geffmov - 25-12-2019 at 12:51
Hi all. I recently synthesised nitric acid by a well known method of using CAN (calcium ammonium nitrate) and stoic conc. sulfuric acid with added
water to calculate aftwr an initial forerun of dilute hn03 distillate 100-121c a 68% azeotrope of hn03 distills off.
The reaction went mostly as anticipated. Almost no nitrous orange gas/vapour was produced during the reaction. What little did the dilute hydrogen
peroxide gas trap dealt with. That was an endothermic reaction.
In reflection of the method i found the distillation agonisingly slow and wanted to speed things up a little. One of my errors may of been using a
spiral coil condensor instead of straightbore leibig?
My main query is this. Can i use an external steam source and by forcing steam through @125c collect the distillate much quicker? Is there any
inherent risks if i adapt the procedure this way?
I planned this time to use a 5l 2neck 24/29 flask one neck has the 2.5KW external steam source with heat controller to be 125c on entering the 5l
flask with a 500mm straightbore leibig running into a 3l receiver and piped off too the dilute hydrogen peroxide gastrap.
I was then going to redistill the distillate to give me 68% hn03.
Ive had good success in the past using an external steam source and collecting various oils much quicker than straight distillation. Im hoping the
same will apply here but i can find no references or examples of this been done. Id just like someone to confirm theres no hidden risks, and im open
to suggestions of alternative adaptations if anyone thinks of a more convenient way?
geoff