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Author: Subject: Erythritol Tetranitrate
Brightthermite
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[*] posted on 18-11-2021 at 18:27


I see in the video you are getting around 50 percent yields with this method. Is that the best you are able to obtain using "The Column"?
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[*] posted on 18-11-2021 at 19:39


I'll watch the video in a bit. Right now I recrystalized my yield and I am astonished to see the dirt that got into my ETN. It is much more powdered than my previous attempt probably because I powdered the stuff before adding it to the mixture.

It will probably be equal to my first yield, but absolutely terrible overall since my first attempt (which went very, very smoothly) ended up with a final yield of 6.5 grams from 5 grams of Erythritol. I will probably end up with 6 grams starting from 15 grams.

I hope with my teflon seals, and the hole I created in my thermometer adapter now sealed again, I hope to get half-decent yields of nitric acid. Even if I need to let them temperature run up very high.

Edit: final yield after recrystalization is 4 grams. There is some mild discoloration as well, which is why I am not going to mix it with my first yield. I think there is something up with it since when I tried to pop some by burning it on aluminum foil and a lighter what happened is some of the stuff dissolved and let off a tiny bit of red fumes. Others popped fine. It isn't 100% worthless, but it's mostly worthless. I'll need to dispose of this batch ultimately.

[Edited on 19-11-2021 by ManyInterests]

[Edited on 19-11-2021 by ManyInterests]
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[*] posted on 19-11-2021 at 12:27


It was only attempt. Maybe is possible obtain 60% from Column device. But 90% sure not.



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[*] posted on 19-11-2021 at 18:55


Well I think my nitric acid situation should be fixed. With the teflon seals my latest attempt yielded 77ml or so of very, very clean acid with a specific gravity of around 1.425. So around 70%. I want to make a few more batches before making maybe one more batch of ETN before I do NHN and RDX. Then I'll consider my chemistry hobby good and solved and move onto another interest... :)

Quote:
It was only attempt. Maybe is possible obtain 60% from Column device. But 90% sure not.


I am not sure if I want to make that specific column, it is an interesting experiment, but I will pass.

Also while writing this comment, I made two batches of nitric acid, one before I quoted you and now this one. I hope it 70%. If it is, then I have enough 68-70% for everything I need. I'll need to get started on WFNA.
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[*] posted on 20-11-2021 at 03:29


HNO3/H2SO4 give always better yields than H2SO4 / nitrate salts for ETN.



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[*] posted on 20-11-2021 at 04:47


Quote:
HNO3/H2SO4 give always better yields than H2SO4 / nitrate salts for ETN.


And much easier and much more efficient. I should have enough HNO3 for my NHN, HDN, and one more ETN synthesis. I will dispose of my last batch since I don't like it. My first batch is still excellent but I will need to pulverize it as It is still a touch grainy. But I am gaining confidence in ETN's stability, so I will powder tiny bits at a time with a rubber spatula.

Edit: my second batch of HNO3 made yesterday appears to have dropped in concentration to around 65%. It's still useable for ETN, I'll need to use a bit more. One thing I learned is that you always must put an excess of sulfuric acid. That's probably why my first batch of that day was much better.

[Edited on 20-11-2021 by ManyInterests]

[Edited on 20-11-2021 by ManyInterests]
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[*] posted on 28-11-2021 at 19:57


As a final note on my latest ETN synthesis. The yield I got was 13 grams after recrystalization and drying. Starting from around 9.9 grams of erythritol. Seems like the slightly less HNO3 concentration didn't affect it that much.

If I have to put a note in, never add any sodium bicarbonate/carbonate into the water when extracting the ETN, it will form a bit of a foam that will make the extraction a bit harder to pull off. I originally thought I did not need to recrystalize this time, but I think it is always a good idea. My yield after the initial extraction was 16.5 grams, but after recrystalizing I got the 13 of very pure ETN.
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