Decaborane , sublimation vacuum

Fig. 10. Apparatus for the sublimation of decaborane. (A) cold finger (B) ground-glass joint for connection to high-vacuum system (C) high-vacuum stopcock ...

Decaborane [J7702-41-9] M 122.2, m 99.7-100 . Purified by vacuum sublimation at 80°/0.1mm, followed by crystn from methylcyclohexane, methylene chloride, or dry olefin-free-n-pentane, the solvent being subsequently removed by storing the crystals in a vacuum desiccator containing CaCl2. 

Decaborane can be satisfactorily purified by sublimation at 65-75° under high vacuum or by recrystallization from heptane. 

All preparations are conducted under an atmosphere of prepurified nitrogen unless specified otherwise. Solvents are vacuum distilled from reservoirs containing appropriate drying agents. Decaborane(14) (See Chapter 5, Section 46) is freshly sublimed prior to use. 

Decaborane (Arfa Product) was sublimated by heating at about 70°C and was intfoduced into the vacuum chamber through a variable leak valve. Boron films were deposited on the heated substrate by thermal decomposition of the decaborane. 

---