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Author: Subject: ETN synthesis problem
Laboratory of Liptakov
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[*] posted on 12-10-2016 at 03:59


My preparation was this: Cool acids on zero. And partially added, for example 1g Er. every 3 minute. And hold temperature between +3 to +5 Celsius. Thus for 10g Er. 10x by 1g Er. After adding 10g is possible instantly or slowly increase temperature on +15 C. And continual stir mixing still 15 minutes. Yield should be 20g ETN +. Dr.



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[*] posted on 12-10-2016 at 04:30


@Laboratory of Liptakov:
Thanks a lot for your feedback. Did you get that yield using 96% H2SO4 and 65% HNO3 or using 98% H2SO4 and higly concentrated HNO3?
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[*] posted on 12-10-2016 at 12:35


H2SO4 96% and HNO3 65 %. Normal concentrations for classic nitration or esterification process.



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[*] posted on 17-10-2016 at 04:51


That's great thank you.
I was wondering, what if one wants to make very small batches of ETN? The quantities I posted before (4ml 65% HNO3, 6ml 96% H2SO4, 1g Erythritol) would lead to about 3 grams of ETN which is a huge amount in my opinion, considering only 1 or 2 grams are needed to detonate very large amount of let's say ammonal.
For example if you wanted to make only 300 mg ETN how would you operate? You could scale down the quantities but it would be very impractical to work with less than 1 ml of solution.
Do you think would be a good idea to just scale down the Erythritol amount to let's say 100 mg and keep the same amount of acid (4ml 65% HNO3 and 6ml 96 % H2SO4) in order to obtain only about 300 mg ETN? Or maybe too much acids for that little dose of Erythritol would cause problems?
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[*] posted on 19-10-2016 at 13:47


No one knows the answer?
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[*] posted on 19-10-2016 at 15:15


It's not "very impractical to work with less than 1 mL." The scale of 10 µL is where it gets difficult. However, making 300 mg ETN isn't any harder than making 3000 mg.



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[*] posted on 19-10-2016 at 18:57


Given a good grasp of technique, sub gram quantities are not too hard. If you are at all sloppy, inexperienced or just under equipped, you do risk throwing a large % of baby out with the bath water, of course. See member Microtek, past master of the tiny scale EM synthesis and device implementation.

One may want to consider: Is the chance of experiencing a personally dangerous outcome more a function of number of times an opporation is repeated, or of the size of the batch being run??? I do not have a hard, definitive answer, but do know that if an operation is repeated enough times, anything that CAN go wrong, DOES.

Is it statistically more dangerous to make 300mg 10 times, or 3g once? 300mg detonated in close enough proximity will still fill your face with glass particles or remove some fingers. 3 grams, all of that plus bothering the neighbors.




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[*] posted on 21-10-2016 at 01:01


I'm sorry, I should have said it is very impractical FOR ME, since I don't have the proper equipment nor the experience required to work with very tiny batches.

Bert, your statement is very sound and I agree with you about the greater risk of accident relative to the making of 300mg for 10 times instead of 3g for 1 time. But accidents must always be expected and accepted in my opinion: I always force myself to work in a manner that guarantees I won't get permanently hurt even if an accident does occur, at any point during the process. When making a few hundreds mg that is fairly possible if very good body and hearing protections are used and proper distance between the explosive and the hand (at least 10cm) is always kept during the whole process. When working with some grams instead, the required protections and distances would be way more severe, so the process would be much harder to fulfill. That's why I prefer making small batches many times expecting detonation anytime than big batches a few times supposing they won't detonate, I think that's what makes a difference between a long and satisfying career and a short one...

So if I wanted to work with smaller batches would you advise me to just scale down all the three ingredients (erythritol, HNO3 and H2SO4) or is it possible to just scale down the erythritol quantity? An higher ratio of acid mixture and erythritol would be a problem in your opinion?
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[*] posted on 21-10-2016 at 08:26


Following proper procedures and using good reagents, and care full monitoring of temps there is very little risk! Careless and sloppy work will increase the risks.

Ironically working with smaller reaction masses increase the risk, as temps can change very fast in a less controllable fashion, with a larger reaction mass you have the benefit of thermal mass to buffer reaction temps.

So I say practice with 3g amounts, and plane your experiments out care fully in advance make sure to have a good thermometer, clean glass wear, and bicarb water, and a wet sponge with it (Clean up any spilled acids on your self or the work surfaces).

There is no such thing as a dangerous substance, just dangerous people!

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[*] posted on 28-10-2016 at 06:01


Thank you, you definitely have a point, I didn't consider that reaction's inertia, which decreases with reagents masses, could cause problems by producing sudden changes of parameters such as temperature.

I have some questions about the neutralization step which has to be done right after the powder is filtered:
- Is it possible to not noticing any fizzing when ETN is washed with sodium bicarbonate solution? (maybe because it was previously washed with a plentiful amount of water)
- What if ETN is continued to be washed with sodium bicarbonate solution for a long time after the fizzing has stopped? Can it be detrimental to ETN properties?

[Edited on 28-10-2016 by Tricka90]
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[*] posted on 28-10-2016 at 07:37


Quote: Originally posted by Tricka90  
- Is it possible to not noticing any fizzing when ETN is washed with sodium bicarbonate solution? (maybe because it was previously washed with a plentiful amount of water)
- What if ETN is continued to be washed with sodium bicarbonate solution for a long time after the fizzing has stopped? Can it be detrimental to ETN properties?

[Edited on 28-10-2016 by Tricka90]


Yes, of course the acid contaminants can mostly be removed by washing with water due to their highly soluble nature.

Washing with a bicarb solution for extended periods likely won't help neutralize the ETN any further but it also isn't going to hurt anything either.

No matter how well the ETN is neutralized with bicarb solution there will still be acids trapped within causing decomposition so it should be recrystallized ASAP.

Also, you seem more cautious than what is reasonable.
I don't even think an accidental detonation of ETN is possible during synthesis.
I've purposely let nitrations runaway many times just to see what would happen, the result was lots of NO2 and nitric acid vapors but never an explosion.
The dehydration and oxidation appears to destroy any ETN that may have formed, once everything calms down you're left with a flask of what appears to be mainly carbon and sulfuric acid.

I understand being cautious but working in 300mg amounts and being afraid to handle even that quantity just seems silly.
ETN isn't going to spontaneously detonate, under ordinary conditions the danger is quite minimal.

[Edited on 28-10-2016 by OneEyedPyro]
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[*] posted on 28-10-2016 at 08:40


I don't think runaway reactions of ETN on the scale that people on here perform it on can lead to an actual detonation. The risk is with large commercial batches I think and I especially would not worry about a 300mg batch.

I agree, don't lose your cautiousness when doing these sorts of things but you don't have to be that paranoid about a 300mg batch that's for sure.
It is nice to see some people on here that are cautious, some peoples posts that have come and gone have been shocking (starting nitration and leaving it overnight in bedroom, runaway nitration reactions in soda bottles).




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[*] posted on 29-10-2016 at 13:47


Thank you for all the help, I really appreciate it.
Yes, I know, maybe I'm too cautious, but I'm just a beginner, maybe I'll develop some more self-confidence later.
Talking about neutralization, as a general rule of thumb how much milliliters of sodium bicarbonate solution (saturate) do you think are needed for gram of ETN? I know that's kind of a difficult question as the quantity could vary a lot from time to time, but I would like to have just a humble guideline.
About recrystallization, I've heard that using ethanol from pharmacy/drugstore is even better than using laboratory grade ethanol because the one sold in pharmacy also contains anti acid compounds, what do you think about it?
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[*] posted on 29-10-2016 at 20:04


It really doesn't matter, for a 25 gram batch I would wash it with about a 500ml of tap water followed by 500ml of bicarb solution and finally a quick rinse with more tap water.

As far as alcohol you can use just about anything, even 70% isopropyl alcohol works decently.
I'd suggest whatever's cheapest.
Remember, recrystallization can be safe or very dangerous depending on your procedure.

Heating a highly flammable solvent that's nearly saturated with ETN in a glass container over a naked flame is full blown darwin award material, yet someone here did exactly that and lost a hand as a result.

I recommend heating some water to about 65C, remove it from heat and away from any possible ignition sources then place your container of alcohol into the hot water, begin adding your ETN bit by bit with gentle stirring making sure not to allow it to settle to the bottom and pool up. Once it's all added you can filter the solution if their appears to be any insoluble impurities, now dump it into 10 times the volume of distilled water with rapid stirring. You can optionally add a few percent urea to the water as a stabillizer, a few percent sodium bicarbonate can be used if you can't find urea.
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[*] posted on 29-10-2016 at 23:16


Thanks a lot OneEyedPyro for the detailed explanation, I'll definitely follow your advices.
The only thing I'm afraid of is recrystallized ETN seems to be more sensitive than non-recrystallized ETN, or at least that's what I've read. If that's true I wouldn't do anything to increase the sensitivity of ETN which is too sensitive already... What do you think about it?
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[*] posted on 30-10-2016 at 01:11


Sensitivity to impact varies a lot based on crystal size, ETN as a very fine low density powder is quite insensitive to impact while large dense crystals will be significantly more sensitive. The method of recrystallization I mentioned yields a very fine powder if done right.

Unrecrystallized ETN can be unpredictable and has a very short shelf life, recrystallization is an absolute necessity in my opinion.

It may be sensitive compared to many other secondaries but no reasonable amount of friction or impact will set it off.
As a fine powder you can place it on a concrete floor and drag a hammer across it with all of your weight and nothing will happen, you could literally wrap it in foil run it over repeatedly with a car and again nothing will happen.

The biggest danger ETN presents is its ability to undergo DDT when ignited or strongly heated. Good charge design is important, if stray sparks from the fuse somehow fell onto the ETN prematurely it could detonate but even that is unlikely.

Now as long as you don't do anything drastic and maintain a reasonable level of respect for it I don't think you'll have any issues, in fact I predict you'll have issues actually getting it to detonate :D
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[*] posted on 30-10-2016 at 01:44


Thank you again OneEyedPyro :) All your advices are very informative and helpful, you definitely have matured lots of experience on the subject!
How much ethanol per gram of ETN is needed, in your opinion, to accomplish your recrystallization process? I think 10ml 95% ethanol per gram of ETN should be appropriate and then, after filtration, 10 times volume of water should be added, as you said, so it's 100ml water if my guess is correct.
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[*] posted on 30-10-2016 at 08:08


Quote: Originally posted by OneEyedPyro  
Now as long as you don't do anything drastic and maintain a reasonable level of respect for it I don't think you'll have any issues, in fact I predict you'll have issues actually getting it to detonate :D


You got that right. I don't use ETN but I do use PETN which is also a secondary with debatable sensitivity.
I plasticize mine and a few times I haven't had as powerful detonator as I usually use with me and it has blown the explosive around in chunks with no detonation at all...
Have also had a couple of low order dets from weaker caps.
So yeah, I wouldn't worry too much....




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[*] posted on 30-10-2016 at 23:17


Tricka. To be perfectly honest with you I've never bothered to do exact measurements.
I simply added ETN until it was having a hard time dissolving then added a bit more hot methanol from a second container in the hot water bath.

I always dumped the solution into the water rather than the other way around.
It's important to pour the solution slowly while stirring the water or the precipitate tends to clump, I found an easy way to avoid this by stirring the water as to get it quickly swirling clockwise while slowly pouring the solution in a counter clockwise motion.

The only problem is that the precipitate is so fine that it's hard to filter, it tends to clog the filter paper a bit and some even escapes through. It makes handling it a bit messy and it can become airborne easily, it does however press nicely and the friction/shock sensitivity is quite low.
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[*] posted on 2-11-2016 at 06:31


Thank you greenlight and OneEyedPyro.

@OneEyedPyro: your recrystallization process seems very safe to accomplish! However since safety is its main priority I think yield won't be optimal, is that correct? If ethanol were heated up by direct flame until boiling point and then ETN were added until saturation then it would be easier to obtain higher yields (but it would be way more dangerous as well!). On the other hand doing your procedure, that is warming ethanol to an initial temperature of about 60°C and letting it decrease a lot during the addition of ETN while staying away from saturation would be way harder to obtain higher yield. What do you think about it? What's the usual yield you use to obtain?

p.s. I agree with you of course: safety first.
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[*] posted on 2-11-2016 at 09:15


it is really simple heat up alcohol, dump in ETN, keep warmed until alcohol volume goes down if you need it to, slowly dump into twice the volume of stirred ice cold water! Filter, dry, store.

At this point there is no effect on yield! you get out what you put in - the acid.

I use 1% by mass urea in the alcohol solution, and 3% by mass urea in the water solution to help act as a stabilizer and acid scavenger, some use ammonia.

I use methanol my self, some times when I want to skimp on the methanol I use an acetone blend, then I drive off the acetone from the methanol then reduce methanol volume and very slowly cool to grow high density crystals, for light fluffy crystals use above technique.
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[*] posted on 18-12-2017 at 18:57
Erythritol Tetranitrate Lab Notes


Hello everyone,

I realize there are many threads on ETN, however I had a pretty smooth synthesis today and thought I'd share my lab notes. It has been years since I've synthesized any energetics as I've been out of country a lot but there is an opportunity to blast some unwanted beaver dams and stumps at a friends farm. So I jumped at the prospect of rendering my services. The project doesn't kick off until next year, but I promise I will return with footage and pictures.

I'll be producing some Nitroglycerine as well. I'll be mixing it with Acetone with a 70/30 mixture to desensitize it and utilize it for making 8 gram booster charges. I'll post those results as well.

Materials:
250ml Sulfuric Acid 98% Lab Grade
130g Ammonium Nitrate - Powdered in grinder
40g Erythritol

The reaction vessel was a 500ml Pyrex beaker immersed in an ice bath. I added the AN slowly over a period of about 45 minutes. I was careful to not allow the temperature to rise above 15* C at any time. A magnetic stir bar was used to stir the nitrating mixture.

I allowed the mixture to stand for 20 more minutes after the final addition of AN and turned the stirring speed to maximum. This ensured all AN was dissolved and the solution was clear. Nitric Acid fumes were present but removed with fume hood.

After the nitrating mixture cooled to 10* C, I began adding Erythritol slowing, keeping the temperature at 10* C. The entire addition took about 15 minutes. I then let it stand for 20 more minutes, stirring occasionally with a glass stirring rod. At this point the mixture had become so thick with ETN crystals that the stir bar was not working.

I crashed the nitrating mixture into a 3000ml glass beaker filled with ice cold water and 10 grams of sodium bicarbonate. There was substantial amounts of bubbling due to the acid contacting the bicarb, but it did not flow over the edge.

I then gravity filtered the precipitate using filter papers and discarded the waste. I rinsed the product with a few liters of bicarb solution. I was impressed with the yield as it appeared to be quite good considering I had used the nitrate salt method. (I need to do another Nitric Acid synthesis if I ever buy a new condensation column after breaking mine :mad: )

I then took the crystals and dissolved them in Acetone. I would have preferred Ethanol, but I'm working with what I got. It took about 200ml of Acetone to fully dissolve the precipitate.

After cleaning the 3000ml Beaker, I filled it with ice water and dissolved 15 grams of Sodium Bicarbonate. I then crashed the ETN in situ into the cold water and used a large stir bar to stir. The ETN recrystalized and was filtered from the water. The crystal structure obtained from using Acetone isn't as desirable as what is achieved with Ethanol, but it is still acceptable. I may just make blasting gel by dissolving in some Nitroglycerine in which case it won't matter, but we'll see. pH paper was used to test for residual acidity.

The crystals were then dried and stored in a dry, cool place. Final dry weight was 48 grams. I was a bit lazy when rinsing the crystals so I probably could have gotten a few more grams if I had been more careful. Overall, a pretty damn good yield.

Notes:

In past ETN synthesis, I have had a problem with low yields. I believe this was due to allowing the nitrating mixture to become too warm (over 15*) which has a negative affect on the production of Nitric acid while adding a Nitrate salt. So for beginners, watch your temperatures and take your time.

When allowing the nitrating bath to stand after adding the Erythritol, I think it's important to keep an eye on your product and stir. If done correctly, at the end of 20 minutes, the mixture should be so thick with ETN crystals that you think you'll break your stirring rod. Don't let it stand too long, I've had product begin to decompose from being left in the acid too long.

Always always recrystallize your energetic materials. It can be a pain in the ass, but not as much of a pain in the ass as when you don't do it and half of your product decomposes overnight. It also ensures a more pure product, which mitigates risk of sensitizing your energetics inadvertently. Also always test your final product with pH paper before drying.

Anyway, hope this will be helpful to some. I'll post my lab notes for the Nitroglycerine and primary synthesis and eventually the results of my blasting expedition. I look forward to some feedback :cool:

PS : Attached is a photo of the final product.


received_380343405754627.jpeg - 210kB


[Edited on 19-12-2017 by EWillies]
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[*] posted on 19-12-2017 at 03:31


Seems pretty low, I did allot of 17g runs and usual return was 23grams products that no3 group is weighty.

I found allot more comes out of the first crash mixture when allowed to stand for a day, so after filtering I keep that water in a storage jug for refiltering
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[*] posted on 20-12-2017 at 03:55


Indeed, it is less than 50% yield. The theoretical yield from 40 g erythritol is 99 g, and nitration of alcohols are typically high yielding; PETN synthesis from WFNA and PE usually gives me more than 95 % theoretical.
I think the nitration system is to blame - IIRC, I have had quite reduced yields using AN/H2SO4 in mannitol nitrations.
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[*] posted on 20-12-2017 at 05:20


You did a synthesis, got some of the intended compound AND you took notes... Congratulations, and thanks for posting.

I have merged your posts with a related existing thread, as some already noted, the reported % yield was well below theoretical, there is quite some discussion on that here.

Here is the FAQ regarding posting, generally you should look for a closely related existing thread unless you have something new and different.

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Additionally, you will want to restrict your posting to chemistry, physics and engineering related to your subject, this is not where you want to post crater videos and such, go to YouTube if you absolutely must.

We don't let organic chemistry posts stray into balls out meth lab implementation/my last batch of fentanyl posts, the energetic section is not for weapons demos or other illegal applications.

Pardon me, I just spent 2 hours since initialy posting this in our office with a BATF agent. Not because we did anything wrong, just a license renewal.

Possibly I am a bit on edge, but PLEASE don't post about blowing up beaver dams in the USA with explosives made not on day of use (manufacturing license, storage magazine, record keeping? BATF!), not at site of use (shipping explosives with no EX#, transported on public roads unplacarded, by a non Hazmat licensed driver with no bills of lading? DOT and PHMSA!) and most especially, doing this for any kind of compensation ("in commerce" MATTERS- Both to DOT for transport of reportable quantities of Hazmat and BATF for engaging in an explosives related business without a license).

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[Edited on 22-12-2017 by Bert]




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