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Author: Subject: ammonium nitrate from cold packs trouble
ManyInterests
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[*] posted on 1-7-2022 at 23:35


Quote:
Likely the best way to obtain higher purity AN is to get CAN and ammonium sulfate.


I'll keep that in mind. Because I will need a little ammonium nitrate for a few things.

At any rate, I am purifying my chlorates, and it seems that something went wrong with my synth. Because i am nowhere near purity. In fact, out of the remaining 405 grams of chlorates that I had left from my thermal composition exercises... turns out that I have over a hundred grams of chloride. I don't know how much since I am drying the left over salt and I am boiling off the methanol I used for the purification.

Like holy shit. I had no idea how little chlorate I actually made. Something is up with my electrolysis.
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[*] posted on 24-1-2023 at 21:42


I decided to resurrect this thread since I am having similar problems with nitrate synthesis but for entirely different reasons:

Firstly I am using this brand of calcium-ammonium nitrate as a starter.

http://www.formedica.com/en/hot-cold-compresses/instant-cold...

In the past I've used this brand extensively to make potassium nitrate, and to a large extent, it produces a working product and I've used it to make good nitric acid and other applications where potassium nitrate is needed (it is not 100% pure and isn't super fast burning, but I never found that to be a problem). I wish I knew what to do to get the purest possible product.

Now remember those cold packs that I opened the thread with? The primacare? I used them to make sodium nitrate, and while that sodium nitrate is far form perfect, it worked for almost everything as well, from picric acid synthesis to making nitric acid (I even made nitric acid with a specific gravity of 1.51, so WFNA or near it).

But when I switched to the formedica brand, I applied the same process as the primacare but I got different results. The burn rate for the sodium nitrate was a snail's pace, and while it did work for nitric acid, I feared that the product is not pure enough for use on its own where I just need sodium nitrate, like picric acid synthesis and such.

I followed Canadian Chemist's process for making sodium nitrate using calcium ammonium nitrate (after filtering out the impurities) and mixing in sodium bicarbonate.

I decided to try something different. I feared I was using too much sodium bicarbonate, so what I did is I weighted out 553.1 grams of CAN from cold packs, filtered out the insolubles, evaporated off all the water, and I ended up with around 418.28 grams of dry CAN, then I added 1.054x that amount in sodium bicarbonate to it (I was using a vast excess of water) and I boiled it. It seemed to work. It was producing a lot of ammonia gas and I boiled it until it reached a super saturation point (the beaker was bumping violently, so I stopped the heating and it cool) then I placed the entire amount in the oven for it to dry overnight and now I've ground up all the chunks into fine bits, dried it some more, then ground it up again (there is still a lot of moisture) and made it a fine powder and it is in the oven again.

I did do a burn test, but I didn't get much in terms of results, but those are the crude chunks that wouldn't grind down, so I guess I shouldn't expect much. I pray that the sodium nitrate I have in the final dry will work. If not, I will dissolve them all again in water and add a little more sodium bicarbonate. Maybe I didn't add enough for everything to react together?

I used a 1:1 ratio of nitrate and granulated sugar for the burn test. it was REALLY slow.

As for some notes: I did get ammonium nitrate cold packs from the US, so I should have some real ammonium nitrate after I filter those and dry them properly. I also did obtain a pound of ammonium sulfate, so I can do the synthesis of ammonium nitrate via CAN and ammonium sulfate.

Can anyone give me the stoichiometric amounts?
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[*] posted on 25-1-2023 at 13:59


Quote: Originally posted by ManyInterests  

Can anyone give me the stoichiometric amounts?

Nope. But i can help you work it out.
Do you have a set of equations for your procedure yet?
Get those and will balance everything and cross reference some literature

Here are some relevant links
http://www.sciencemadness.org/talk/viewthread.php?tid=159262...
http://www.sciencemadness.org/talk/viewthread.php?tid=59080#...
Looks like you been stuck on this for a while. Will get you sorted.

Have you tried thermal decomposition?
Pnta but will produce NOx that can be turned into HNO3 and you can use that to make any salt you need




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[*] posted on 25-1-2023 at 17:37


Thanks, I am looking into those now.

for my sodium nitrate, my latest synthesis is a lot more successful than previous one. Better burn rate with visible golden flames. It should work for all that I need, but I would like a better handle on it for obvious reasons. One of the first things I made was potassium nitrate and that was actually quite successful, though it didn't burn at the same speed at commercially available potassium nitrate (which I cannot obtain in Canada, sadly).

Edit: Wow, those methods for gauging whether it is calcium nitrate, calcium-ammonium nitrate, and how much ammonium nitrate there might be in sound really fascinating, I will definitely be working on those soon.

[Edited on 26-1-2023 by ManyInterests]
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