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Energetics-testin
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Yellow ETN ???
I don't know what I did or what went wrong but when I made my first ETN synthesis, it was a bright yellow granular powder instead of a white powder
My nitric acid is like 80%+( I made it by the sodium bisulfate process)
My sulfuric acid is 98%(bought it)
My erythritol is a mix of erythritol and monk fruit extract
https://www.lakanto.com/products/lakanto-classic-sugar-free-...
my acetone is 100% pure
i nitrated the erythritol for 2hours in an ice bath,then I poured the mix in acetone and it precipitated a low amount of white granular sugar..I took
the acetone mixture and poured it slowly into icecold water..the ETN precipitated out but it was a bright yellow oily liquid instead of being a white
precipitate.
Anyone knows what happened or was it just because of the impurities in the erythritol mix ?
My other batches were perfectly fine(not yellow) and I did the same procedures.
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Tsjerk
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You poured the nitration mix into acetone? Is that a standard procedure?
[Edited on 13-6-2022 by Tsjerk]
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B(a)P
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The residual acid might have made all sorts of things with the acetone.
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katyushaslab
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I have so many questions, but below are the main two.
1. Why not purify the erythritol first? The yellow crap could be nitrated whatever the fuck is mixed in with it. Other polyols, sugars, whatever.
2. Why are you quenching the reaction in acetone? Ice water would be the normal method, then filter, wash with bicarb, and recryst from acetone?
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Herr Haber
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Quote: Originally posted by Tsjerk  | You poured the nitration mix into acetone? Is that a standard procedure?
[Edited on 13-6-2022 by Tsjerk] |
If you are aiming for a Darwin Award yes.
OP seems out of his depth if he cant follow a simple procedure described a thousand times on youtube and in forums.
Edit: Oh well, maybe not so much a Darwin Award. If the nitration mixture was correctly prepared it should be no more than 80% H2SO4 when the reaction
is complete.
[Edited on 13-6-2022 by Herr Haber]
The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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Laboratory of Liptakov
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Novice researchers often have a strong urge to simplify any operation, procedure. I used to be like that also. Fortunately, I survived such seasons.
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite and KC primer (2024)
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Energetics-testin
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| Quote: Originally posted by katyushaslab | I have so many questions, but below are the main two.
1. Why not purify the erythritol first? The yellow crap could be nitrated whatever the fuck is mixed in with it. Other polyols, sugars, whatever.
2. Why are you quenching the reaction in acetone? Ice water would be the normal method, then filter, wash with bicarb, and recryst from acetone?
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1:the erythritol mix cannot be purified i think.Erythritol and the monk fruit extract are stuck together both of them are very soluble in pretty much
all solvants so yeah i just dont know how to separate them
2:The procedure said to do that (nitration mix poured into ice cold acetone or ethanol then precipitated out by adding it to ice cold water
only the first time it turned yellow..i did the same procedure 1 day later and it gave me normal ETN
[Edited on 13-6-2022 by Energetics-testin]
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Energetics-testin
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| Quote: Originally posted by Herr Haber | | Quote: Originally posted by Tsjerk | You poured the nitration mix into acetone? Is that a standard procedure?
[Edited on 13-6-2022 by Tsjerk] |
If you are aiming for a Darwin Award yes.
OP seems out of his depth if he cant follow a simple procedure described a thousand times on youtube and in forums.
Edit: Oh well, maybe not so much a Darwin Award. If the nitration mixture was correctly prepared it should be no more than 80% H2SO4 when the reaction
is complete.
...the nitration mixture was correcly prepared and everything was kept well below 5c..i did this exact procedure 4 times and im still alive and well.
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Herr Haber
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| Quote: Originally posted by Energetics-testin |
...the nitration mixture was correcly prepared and everything was kept well below 5c..i did this exact procedure 4 times and im still alive and well.
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I have no problem with the nitration mixture nor the temperature but with quenching in acetone.
I may not be a trained chemist but at least I think about what I'm doing and what the result will be.
Your improvised Aldol condensation with energetics in the middle shows what seems to me like a distinct lack of thinking otherwise known as cookery.
Can you show us your procedure or it's origin ? Because that is silly as it gets.
No procedure that I know of on this forum is close to being that counterproductive. Nope, not even the guy who didnt understand why adding a mix of
Erythritol and KNO3 to H2SO4 was giving him bad yields...
Procedures on Youtube are the standard nitration, crash in ice, dissolve in acetone.
No procedure in Urbanski is even remotely close to that.
The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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Tsjerk
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Any reference? I'm really interested. It's good practice to reference the procedure when you start a topic anyway.
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katyushaslab
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| Quote: Originally posted by Energetics-testin |
1:the erythritol mix cannot be purified i think.Erythritol and the monk fruit extract are stuck together both of them are very soluble in pretty much
all solvants so yeah i just dont know how to separate them
2:The procedure said to do that (nitration mix poured into ice cold acetone or ethanol then precipitated out by adding it to ice cold water
[Edited on 13-6-2022 by Energetics-testin] |
1. Both probably have different solubilities in some solvent (water, alcohol). A recrystalization will clean it up.
2. What procedure? Link please? That is *not* correct.
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Energetics-testin
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to be honest i didnt follow any specific procedure because I dont have ethanol and I found out that acetone dissolves ETN easily so I used it instead
of ethanol but yeah i didnt follow any real procedure because i didnt find any synthesis that used acetone instead of ethanol.....so i tried it anyway
and im pretty sure its good quality ETN
New synthesis of ETN:3ml RFNA\3ml 96 %H2S04\1.67g Erythritol\8ml Acetone\100ml of distilled water
started by cooling down the nitric acid to the ice bath temperature,Idid the same for the 3ml of H2SO4
when it was all cooled down i added the sulfuric acid to the nitric acid
Ididnt notice a change in temp.
I added the Erythritol by small ammount*25mg*.
At the fourth addition it formed a slushy crystal solution,I continued adding ET to the mix because there was still alot of unreacted acids left.
When started to see that there wasnt much acid left I stopped adding ET.
Once that was done its still looked like a slushy.
I put the small 10 ml beaker in a normal household freezer overnight
12H later
I took out the beaker and placed it in an ice bath.
I took the 8ml of acetone and placed it in the same ice bath as the beaker
30 min later
I took the beaker and started pouring batches of 1ml into the acetone(still in the bath)
The white slushy mix was dissolved and a granular looking sugar precipitated out,The acetone solution turned purple\pink(idk why)
When it turned purplepink i was sure i had fucked up..but i continued anyway.
I took about 20 ml of distilled room temp water and added it to a beaker.
I started adding the acetone to the water.
A precipitate forms and sinks to the bottom.
the precipitate is washed till its white and not yellow.
Separate the water from the precipitate(use any method but dont heat beyond 50c)
the precipitate is placed on a coffee filter and allowed to dry outside for an hour or more( it was 30c outside when i did it)
Once all dried the final yield was 2.36g of good looking,white powder
the white powder should be ETN right ? and if no what is it ?
and no i didnt neutralize the acids,i didnt think it was that important because i used so much water to clean the ETN that I was pretty sure there
werent any trace of acid
[Edited on 13-6-2022 by Energetics-testin]
[Edited on 13-6-2022 by Energetics-testin]
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Energetics-testin
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aright sorry everyone, im dumb..i didnt follow any procedure i just followed what the science madnnes wiki said but i replaced the ethanol by acetone
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Energetics-testin
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I did some small scale testin..does it seems to be ETN ?
first vid is the damage made from 0.03g
the third one is a*open*air* burn test
and the fourth one is a detonation of 0.02g
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[Edited on 13-6-2022 by Energetics-testin]
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Tsjerk
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So you dumped the acid in acetone because it was what you had on hand, you didn't neutralize any acid because you thought it would be fine and you
were left with flame sensitive ETN? Did I get that right?
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Herr Haber
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Uhhh errr.... Well, that'll teach you for trusting the wiki !
Just kidding, I apologize if I seemed to be barking at you earlier but it has been nagging me more and more for some years how people put their lives
at risk trying to be smarter than thousands before them.
If you search the forum you will find many less hazardous procedures. Some work better than others.
Yours seem to be correct up until the last part  By head, it seems you could use
a bit more sulphuric acid. You dont need to keep the reaction in the freezer, you probably would have put the reaction on hold if it wasnt complete by
then. It is usually done 30 minutes after the last addition.
You just should crash the nitration mixture in ice cold water, filter the crude ETN, wash with plenty of water and then only dissolve in acetone
before again crashing in water to which you will have added a bit of baking soda.
The main impurity should be sodium sulfate. Repeat starting from acetone if your products seems weird to you or if you plan for long term storage.
I dont know how or when you plan on neutralizing the acids with your procedure but the reason you do it is to avoid acid inside the cristals that will
end up decomposing your product. Your procedure doesnt seem to do that at all which may be the reason one of your batches came yellow. If your product
smells of anything just recrystallize it as many time as needed.
The product isnt soluble in water so you shouldnt be losing any no matter how many times you need. If done twice correctly it should be stable for
years at room temperature.
The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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Energetics-testin
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| Quote: Originally posted by Tsjerk | So you dumped the acid in acetone because it was what you had on hand, you didn't neutralize any acid because you thought it would be fine and you
were left with flame sensitive ETN? Did I get that right?
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Yeah pretty much..ETN isnt flame sensitive normally ??
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Energetics-testin
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| Quote: Originally posted by Herr Haber | Uhhh errr.... Well, that'll teach you for trusting the wiki
Hahahaha
And yeah my *ETN* smells like laundry
I'll neutralize the rest of what I got left.
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MineMan
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| Quote: Originally posted by Energetics-testin | | Quote: Originally posted by Tsjerk | So you dumped the acid in acetone because it was what you had on hand, you didn't neutralize any acid because you thought it would be fine and you
were left with flame sensitive ETN? Did I get that right?
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Yeah pretty much..ETN isnt flame sensitive normally ??
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Comment of the year. Thank you for this gift
[Edited on 15-6-2022 by MineMan]
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Tsjerk
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You should have a look at the difference between primary and secondary explosives. ETN is a secondary and it should take a bit of effort to make it
detonate.
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Herr Haber
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Fact remains: the procedure on the wiki is incorrect.
The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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Tsjerk
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Yes, but you should also not base the preparation of any compound, definitely not an explosive, on one procedure when many are available.
[Edited on 15-6-2022 by Tsjerk]
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Energetics-testin
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alright alright Ill follow a real procedure next time.
could you link a procedure ?
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Energetics-testin
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| Quote: Originally posted by Tsjerk | Yes, but you should also not base the preparation of any compound, definitely not an explosive, on one procedure when many are available.
[Edited on 15-6-2022 by Tsjerk] |
okay okay sorry i wont make this mistake again
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Tsjerk
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This is one of the best, if not the best, times to use the phrase: UTFSE.
And maybe read the sticky "Life after detonation".
[Edited on 15-6-2022 by Tsjerk]
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