Sciencemadness Discussion Board

ETN first attempt

insutama - 29-1-2021 at 14:56

I am about to attempt my first ETN synth I was just wondering if i could use the same mix of acids i used when i made PETN
34 ml of 67% HNO3
24.8 ml of 98% H2SO4

and i was gonna use 10 grans Erythritol

any suggestions ?

XeonTheMGPony - 29-1-2021 at 18:54

Search the forum, do the math?

insutama - 29-1-2021 at 20:38

Okay I did some calculations and what I have come up with is
24mg HNO3 67%
36mg H2SO4 98%
6 grams Erythritol

I put this here incase anyone else was looking for this info Ill let you know how it turns out

Laboratory of Liptakov - 30-1-2021 at 08:05

You mean sure mililiters not miligrams I estimate. You need 24 ml x 1.4 = 33,6 g HNO3 + 36 x 1,85 = 66,6g H2SO4.
+ 6g Erythritol........:cool:

insutama - 30-1-2021 at 12:19

lol ya i meant ml my bad i just made it and everything went smooth its drying now ill have to test it tomorrow

XeonTheMGPony - 30-1-2021 at 16:40

Hope fully you read all the big threads to save time and help ensure a good clean pure product!

insutama - 30-1-2021 at 20:24

Seemed to work out good i did a half batch to test it so only used 3 grams of erythritol its still drying ill post the weight when its fully dried came out a nice white powder no discoloration ill do a acetone recrystallization once its dried

Jebby - 20-2-2021 at 12:14

I used Roto Professional liquid drain cleaner and spectracide stump remover In a failed attempt to synthesize ETN and when I mixed the 100g of drain cleaner and 40g of stump remover it turned from a slight yellow color to a almost red color the consistency was that of pudding and apple sauce (viscous and very slightly gritty or chunky). I was wondering if anyone knows what caused this and how I can prevent it.

B(a)P - 20-2-2021 at 13:35

The solid was likely potassium sulphate. Was the mixture letting off a gas? The red colour may have been dissolved NO2.
Did you cool the acid before adding the KNO3. The reaction is very exothermic and additions need to be done in portions with cooling.

Jebby - 22-2-2021 at 06:00

The acid was cooled to around 0°C. It was letting of a white vapor. Do you think that the potassium sulphate would hinder the nitration of the Erythritol?

B(a)P - 22-2-2021 at 13:13

Quote: Originally posted by Jebby  
The acid was cooled to around 0°C. It was letting of a white vapor. Do you think that the potassium sulphate would hinder the nitration of the Erythritol?


Potassium sulfate will not hinder the nitration of erythritol. There are many threads on this forum discussing the nitration of erythritol, have you tried working your way through those? If so can you give a bit more detail on what you did following the the addition of KNO3 to H2SO4.If you are nitrating erythritol with H2SO4 and a nitrate salt you will always end up with a nitration mixture of the consistency you described.

Jebby - 23-2-2021 at 08:22

I have tried to work through a synthesis that I found on bitchute the only real big problem was the solubility, I have been told to add more SA to dissolve it completely. I will have to try the synthesis again today.

B(a)P - 23-2-2021 at 12:01

Quote: Originally posted by Jebby  
I have tried to work through a synthesis that I found on bitchute the only real big problem was the solubility, I have been told to add more SA to dissolve it completely. I will have to try the synthesis again today.


The trouble with copying what you see on a video is that you will often miss important details that the producer glosses over or omits all together. This is particularly true when you are using technical grade reagents. Did the producer of the video also use technical grade reagents, were they the same concentration or brand as you are using, are you sure any additives in your reagents won't hinder the reaction? If you work your way through other peoples mistakes you are much more likely to succeed. Also it is a good idea to find credible published procedures to have as a reference. When you are working with toxic or energetic reactants or products it is advisable to be very certain of the required reaction conditions be aware what could go wrong and have measures in place to mitigate against a worst case scenario. Know that although ETN is classified as a secondary explosive it is, compared to many other secondaries, very sensitive to thermal shock and in its liquid state it behaves more or less as a primary.
It is important to write out the reaction formula and work your way through the stoichometry to make sure you are convinced that you are using the correct mass of reactants. This will allow you to modify your approach if you are using reagents of a different concentration to the video you are basing your synthesis on. It will also allow you to test your yield to see how successful the synthesis was and help make improvements in the future.
Out of curiosity what video are you following? What made you think the consistency of your mixed acids caused your reaction to fail?

DBX Labs - 23-2-2021 at 15:53

Quote: Originally posted by B(a)P  
Quote: Originally posted by Jebby  
I have tried to work through a synthesis that I found on bitchute the only real big problem was the solubility, I have been told to add more SA to dissolve it completely. I will have to try the synthesis again today.


The trouble with copying what you see on a video is that you will often miss important details that the producer glosses over or omits all together. This is particularly true when you are using technical grade reagents. Did the producer of the video also use technical grade reagents, were they the same concentration or brand as you are using, are you sure any additives in your reagents won't hinder the reaction? If you work your way through other peoples mistakes you are much more likely to succeed. Also it is a good idea to find credible published procedures to have as a reference. When you are working with toxic or energetic reactants or products it is advisable to be very certain of the required reaction conditions be aware what could go wrong and have measures in place to mitigate against a worst case scenario. Know that although ETN is classified as a secondary explosive it is, compared to many other secondaries, very sensitive to thermal shock and in its liquid state it behaves more or less as a primary.
It is important to write out the reaction formula and work your way through the stoichometry to make sure you are convinced that you are using the correct mass of reactants. This will allow you to modify your approach if you are using reagents of a different concentration to the video you are basing your synthesis on. It will also allow you to test your yield to see how successful the synthesis was and help make improvements in the future.
Out of curiosity what video are you following? What made you think the consistency of your mixed acids caused your reaction to fail?


I believe that Jebby is referring to this video.
https://www.bitchute.com/video/XrjpCnYs7fVL/
From my recollection, the solution of 40 grams AN in only 100 grams SA is quite difficult to produce with impure AN. As mentioned in the video, recrystallization is necessary.

I just realized that KNO3 was mentioned as the source of nitrate. If that's still the case, this video is not relevant.

[Edited on 23-2-2021 by DBX Labs]

Pyro_cat - 23-2-2021 at 19:32

I got it to work first try with the three off the shelf reagents.

You need a thick sloppy mix of KNO3, Sulfuric and add in one quarter the amount of E you have to KNO3 stir temps time

Thick sloppy mix means your ratio is right.

My first nitration experiments were with cotton and I learned from that mixing up that goop.



[Edited on 24-2-2021 by Pyro_cat]

Jebby - 24-2-2021 at 07:00

The link that DBX posted was the video I was talking about. The reason I thought the consistency of the mixed acids caused a failure is because I didn’t think that the nitration would occur because of how hard it would be to mix. B(a)P I’d like to thank you for the help as I am relatively new to all this, and your advice is very helpful.

DBX Labs - 24-2-2021 at 12:31

Yeah, AN/SA nitrating mixtures are thin and clear when pure even down to 0C. On the other hand, KNO3/SA mixtures are rarely anything but thick and gooey. That’s why I prefer AN over KNO3 for most all nitrations, nitrocellulose included.

B(a)P - 24-2-2021 at 13:27

I have tried with technical grade (from the hardware store) KNO3 and H2SO4 and never achieved better than 60% yield. With this reaction it is a thick paste and it needs continual stirring with a glass rod. The erythritol needs to be added in small portions with lots of stirring in between to mitigate localised hotspots due to the consistency of the reaction mixture.
With laboratory reagent grade azeotropic mixed acids I have achieved 95% yield.
If you are new to this and you are basing your reaction on that video only you are missing an important step, you need to do more research.
Read through the following threads.
https://www.sciencemadness.org/whisper/viewthread.php?tid=24875#pid290333

https://www.sciencemadness.org/whisper/viewthread.php?tid=7209#pid82290

I have added some additional resources that may be helpful.
Keep your quantities small at first to conserve reagents while you are working out your procedure, but most of all for safety. Best of luck.

Attachment: Erythritol Tetranitrate as a Sensitizer in Ammonium Nitrate Based Explosives.pdf (213kB)
This file has been downloaded 408 times

Attachment: Characterization and Analysis of Tetranitrate Esters.pdf (806kB)
This file has been downloaded 369 times

Jebby - 28-2-2021 at 12:05

I can’t thank you enough B(a)P. Your help has been much appreciated.

Industrial Adhesive - 1-4-2021 at 20:30

Quote: Originally posted by Jebby  
I used Roto Professional liquid drain cleaner and spectracide stump remover In a failed attempt to synthesize ETN and when I mixed the 100g of drain cleaner and 40g of stump remover it turned from a slight yellow color to a almost red color the consistency was that of pudding and apple sauce (viscous and very slightly gritty or chunky). I was wondering if anyone knows what caused this and how I can prevent it.
its from potassium sulfate.

Industrial Adhesive - 1-4-2021 at 20:34

Quote: Originally posted by Jebby  
I used Roto Professional liquid drain cleaner and spectracide stump remover In a failed attempt to synthesize ETN and when I mixed the 100g of drain cleaner and 40g of stump remover it turned from a slight yellow color to a almost red color the consistency was that of pudding and apple sauce (viscous and very slightly gritty or chunky). I was wondering if anyone knows what caused this and how I can prevent it.
its from potassium sulfate.