Sciencemadness Discussion Board - Yellow ETN ???

Yellow ETN ???

Energetics-testin - 12-6-2022 at 14:42

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.

Tsjerk - 13-6-2022 at 00:50

You poured the nitration mix into acetone? Is that a standard procedure?

[Edited on 13-6-2022 by Tsjerk]

B(a)P - 13-6-2022 at 01:38

The residual acid might have made all sorts of things with the acetone.

katyushaslab - 13-6-2022 at 04:44

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?

Herr Haber - 13-6-2022 at 06:37

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]

Laboratory of Liptakov - 13-6-2022 at 07:26

Novice researchers often have a strong urge to simplify any operation, procedure. I used to be like that also. Fortunately, I survived such seasons.

Energetics-testin - 13-6-2022 at 08:50

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?

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]

286411531_557402995931984_407478449163859463_n.jpg - 20kB

Energetics-testin - 13-6-2022 at 09:15

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]

Herr Haber - 13-6-2022 at 11:34

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.

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.

Quote: Originally posted by Energetics-testin

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

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.

Tsjerk - 13-6-2022 at 11:56

Quote: Originally posted by Energetics-testin

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

Any reference? I'm really interested. It's good practice to reference the procedure when you start a topic anyway.

katyushaslab - 13-6-2022 at 12:58

Quote: Originally posted 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.

Energetics-testin - 13-6-2022 at 14:11

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]

Energetics-testin - 13-6-2022 at 14:25

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 - 13-6-2022 at 15:17

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]

Tsjerk - 14-6-2022 at 07:27

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?

Herr Haber - 14-6-2022 at 08:11

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.

Energetics-testin - 14-6-2022 at 10:40

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?

Yeah pretty much..ETN isnt flame sensitive normally ??

Energetics-testin - 14-6-2022 at 11:08

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.

MineMan - 14-6-2022 at 23:45

Quote: Originally posted by Energetics-testin

Quote: Originally posted by Tsjerk

Yeah pretty much..ETN isnt flame sensitive normally ??

Comment of the year. Thank you for this gift

[Edited on 15-6-2022 by MineMan]

Tsjerk - 15-6-2022 at 01:34

Quote: Originally posted by Energetics-testin

Yeah pretty much..ETN isnt flame sensitive normally ??

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.

Herr Haber - 15-6-2022 at 03:57

Fact remains: the procedure on the wiki is incorrect.

Tsjerk - 15-6-2022 at 05:02

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]

Energetics-testin - 15-6-2022 at 07:34

Quote: Originally posted by Herr Haber

Fact remains: the procedure on the wiki is incorrect.

alright alright Ill follow a real procedure next time.

could you link a procedure ?

Energetics-testin - 15-6-2022 at 07:42

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

Tsjerk - 15-6-2022 at 08:37

Quote: Originally posted by Energetics-testin

could you link a procedure ?

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]

Energetics-testin - 15-6-2022 at 11:08

ur useless dude

and ive read it many time dont worry.

Herr Haber - 15-6-2022 at 11:56

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]

Words of wisdom there !

Additionally, reading / viewing different sources (for any synth) will give a better understanding of the reaction you are trying to carry which will in turn allow you to adapt it to your setting and available reagents.
This saves time, money, efforts and maybe limbs.

It might even make you curious and try different conditions for your synth just to see what happens... I dont recommend that with energetics obviously. Once you start experimenting, taking notes and trying to refine a procedure to achieve a specific goal after you have gained enough understanding then I guess you're on the right track to call that science

@OP: Tsjerk is a nice guy. Also, you should wear gloves when playing with acids (yellow skin, fun). You'll find other threads in the forum with all the information someone who apparently managed to distill some acid would need to conduct that synth in a safer way.

Energetics-testin - 15-6-2022 at 13:24

Ok ok thx for the knowledge

I did and yall slapped me on my hands

i tried to make another way to synthesize ETN and the feedback i got was that im stupid.

Ive been doing amateur chemistry for about 4 years and ive always taken notes and tried new procedures and new ways of making a compound.

And for the acid my gloves were all made of latex so i just did it barehand.I bought other gloves since then

XeonTheMGPony - 15-6-2022 at 15:53

Take a few nice deep breaths with eyes closed, do it slowly, relax, Now that we're relaxed and eyes rested, mix up a tasty beverage, Now lets start with a look through other pages here in energetics, lets see what we find.

Now that we did that and found a few massive threads dedicated to this one topic lets spend some time reading every thing!

With energetics, if some thing goes wrong you will be lucky to just come out maimed a bit, it is very un forgiving even for those who do it professionally, there is a reason we harp on about the trivial safety infractions as they can add up to a free trip to the morgue or worse. Oh yes, forgot to mention there are worse things then death!

Now if you relax a bit, take it all in good trust and plod through the bumps in the ride you'll find a darth of knowledge on here that will meet with what you have on hand to a procedure that will yield good results easier with minimal risk!

B(a)P - 15-6-2022 at 16:01

Before you try to invent a new procedure, it is a good idea to perfect existing ones that are known to work. This helps you to understand the reaction conditions and what you can expect from your product, ie its properties. If you had done this you would already know that ETN is flame sensitive and you could compare your notes from your previous experimentation to your observation of the product you made with this modified procedure. It is impossible to know if you have achieved the result you are after if you don't know how the end product behaves.
No one is slapping you on the hands, they are giving you sound advice. They have taken the time to post on this thread after you asked for advice. You might not be getting the answers you want, but that is because the people reading your post know how unforgiving energetics can be.
It is great that you have found a hobby that you enjoy in amateur chemistry. Please don't feel discouraged with the reaction that you have received from your post. Rather, for future posts put a little more thought and care into them and they will be better received. My two cents worth: avoid using abbreviated words like 'thx', when you post a question show that you have done some research to try to get to the answer yourself already and avoid emotive posts.
I will leave this here to give an indication of the flame sensitivity of ETN others have experienced.
http://www.sciencemadness.org/talk/viewthread.php?tid=16612
I would be very curious to hear if, through your testing, you think there is a difference between the crude product that made (the one in your videos) and the recrystallised product.
Have fun and stay safe!

Edit - Well put Xeon, I wouldn't have posted if I had seen yours first.

[Edited on 16-6-2022 by B(a)P]

Energetics-testin - 15-6-2022 at 22:20

Quote: Originally posted by XeonTheMGPony

Take a few nice deep breaths with eyes closed, do it slowly, relax, Now that we're relaxed and eyes rested, mix up a tasty beverage, Now lets start with a look through other pages here in energetics, lets see what we find.

Now that we did that and found a few massive threads dedicated to this one topic lets spend some time reading every thing!

With energetics, if some thing goes wrong you will be lucky to just come out maimed a bit, it is very un forgiving even for those who do it professionally, there is a reason we harp on about the trivial safety infractions as they can add up to a free trip to the morgue or worse. Oh yes, forgot to mention there are worse things then death!

Now if you relax a bit, take it all in good trust and plod through the bumps in the ride you'll find a darth of knowledge on here that will meet with what you have on hand to a procedure that will yield good results easier with minimal risk!

Sorry

I'll be better

Energetics-testin - 15-6-2022 at 22:51

Quote: Originally posted by B(a)P

I would be very curious to hear if, through your testing, you think there is a difference between the crude product that made (the one in your videos) and the recrystallised product.
Have fun and stay safe!

Edit - Well put Xeon, I wouldn't have posted if I had seen yours first.

[Edited on 16-6-2022 by B(a)P]

I will,thank you for your wisdom and im sorry.

After reading a bit of the *life after detonation*&*ETN:almost killed myself*..... I think IWill go back to *normal* chemistry and leave the energetic world for a while,i dont have enough knowledge yet to be working with energetics.

And sorry im french,my English is not that good.

[Edited on 16-6-2022 by Energetics-testin]

ManyInterests - 17-6-2022 at 13:43

I've just looked through this thread. I was going to repost my steps in how I made ETN and then recrystalized it, but I will post a link to Darian Ballard's videos on the matter that I used to great effect.

https://www.bitchute.com/video/78uQsxtKK3rE/

The above video is the initial synthesis of ETN.

https://www.bitchute.com/video/sPXzSrbiW7aO/

The above is the recrystalization. You only do the recrystalization AFTER you have removed the ETN from the acid mixture AND cleaned it of all the acids.

ETN is 100% insoluble in water, you can't dissolve it in that no matter how hard you try.

Energetics-testin - 19-6-2022 at 14:02

Quote: Originally posted by ManyInterests

I've just looked through this thread. I was going to repost my steps in how I made ETN and then recrystalized it, but I will post a link to Darian Ballard's videos on the matter that I used to great effect.

https://www.bitchute.com/video/78uQsxtKK3rE/

The above video is the initial synthesis of ETN.

https://www.bitchute.com/video/sPXzSrbiW7aO/

The above is the recrystalization. You only do the recrystalization AFTER you have removed the ETN from the acid mixture AND cleaned it of all the acids.

ETN is 100% insoluble in water, you can't dissolve it in that no matter how hard you try.

Thank you for sharing the links and your knowledge.

OneEyedPyro - 25-7-2022 at 00:20

Maybe I read this incorrectly, I didn't bother to read all the responses... But for the love of God tell me you aren't implying that you crashed the nitration mixture straight into acetone

You crash the nitration mixture into 10 times the volume of cold water, filter off the ETN that precipitates, dry it out, add the dry ETN to a suitable solvent that has been pre heated preferably in a metal container in a water bath to no more than 60C, dissolve as much as you can and crash that into cold water while rapidly stirring said water.

Seriously, I hope I read that one wrong lol.

ManyInterests - 25-7-2022 at 09:31

Quote: Originally posted by OneEyedPyro

Maybe I read this incorrectly, I didn't bother to read all the responses... But for the love of God tell me you aren't implying that you crashed the nitration mixture straight into acetone

That's what basically what he did. I find it weird. The process for making ETN is documented in both text and video (look at my previous post on this thread). In another thread there was someone (who I posted my process of making ETN, based on Darian Ballard's video) who failed to make ETN because he put his erythritol in sulfuric acid first, which I am certain destroyed it, before he added his nitrates. I gave a full step-by-step process of how I did it there. I should pull up that response.

Energetics-testin - 25-7-2022 at 13:58

Quote: Originally posted by OneEyedPyro

Maybe I read this incorrectly, I didn't bother to read all the responses... But for the love of God tell me you aren't implying that you crashed the nitration mixture straight into acetone

.[/rquote/

I did and I explain exactly what I did in the first page of this thread.

I was dumb and had no real knowledge about nitration.

OneEyedPyro - 25-7-2022 at 14:28

Quote: Originally posted by Energetics-testin

I did and I explain exactly what I did in the first page of this thread.

I was dumb and had no real knowledge about nitration.

Well, for future reference don't add a mixture of a strong oxidizing compound, a strong dehydrating compound and a powerful high explosive to a highly volatile and flammable solvent that's easily oxidized and dehydrated lol.

That is honestly up there with some of the crazier stuff I've seen on this forum in a while.
All that said, I'm glad you didn't have a bad accident and it's good that you came here for advice. Not judging you for not knowing, it's just really silly for me to think about.

Energetics-testin - 27-7-2022 at 11:37

Now I know..hahaha

Yeah im glad I didnt have an accident.

After learning a lil bit about nitration and chemistry in general..Im embarassed by my post hahahaha

And sorry my bad English