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Samarium: Oxide Reduced with Graphite at 1700 °C in Vacuum and Distilled Twice (Downing, Gorski and Koerner, US 3,104,970)
Samarium holds on to oxygen too hard for ordinary smelting. Heated with graphite in a hard vacuum it boils off as samarium carbide vapour; a second distillation of that carbide, caught on a tantalum plate, gives the metal itself.
Result: samarium metal, 99.7 % pure.
Source: J. H. Downing, H. L. Gorski and E. L. Koerner, US 3,104,970 (1963), Example I. Work at 1700 °C under vacuum. Picture drawn by Youblob.
Advanced
1 day
Instructions
1
1
Mix and pellet
Mix and pellet
Mix intimately 79 parts by weight of 99.9 % samarium oxide with 21 parts of powdered graphite (12.7 % more carbon than the oxygen needs), with no particle larger than about 50 microns. Press into pellets 0.75 in across; pellets let the gases and vapour escape.
Materials for this step:
Samarium Oxide1 79 parts by weightTools needed:
Graphite Powder
Hydraulic Press2
2
Reduce and distil to carbide
Reduce and distil to carbide
Heat the pellets in a vacuum induction furnace to 1700 °C under 0.5 micron or less and hold three hours. Samarium carbide condenses on a graphite condenser (carbon resists the carbon monoxide given off). Only a little oxide and carbon stay behind; they can go back into the next charge.
Tools needed:
Graphite Crucible
Induction Furnace
Vacuum Pump
Graphite Condenser3
3
Distil the metal onto tantalum
Distil the metal onto tantalum
Heat the carbide from the first condenser to 1700 °C under 0.05 micron and hold two hours. Samarium metal condenses on a tantalum condenser: 99.7 % samarium, 0.05 % carbon, 0.10 % oxygen.
Tools needed:
Graphite Crucible
Induction Furnace
Vacuum Pump
Tantalum CondenserMaterials
1- 1 79 parts by weightPlaceholder
Tools Required
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