OneEyedPyro
Hazard to Others
Posts: 280
Registered: 7-10-2015
Member Is Offline
Mood: No Mood
|
|
PETN purification
I recently got my hands on some pentaerythritol and decided to give PETN synthesis a shot.
Long story short due to a silly miscalculation I ended up with about 25 grams of what was clearly in an under nitrated product, a simple
recrystallization from acetone didn't help.
I was wondering if there are any solubility exploits I could use to remove the lower nitrates, I've of course considered nitrating it again but was
just curious about the solubility of the various nitrates of PE. I did some digging through patents and such but found practically no mention of the
lower nitrates.
[Edited on 7-4-2016 by OneEyedPyro]
|
|
hissingnoise
International Hazard
Posts: 3940
Registered: 26-12-2002
Member Is Offline
Mood: Pulverulescent!
|
|
Quote: | Long story short due to a silly miscalculation I ended up with about 25 grams of what was clearly in an under nitrated product
|
Why do you think it's under-nitrated?
The lower nitrates are easily soluble, afaik!
|
|
OneEyedPyro
Hazard to Others
Posts: 280
Registered: 7-10-2015
Member Is Offline
Mood: No Mood
|
|
It appears to be very weakly soluble if not insoluble in water yet soluble in acetone while PE should be insoluble in acetone yet weakly soluble in
water.
A hammer test gave no reaction after about a dozen solid strikes and it burned without too much vigor, I haven't actually tried detonating it via
primary but I'm fairly confident it's under nitrated.
I added a bit too much PE and didn't catch the mistake until looking back at my notes, I guess basic math is too much for me
[Edited on 7-4-2016 by OneEyedPyro]
|
|
hissingnoise
International Hazard
Posts: 3940
Registered: 26-12-2002
Member Is Offline
Mood: Pulverulescent!
|
|
The hammer-test can be very hit-and-miss if you don't tape the explosive, alufoil wrapped, to the face of the hammer . . . ?
And the blow should be of iron against iron!
|
|
OneEyedPyro
Hazard to Others
Posts: 280
Registered: 7-10-2015
Member Is Offline
Mood: No Mood
|
|
I tried your suggestion for the hammer test and it worked after a few sharp blows.
PETN appears to be much less shock sensitive than I had expected, I suppose being a rather fine powder that should be no surprise.
Thanks for the help.
|
|
hissingnoise
International Hazard
Posts: 3940
Registered: 26-12-2002
Member Is Offline
Mood: Pulverulescent!
|
|
You're welcome ─ and BTW, distilling your acid will give higher yields and a cleaner product than nitration by salt/acid mixtures . . . ?
|
|
OneEyedPyro
Hazard to Others
Posts: 280
Registered: 7-10-2015
Member Is Offline
Mood: No Mood
|
|
I'm in need of some labware so it's acid/salt nitrations for now.
I'm thinking about picking up some of the basics (hot/stir plate, distillation setup) from Elemental Scientific since they are owned by a fellow
sciencemadness member and I'm only a couple hours drive from them.
|
|
hissingnoise
International Hazard
Posts: 3940
Registered: 26-12-2002
Member Is Offline
Mood: Pulverulescent!
|
|
Maybe you might ask this member (whoever he is?) why the site of a science company based in Nebraska has itself a German language version . . . ?
|
|
OneEyedPyro
Hazard to Others
Posts: 280
Registered: 7-10-2015
Member Is Offline
Mood: No Mood
|
|
tomholm is the member that owns the company and they're based in Minnesota.
No idea why they have a German version.
|
|
tomholm
Owner of BME Lab and Science and Elemental Scientific
Posts: 187
Registered: 24-2-2014
Location: United States
Member Is Offline
Mood: Good
|
|
German version
We are www.elementalscientific.net .
there is another company based in Omaha with the web site elementalscientific.com . I assume they are the ones with the German version. They may do
a lot of business there.
|
|