November 25, 2024, 10:33:55 AM
Forum Rules: Read This Before Posting


Topic: Can you make fuming nitric acid from 65% HNO3 and conc. sulphuric?  (Read 4218 times)

0 Members and 2 Guests are viewing this topic.

Offline zuriel

  • Full Member
  • ****
  • Posts: 107
  • Mole Snacks: +2/-1
Hi Folks,

I want to do a nitration but have no fuming nitric at the moment. Someone told me that if I mix equal volumes of nitric 65% and conc. sulphuric that it should do the job but I'm a bit sceptical. I can get more fuming soon but don't want to wait the while.

Can anyone offer any advice?

Thanks!

Offline phth

  • Chemist
  • Full Member
  • *
  • Posts: 528
  • Mole Snacks: +39/-4
Re: Can you make fuming nitric acid from 65% HNO3 and conc. sulphuric?
« Reply #1 on: January 28, 2015, 01:29:47 PM »
boiling point should should work unless you chose an azeotropic mixture.  How can you extract nitric acid from a azeotropic mixture?

Offline zuriel

  • Full Member
  • ****
  • Posts: 107
  • Mole Snacks: +2/-1
Re: Can you make fuming nitric acid from 65% HNO3 and conc. sulphuric?
« Reply #2 on: January 28, 2015, 01:31:44 PM »
Sorry phth I'm not sure I understand your suggestion.

Offline TheUnassuming

  • Chemist
  • Full Member
  • *
  • Posts: 461
  • Mole Snacks: +48/-1
Re: Can you make fuming nitric acid from 65% HNO3 and conc. sulphuric?
« Reply #3 on: January 28, 2015, 02:59:44 PM »
Not sure of your substrate, but its a standard for undergrad o-chem labs to use HNO3 and H2SO4 to nitrate a benzyl ring.  Check out the wiki page on nitration for links to orgsyn papers that will give you a good starting point.
When in doubt, avoid the Stille coupling.

Offline zuriel

  • Full Member
  • ****
  • Posts: 107
  • Mole Snacks: +2/-1
Re: Can you make fuming nitric acid from 65% HNO3 and conc. sulphuric?
« Reply #4 on: January 28, 2015, 03:25:19 PM »
Thanks for the tip!  :)

Offline phth

  • Chemist
  • Full Member
  • *
  • Posts: 528
  • Mole Snacks: +39/-4
Re: Can you make fuming nitric acid from 65% HNO3 and conc. sulphuric?
« Reply #5 on: January 28, 2015, 03:34:13 PM »
I am saying that HNO3 is the lowest boiling point.  Therefore it can be distilled to purify, and furthermore titrated.  IF you're serious about being a chemist you have to teach yourself about azeotropic distillations, the sooner the better.

Offline zuriel

  • Full Member
  • ****
  • Posts: 107
  • Mole Snacks: +2/-1
Re: Can you make fuming nitric acid from 65% HNO3 and conc. sulphuric?
« Reply #6 on: January 28, 2015, 07:45:20 PM »
I'm going to try the method that employs 1:1 mix of 65% nitric and conc. sulphuric for now at least.

I'd be interested in synthesising a poly nitrated phenyl acetic acid too (both meta and para positions) and I found a really old journal that makes it by just refluxing phenyl acetic acid in fuming nitric - I wonder would this work for the sulphuric/nitric mix.

Azeotropic distillation - although it seems a viable option - is totally impractical to me for now. Plus I still have MANY years to go before I'd ever consider myself a very serious chemist lol.

Thanks all for answers/suggestions.

Sponsored Links