Melting behavior, glass transitions, solvent loss, decomposition, crystallization, and polymorphic transformations frequently determine whether pharmaceutical products remain stable, manufacturable, and commercially viable. Because many of these changes cannot be observed visually or chemically, thermal analysis often provides critical insight into material performance throughout development and manufacturing. Triclinic Labs applies differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), hot-stage microscopy, and complementary techniques to characterize thermal behavior and help clients make informed formulation, manufacturing, quality, and regulatory decisions.
Thermal analysis measures how a material responds as temperature changes. DSC records heat flow; TGA records mass change; microcalorimetry records heat output from small or slow processes; hot-stage microscopy adds visual observation of melting, crystallization, and phase transitions.
Use it for melting points, glass transitions, crystallization, desolvation, dehydration, degradation, moisture/volatile content, amorphous-content work, compatibility screens, cocrystal eutectic observations, and stability-risk interpretation.
Thermal events can overlap, heating can create artifacts, decomposition can mimic or obscure transitions, and DSC/TGA often cannot identify a phase by itself. Pair thermal data with X-ray powder diffraction (XRPD), Raman/infrared (IR) spectroscopy, nuclear magnetic resonance (NMR) spectroscopy, microscopy, or chromatography when identity matters.
Thermal methods can often be scoped for small material quantities, but the amount depends on technique, pan type, replicate needs, volatile content, and whether current good manufacturing practice (cGMP) or validation work is required. Confirm exact amounts at project intake.
XRPD, variable-temperature XRPD (VT-XRPD), dynamic vapor sorption (DVS), Karl Fischer titration, Raman spectroscopy, Fourier-transform infrared (FTIR) spectroscopy, microscopy, and chromatography can compete or complement thermal methods when the question is phase identity, water content, chemical degradation, or performance impact.
FDA reviewers care whether thermal methods are fit for purpose, validated where used for release/stability, specific enough for the quality attribute, and supported by orthogonal evidence when the result affects form control, amorphous content, residual solvent, or degradation claims.
Common mistakes include assigning a DSC peak without residual-solid analysis, using a vented pan when water/solvent retention matters, missing sample-history effects, and reporting onset values without explaining the transition and its relevance.
Triclinic uses thermal analysis to evaluate real-world material behavior involving melting, glass transition, crystallization, desolvation, dehydration, degradation, amorphous content, and thermal stability. Applications include form selection, stability risk assessment, process troubleshooting, residual solvent or water loss evaluation, and cases where DSC, TGA, microcalorimetry, or hot-stage observations explain why a material changes under heat or storage stress.
The table below lists the specific platforms, brands, models, software, detectors, and capability notes relevant to this service area.
| Instrument or platform | Brand, model, software, or detector | Additional capabilities and use |
|---|---|---|
| Thermogravimetric analysis | TA Instruments Q50 and TA Discovery 5500 TGA systems | Mass-loss, moisture/volatile content, decomposition, oxidative stability, and residue/composition analysis. |
| TGA-IR evolved-gas analysis | TA TGA with Thermo Nicolet 6700 IR interface; DTGS detector; gas cell to 250 °C; transfer line to 225 °C; nitrogen or helium purge | Evolved-gas identification, volatile/decomposition-product interpretation, and coupling of weight-loss events to IR spectra. |
| TGA software | Thermal Advantage Release 5.5.3; TRIOS v.4.3.1.39215 for Discovery 5500 workflows | Thermal-method acquisition, processing, reporting, and data review. |
| Differential scanning calorimetry | TA Instruments Q2000 and Q2500 Discovery DSC systems | Melting, crystallization, glass transition, heat capacity, compatibility, and transition-enthalpy measurements. |
| Modulated DSC capability | TA Discovery DSC configuration with modulated DSC support | Separation of overlapping reversible/non-reversible events and improved amorphous-content / glass-transition interpretation. |
| DSC software | Thermal Advantage Software v.5.5.3 | DSC acquisition and thermal-event analysis for cGMP and non-GMP workflows. |
This example shows why visual thermal evidence can be useful when DSC or TGA events overlap or need explanation. Hot-stage optical microscopy can reveal melting, crystallization, and cocrystal formation under a programmed temperature condition. The example below shows formation of a cocrystal at the eutectic region.
These examples include technical resources, regulatory guidances, or literature relevant to the technique. Download buttons are placed at the bottom-left of each example.
Author: Triclinic Labs
Publication date: 2025
Abstract: This application note uses modulated DSC to quantify amorphous content in crystalline API by evaluating heat-capacity change at the glass transition, illustrating how thermal methods can support low-level amorphous-content control and stability interpretation.
Author: Melanie Bevill, Chris Seadeek, Nico Setiawan, Shawn Comella, Blaise Mibeck, and Steef Boerrigter
Publication date: November 2023
Abstract: Solid-form screening and selection connect crystallinity, stability, solubility, hygroscopicity, manufacturability, regulatory needs, and IP objectives. Analytical techniques should therefore be selected according to the development decision rather than a fixed instrument list.
Author: International Council for Harmonisation / FDA
Publication date: 2024
Abstract: FDA notes that ICH Q2(R2) and Q14 describe validation and development principles for analytical procedures used to assess drug substance and drug product quality. These guidances frame FDA expectations for specificity, accuracy, precision, range, robustness, lifecycle management, and fit-for-purpose method evidence.
Use this technique when its evidence better matches the sample, matrix, or development decision.
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View techniqueUse this technique when its evidence better matches the sample, matrix, or development decision.
View techniqueUse this technique when its evidence better matches the sample, matrix, or development decision.
View techniqueUse this technique when its evidence better matches the sample, matrix, or development decision.
View techniqueUse this technique when its evidence better matches the sample, matrix, or development decision.
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Tell Triclinic what sample you have, what decision the data must support, what prior data are available, and whether cGMP, release, validation, or regulatory documentation is required.
