zeroberts - 6-10-2015 at 19:37
Hi all-
First off: brief introduction. I'm a hobby pyrotechnician from Minnesota. I started into fireworks about six years ago. I've worked with a number of
compositions and accrued innumerable hours of well earned experience over these years. The finer points of toxic and hazardous chemicals, and working
with a 0.00 margin of error are old friends by now. But like many fun seekers I feel the need to graduate into bigger bangs. I've been lurking here
for some time and it's time I show my face.
So. ETN is where I've chosen to launch my foray. In short, the problem I've encountered is this: in using a mixed acid nitration process; while adding
erythritol I find that there is no "slurry" action. There is a cloudiness while adding and stirring, and some apparent crystal formation thereafter
but the mix soon turns clear. I've spent hours researching procedure after procedure, and have followed procedure with excellence. I'm left to believe
something is amiss chemically.
Your garden variety pyrotechnic compositions (while some in practice prove just as deadly if not handled with extreme care) lack the subtle
complexities of this process. So I come seeking wisdom haha. Based on information provided: can anybody steer me towards my solution?
Hawkguy - 6-10-2015 at 21:25
Just add water
zeroberts - 6-10-2015 at 21:43
How much then
Also please tell me that isn't a joke playing off the word "solution"
[Edited on 7-10-2015 by zeroberts]
Metacelsus - 7-10-2015 at 07:05
I think what he means is to pour the solution into water; the ETN should precipitate.
zeroberts - 7-10-2015 at 19:18
I have observed no precipitate.
Also: titration tests of my nitric acid result about 66%. Fuming nitric acid has the advantage of simplicity and even convenience in synthesis,
however I'm having difficulty discerning any clear answers on the employment of fuming nitric acid in the nitration process; specifically concerning
Erythritol.
I hate to sound ignorant, but I moreso hate to remain ignorant haha. Any and all guidance is graciously welcome.
Bert - 7-10-2015 at 19:37
Google this string:
"sciencemadness.org ETN synthesis"
Read for several days, possibly for several WEEKS, depending on how much free time you have for this.
zeroberts - 7-10-2015 at 20:41
I'll dip my quill and put my nose In the books then. I seem to operate at 10:1 for "research:lab" when I'm sliding down the learning curve, and I've
run out my clock in the lab anyway. Thanks!
hyfalcon - 8-10-2015 at 02:19
Bert, the search string is site:sciencemadness.org etn synthesis
OneEyedPyro - 8-10-2015 at 04:21
Well clearly you're not reaching full nitration as the mono, di and trinitrates are soluble in water.
You need to give a bit more detail regarding your synthesis ratios, purity of chemicals, your procedure etc for anyone to really help you.
My advice is to use AN or NaNO₃ in place of HNO₃ and use a slight excess of nitrate salt/H₂SO₄ to ensure full nitration.
Also, I get good yields by running it at 20C for about 2 hours, be sure to stir it regularly once things start to thicken up to avoid hot spots and a
potential runaway.
hyfalcon - 8-10-2015 at 06:05
READ:
http://www.sciencemadness.org/talk/viewthread.php?tid=20638
Bot0nist - 8-10-2015 at 07:45
A good read, hyfalcon.
I like this write up, as well.
http://www.sciencemadness.org/talk/viewthread.php?tid=7209
This .pdf file, to be exact.
[Edited on 8-10-2015 by Bot0nist]
zeroberts - 9-10-2015 at 19:51
Returning to report a resounding success this time.
I was turning circles reviewing my procedure and materials. Over the years I've maintained a personal policy of adhering strictly to a written
procedure to ensure quality and prevent deviations or omissions. My ETN and HNO3 procedures are two separate cards and I was not reviewing the latter
for errors. After much reading I turned to my HNO3 procedure to root out a computational error I realized I had made.
Tonight I started from square one with revised procedures, and ran a flawless preparation. Every step yielded desired results as prescribed.
Temperature was steady and under control, consistency was manageable, and the process was completed to my satisfaction. Points awarded to the
community for being a useful resource.
OneEyedPyro - 10-10-2015 at 03:29
That's great to hear!
So what was the computational error?
Erythritol nitration can be kind of a pain in the ass, it seems reaching trinitrate is easy but that last nitro group is the hardest to put on and
your acids will be at their weakest towards the end of the nitration, things start to get thick and the material being nitrated is no longer in such
intimate contact with the acids which results in that last nitro group having an even harder time bonding, that's why I like working with a slight
excess of acids and running it at a bit higher than usual temps.
zeroberts - 10-10-2015 at 08:07
I'm actually embarrassed to admit it; but a simple in-flight error while writing my procedure left a drastic offset in my calculation of concentration
which resulted in inadequate nitric acid.