Sciencemadness Discussion Board

Phase Separations

Hexavalent - 14-2-2012 at 13:11

I have nearly finished a synthesis of hydrazine sulfate via the hoffman rearrangement on urea, but, the butanone azine which is formed just will not separate out from the other stuff in the mixture as an organic phase.

At the moment, I just have a faint-yellow turbid mixture . . .anyone have any ideas on how to promote phase separation? I was thinking adding saturated NaCl or even solid NaCl, but I wanted to check before doing it lest I ruin my product.

I am also aware that extraction using toluene and then absorption into the H2SO4 used for hydrolysis also seems to work, but, I have no toluene available.

Help?

Hexavalent - 14-2-2012 at 13:14

I should also point out that I followed the procedure that UnintentionalChaos gives on his YouTube channel, but I used an equivalent amount of household bleach instead of the 12.5% NaOCl that he actually specifies.

UnintentionalChaos - 14-2-2012 at 14:14

Quote: Originally posted by Hexavalent  
I should also point out that I followed the procedure that UnintentionalChaos gives on his YouTube channel, but I used an equivalent amount of household bleach instead of the 12.5% NaOCl that he actually specifies.


What concentration is the bleach? And do you mean equivalent moles or volume...hopefully the former. I would try saturating the solution with NaCl and see where that gets you. The solution already has plenty of NaCl in it...more isn't going to hurt.

Also, please start using the edit feature instead of multiposting.

Also, also, U2Uing me here and sending me a private message on youtube AND posting a comment to my youtube profile with the same question will not make me respond faster.

[Edited on 2-15-12 by UnintentionalChaos]

Hexavalent - 14-2-2012 at 14:32

The bleach says 'less than 5% chlorinated bleaching agent' or something similar. . . .which makes things quite ambiguous. I actually went 'he used just over 12%, so, if I assumed that my bleach was 4%, I need x3 times the volume. Stupid, I know.

Can anyone offer any better suggestions?