zephler1 - 7-10-2014 at 09:26
Generating BH3•THF via NaBH4 + BF3•THF is a well known process; however, any references that I have read do not describe the glassware setup for
such an operation. Assuming a 3 neck round bottom is used, one neck for thermometer, on with a suba seal which is penetrated by a syringe tip to have
a low stream of Ar going through the system, and a reflux column in the remaining neck, how does one handle the toxic and pyrophoric gas coming out
the top of the reflux column?
One idea that comes to mind is to have a hose attached to the top of the condenser which passes through a bubbler of mineral oil, and then into a
beaker of water to kill off BH3 (B2H6) - what do ha think?
Dan Vizine - 7-10-2014 at 20:49
When Dupont needed to scavenge boranes, they bubbled effluents through ammonia in their Niagara Falls plant.
Brain&Force - 7-10-2014 at 21:19
Yes, ammonia, or any other Lewis acid, will form an adduct with diborane.
DJF90 - 7-10-2014 at 22:53
You'll likely be doing the reaction in THF, which forms an adduct with the BH3 as produced. Special precautions were not needed when I've done this
before, but do be cafeful with the quench post reaction (very vigorous reaction with large gas evolution). Other than that you ought to be fine so
long as you're not sniffin it...