Preparation
The vacuum-sealed ampoules with the starting materials are broken by vigorous shaking in an evacuated 5-liter flask closed by a ground glass stopper with a stopcock. To complete the deuterolysis, the mixture is left standing in the dark for two days, with occasional shaking. The reaction should not be accelerated by heating or disproportionation (4 D3PO3 = 3 D3P04 + PD3) will occur, and the DBr will be contaminated with PD3. After sealing the flask to a high vacuum system, the impure gas is condensed in a receiver cooled with liquid nitrogen and purified by fractional distillation, using a low-temperature distillation flask.only half of the deuterium feed is converted to desired products.
