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Author: Subject: ETN synth with FeSO4 contaminated AN. Deadly or not?
Weeblordd
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[*] posted on 28-3-2024 at 02:46
ETN synth with FeSO4 contaminated AN. Deadly or not?


Is it safe to synthesize ETN with ammonium nitrate that is contaminated with iron (II) sulfate? Or would it turn out to be more sensitive or would it decompose faster or what can I expect?

Asking because I have some ammonium nitrate that I synthesized from fertilizer grade calcium nitrate and ammonium sulfate (both), I found out its likely that my ammonium sulfate was contaminated with iron (II) sulfate because when dissolved it in water it colors it strongly yellow. Unfortunately recrystallization doesn't help because the iron (II) sulfate crystallizes together with the AN, I think the easiest way to purify it would be to acidify the contaminated ammonium nitrate and distill the resulting nitric acid and then react it with ammonia to produce ammonium nitrate, but that's more expensive than I'd prefer. So I'm thinking of just using this contaminated AN as is for the ETN synth, but I have no clue if its gonna alter ETN's performance in a bad way or not. Can someone help?


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OneEyedPyro
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[*] posted on 28-3-2024 at 04:00


Quote: Originally posted by Weeblordd  
Is it safe to synthesize ETN with ammonium nitrate that is contaminated with iron (II) sulfate? Or would it turn out to be more sensitive or would it decompose faster or what can I expect?

Asking because I have some ammonium nitrate that I synthesized from fertilizer grade calcium nitrate and ammonium sulfate (both), I found out its likely that my ammonium sulfate was contaminated with iron (II) sulfate because when dissolved it in water it colors it strongly yellow. Unfortunately recrystallization doesn't help because the iron (II) sulfate crystallizes together with the AN, I think the easiest way to purify it would be to acidify the contaminated ammonium nitrate and distill the resulting nitric acid and then react it with ammonia to produce ammonium nitrate, but that's more expensive than I'd prefer. So I'm thinking of just using this contaminated AN as is for the ETN synth, but I have no clue if its gonna alter ETN's performance in a bad way or not. Can someone help?




Iron sulfate is a bit soluble in water while ETN effectively is insoluble.
ETN requires at least a single recrystallization to eliminate all acidity which should remove the vast majority of iron impurities. Two dissolve and crash recrystallizations with ethanol, methanol, acetone etc will give nearly 100% pure ETN.

You should be fine with trace impurities in your AN, but I'd try a small batch first.

[Edited on 28-3-2024 by OneEyedPyro]
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Weeblordd
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[*] posted on 28-3-2024 at 04:36


Well ChatGPT tells me iron sulfate enters the crystal lattice of ammonium nitrate as it crystallizes meaning I'll never really be able to get it pure by crystallization alone, and I really hope that iron sulfate won't enter the crystal lattice of ETN.

Still though I suppose ye, considering the amount of solvents you gotta use for ETN I guess it really would eliminate most of the impurities, will do a small batch first
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Trashcanman
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[*] posted on 28-3-2024 at 13:16


Quote: Originally posted by Weeblordd  
Well ChatGPT tells me iron sulfate enters the crystal lattice of ammonium nitrate as it crystallizes meaning I'll never really be able to get it pure by crystallization alone, and I really hope that iron sulfate won't enter the crystal lattice of ETN.

Still though I suppose ye, considering the amount of solvents you gotta use for ETN I guess it really would eliminate most of the impurities, will do a small batch first


ChatGPT has gotten worse between every time that I have used it.
It has the tendency to fuck up every answer related to chemistry and physics.
I wouldn't use it for anything important.

It turned from ChadGPT:cool: to SoyjackGPT:o




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Weeblordd
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[*] posted on 29-3-2024 at 01:40


Yeah tbh that has been my experience with ChatGPT as well xD you really have to double-check that info. Anyway, I hope FeSO4 doesn't contaminate the ETN even after recryst with DH2O and then a second recryst with IPA or acetone and then stabilization with urea or baking soda
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Etanol
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[*] posted on 29-3-2024 at 03:21


Add water ammonia:
FeSO4+2NH3=>Fe(OH)2+(NH4)2SO4
then add Ca(NO3)2:
(NH4)2SO4+Ca(NO3)2=>CASO4+2NH4NO3

Fe(NO3)2 decomposes easily when heated into NOx.
In addition, FeSO4 introduces crystallization water into the mixture. It is FeSO4*7H2O.
However, since the impurity is small and you do not heat the nitration mixture, it is not dangerous.
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fx-991ex
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[*] posted on 29-3-2024 at 05:06


Quote: Originally posted by Etanol  
Add water ammonia:
FeSO4+2NH3=>Fe(OH)2+(NH4)2SO4
then add Ca(NO3)2:
(NH4)2SO4+Ca(NO3)2=>CASO4+2NH4NO3

Fe(NO3)2 decomposes easily when heated into NOx.
In addition, FeSO4 introduces crystallization water into the mixture. It is FeSO4*7H2O.
However, since the impurity is small and you do not heat the nitration mixture, it is not dangerous.


What about heating the AN for crystallization/drying, any danger?
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Weeblordd
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[*] posted on 30-3-2024 at 10:12


That's a lifesaver thank you. Will try doing that when I get the chance if I find out the FeSO4 impurity doesn't satisfy the results I get. And I don't think heating the FeSO4 contaminated AN for crystallization and drying poses any danger
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