GAC materials

The impact of chain length and GAC characteristics on PFAS thermal degradation · University of Nevada, Reno · Master's

Left open

Perform high-temperature TGA-DSC and LFA experiments from room temperature to 2,000°C to measure specific heat and thermal conductivity of char materials. Blocker: Requires specialized high-temperature physical lab equipment (TGA-DSC, LFA) and synthesized physical char material samples.

Development, manufacturing, characterization, and modeling of a novel alumina/polysiloxane/boron carbide ablative composite · UT Austin · PhD

Left open

Apply frictional ignition thermal runaway criteria and tribochemical models to practical high-pressure oxygen engineering systems. Blocker: Vague scope lacking specific engineering targets and requiring physical testing or proprietary engineering design data

Tribochemistry of Frictional Ignition in High-Pressure Oxygen · MIT · PhD

Left open

Determine molecular weights of polymers lacking manufacturer specifications using DSC techniques to refine the dataset. Blocker: Requires physical polymer samples and wet lab experimental equipment (Differential Scanning Calorimetry / DSC).

Data-Driven Approaches for Predicting Polymer Solution Phase Behavior: Integrating High-Throughput Experimentation and Machine Learning · Georgia Tech · PhD

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