p-melt-envelope-sampling
P-02 melt envelope by capillary and DSC
Two independent measurements of the same melt band, reported together so that a disagreement between them is visible. The capillary method gives the practical band a maker can feel; the calorimeter gives the peak temperatures that explain it.
Procedure
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01
Melt 40 g of the wax in a water bath to 15 C above its supplier clear point and hold for ten minutes, stirring with a glass rod.
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02
Draw six capillary tubes to a 10 mm column and chill them at 4 C for two hours. Tubes with a bubble or a gap in the column are discarded, not topped up.
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03
Raise the bath at 0.5 C per minute from 25 C. Record the temperature at which the column first deforms (solidus), at which it slumps (slab) and at which it turns fully clear.
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04
Cool at the same rate and record the temperature at which the first crystal appears in each of the six tubes. The median is the congealing point reported on the specimen page.
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05
Run the same lot on the calorimeter at 5 C per minute from 10 C to 90 C, seal and crimp each pan, and report every endothermic peak above 0.2 mW.
A single melt point is a marketing number. What a maker needs is the band and the shape of the transition inside it, which is why every specimen on this site carries four temperatures rather than one, taken from two instruments that fail in different directions.
Instruments used
- Stirred water bath, 0.1 C resolutionGrant GD100
- Capillary tubes, 1.1 mm ID, open both ends100 per box
- Differential scanning calorimeterTA Q20
- Sealed aluminium sample pans, crimped40 ul
- Glass stirring rod, 6 mmno brand
Sampling table
| Sample mass, capillary | 10 mm column |
|---|---|
| Sample mass, calorimeter | 8 to 12 mg |
| Lots per specimen | 3 |
Quantities produced
- Solidus, Cfirst deformation of the column
- Slab temperature, Ccolumn slumps under its own weight
- Clear point, Clast opal haze disappears
- DSC peak temperatures, Cevery peak above 0.2 mW
Environment: Lab bench at 20-23 C, bath controlled to +/-0.2 C, no draught across the capillary rack
Protocols cited
No published burn report cites this protocol yet.