A Comprehensive Guide to Using High-Temperature Analysis Crucibles in DSC and TGA

What is Differential Scanning Calorimetry (DSC) and How Do Crucibles Play a Role?

Unstable heat flow or uneven melting can lead to wrong conclusions in DSC. Bad crucible choice can distort your analysis, wasting both time and samples.

DSC measures heat flow in materials as they heat up. The crucible holds the sample and ensures accurate, reproducible measurement by controlling the sample environment.

In my DSC work, I rely on aluminum crucibles for their excellent thermal transfer and purity. Platinum and ceramic crucibles get used for high-temperature or special tests. The crucible’s main job is to protect the sample and let the heat flow cleanly between the sample and the instrument’s sensors. The following table shows which crucible type matches the DSC analysis:

Well-matched crucibles keep baseline data flat and boost the quality of every DSC curve your lab records.

How to Properly Prepare Your High-Temperature Crucible for TGA Testing?

TGA results can become wrong if the crucible holds residue or has damaged surfaces. Cross-contamination or missed details often ruin whole test series.

Always clean, inspect, and bake your crucibles before TGA analysis to prevent contamination, reduce baseline drift, and support precise weight measurements during thermal decomposition.

I use a step-by-step checklist for every run: (1) Wash all pans in a lab washer, (2) dry thoroughly, (3) check for cracks or stains, and (4) pre-bake at a temperature just below the main test. Pre-baking removes hidden moisture and surface contaminants. Only flawless crucibles reach the instrument tray. Table below summarizes my prep workflow:

This regular routine cuts down on failed runs and protects sensitive TGA sensors from damage or drift.

The Do's and Don'ts of Using Crucibles in High-Temperature Analysis

Skipping best practices or using the wrong technique with crucibles can end in broken devices or missing data—costing your lab time and money.

Do always use dedicated tools, handle pans with clean gloves, and check fit before each run. Don’t scrape, overheat, or use pans beyond their rated lifespan.

Over many years, I have found these habits stop most lab problems. Always log pan usage to avoid using old or worn-out crucibles. Rotating pans avoids early wear. Never overload crucibles or force them into position. See my habit breakdown here:

Strong habits and strict do’s and don’ts keep most errors and losses out of my high-temperature analysis work.

Understanding the Crucible Selection Process for Accurate Thermal Testing

Poor crucible selection leads to bad test sensitivity and off-target results. Labs risk wasting time, samples, and budget if they skip this step.

Choose crucibles for thermal analysis by matching material, volume, instrument type, and max temperature to your sample and testing needs.

I always start selection with a review of the test protocol. Critical samples need non-reactive materials, while routine tests can use lower-cost pans. Volume must fit both the sample and the instrument tray. Only then do I match the max temperature. My comparison table here:

The labs that choose and log crucible specs for each test class see better accuracy, less downtime, and lower operating costs.

Conclusion

Correct crucible handling, preparation, and selection protect your data and equipment, making thermal analysis in DSC and TGA accurate, repeatable, and reliable for all lab users.

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