Sciencemadness Discussion Board

Synthesis of ETN & Fuming Nitric Acid

wessonsmith - 3-7-2019 at 06:20

I am trying to decide if I should go through the trouble of a synthesis video for ETN and Fuming Nitric acid. My ETN synthesis method is based on the 1928 patent method which does not require any cooling of the mixed acids.

My Fuming Nitric Acid synthesis produces 300mL in 1.15hrs from 850g Potassium Nitrate and 510mL 98% Sulfuric Acid.

So, with 180g of Erythritol and the 300mL of Fuming Nitric acid, and an additional 440mL of 98% Sulfuric Acid(dehydration of the Erythritol) I can produce approx 285g - 300g of 2x recrystallized ETN.

Total cost breakdown for the main precursors:
ETN Manufacture (180g)

Erythritol 180.0g $1.92
98% Sulfuric Acid 440mL $6.98
94ish% Nitric Acid 300mL $10.54

I have done this synthesis many times so I have it down to a science. I even have a simple method to eliminate dangerous NO2 gases from escaping from the Fuming Nitric acid synthesis. All of my equipment can be purchased from eBay.

I have seen other synthesis videos of both ETN and Fuming Nitric acid and they seem cumbersome and/or time-consuming for very little product.

If someone else has already done this with equally good results, please post a link. Thanks!!!

underground - 3-7-2019 at 07:48

Why do you bother with FNA for ETN synthesis. You can just use directly 200g H2SO4, 65g kno3, 15g E. Do you think the extra effort worth for a bit better yields ?

You actually use 180gE, 850g

wessonsmith - 3-7-2019 at 07:59

Quote: Originally posted by underground  
Why do you bother with FNA for ETN synthesis. You can just use directly 200g H2SO4, 65g kno3, 15g E. Do you think the extra effort worth for a bit better yields ?

You actually use 180gE, 850g


For me, the synthesis of FNA is very fast and easy. Plus no NO2 fumes, which is a big plus. From what I have seen, the yield using my method is much better using FNA than the method you described.

Yes, I use 180g of Erythritol and 850g KNO3. I do this amount because my FNA production uses a 1000mL round bottom flask limiting my FNA to 300mL. So 300mL of FNA is enough to convert 180g of Erythritol into 300g of ETN.

Rocinante - 3-7-2019 at 09:25

There is a guy on BitChute that claims/shows ETN synthesis with 100 g of 96 % SA (some 60 ml), 40 g of ammonium nitrate and 10 g E with near 100 % yields - i.e. about 23 g of ETN. He starts at - 18°C.

His synthesis would be the cheapest one, I tried it and got only 11 g of product. Not sure about his way because of it.

https://www.bitchute.com/video/XrjpCnYs7fVL/





[Edited on 3-7-2019 by Rocinante]

[Edited on 3-7-2019 by Rocinante]

underground - 3-7-2019 at 10:10

ETN yields are almost never that high just like some patents or guys say. Useing PE instead of E and nitrate it up to 70+ °C after 30 min with mixed acids yields go high. That is why nowdays i use PE instead of E.

[Edited on 3-7-2019 by underground]

wessonsmith - 3-7-2019 at 10:29

Quote: Originally posted by Rocinante  
There is a guy on BitChute that claims/shows ETN synthesis with 100 g of 96 % SA (some 60 ml), 40 g of ammonium nitrate and 10 g E with near 100 % yields - i.e. about 23 g of ETN. He starts at - 18°C.

His synthesis would be the cheapest one, I tried it and got only 11 g of product. Not sure about his way because of it.

https://www.bitchute.com/video/XrjpCnYs7fVL/

[Edited on 3-7-2019 by Rocinante]


Actually, according to my math, it's not cheaper.

His method:
Erythritol 180g
NH4NO3 720g
H2SO4 1800g (984mL)

V.s

My method:
Erythritol 180g
KNO3 850g
H2SO4 950mL(total SA for Nitric production and dehydration of Erythritol)


Plus his method takes a lot LONGER and makes a fuming mess plus the danger of a runaway. When you factor in your getting 11g of ETN which sounds about right, his method is dangerous and time-consuming for resources used. Not to mention I am making 300g of ETN with a 2000mL reaction vessel. His method would require a MUCH larger reaction vessel to get it to work and trying to keep the reaction mixture cool with that much stuff would be impossible. In fact, by the looks of it, his method would be almost impossible to make more than 60g of ETN. The cooling would be next to impossible.

caterpillar - 3-7-2019 at 10:31

There is no need in distillation if you wanna make ETN. Use AN, dissolved in H2SO4 instead. If you make conc NA, use it for RDX or HMX.

wessonsmith - 3-7-2019 at 10:39

Quote: Originally posted by underground  
ETN yields are almost never that high just like some patents or guys say. Useing PE instead of E and nitrate it up to 70+ °C after 30 min with mixed acids yields go high. That is why nowdays i use PE instead of E.

[Edited on 3-7-2019 by underground]


You are correct about yields. I like ETN over PETN because of the OB% I take advantage of this with my Thermobaric mixtures as well as my ETN/NHN binary Composition. More bang from the synergy. Plus Erythritol is sold on Amazon with no chance of being put on a watch list when you by 20lbs:)

wessonsmith - 3-7-2019 at 10:43

Quote: Originally posted by caterpillar  
There is no need in distillation if you wanna make ETN. Use AN, dissolved in H2SO4 instead. If you make conc NA, use it for RDX or HMX.


Using the method you describe, how much ETN can you produce at a time?

twelti - 3-7-2019 at 11:25

Distilling seems like a hassle, and a certain element of risk IS involved. Takes up space and time, which I have the least of. FNA is more dangerous to handle and store than 70% NA. I don't see how saving a few dollars on yield factors into the equation one way or the other, at least not for me, and the amounts I'm interested in using. Could be useful in the future however, so keep posting!

wessonsmith - 3-7-2019 at 11:30

Thanks for the feedback.

[Edited on 3-7-2019 by wessonsmith]

twelti - 3-7-2019 at 12:03

Quote: Originally posted by underground  
Useing PE instead of E and nitrate it up to 70+ °C after 30 min with mixed acids yields go high. That is why nowdays i use PE instead of E.

[Edited on 3-7-2019 by underground]

Are you just using the standard procedure but going up to 70 rather than 50 degrees at the end?

underground - 3-7-2019 at 13:05

70+ at the end. Yea standard procedure just like ETN. ETN will decompose at such temps but PETN wont.

[Edited on 3-7-2019 by underground]

wessonsmith - 3-7-2019 at 13:14

Quote: Originally posted by underground  
70+ at the end. Yea standard procedure just like ETN. ETN will decompose at such temps but PETN wont.

[Edited on 3-7-2019 by underground]


Yeah, I nitrate my ETN at 55°C. Been doing that since day one, 3 yrs ago.

[Edited on 3-7-2019 by wessonsmith]

underground - 4-7-2019 at 06:06

I nitrate ETN at max 23°C. If i go above 30°C it will decompose (kno3/h2so4 method).

wessonsmith - 4-7-2019 at 06:20

Quote: Originally posted by underground  
I nitrate ETN at max 23°C. If i go above 30°C it will decompose (kno3/h2so4 method).


Using your method, how much ETN can you produce per session.

underground - 4-7-2019 at 10:34

What do you mean by "per session". My yields are about 65%. You can scale it up as much as you want.

[Edited on 4-7-2019 by underground]

wessonsmith - 4-7-2019 at 11:10

Quote: Originally posted by underground  
What do you mean by "per session". My yields are about 65%. You can scale it up as much as you want.

[Edited on 4-7-2019 by underground]


What I was trying to ask was how much you can make at one time. The reason why I ask is it seems with the method you are using it would be very difficult to keep a larger amount cool.

underground - 4-7-2019 at 11:56

You can put the H2SO4 into deep freeze and procced with a lot of ice. Than is for ETN. For PETN is quite easier cause it is not that sensitive to temperature like ETN.

[Edited on 4-7-2019 by underground]

Rocinante - 4-7-2019 at 14:37

65 % yields using KNO3? Can you give us the exact ratios/procedure?

underground - 4-7-2019 at 14:53

200g H2SO4, 65g kno3, 15g E. Fine powders and completely dry from a desiccator bag. H2SO4 boiled down to azeotrope (98%). Add KNO3 to H2SO4 by keeping temp below 10C. After addition of KNO3 completed, drop the temp below 6C then add E i small portions while keeping temp below 6C. After the addition of E completed, keep below 6C for 15min. Then slowly increase the temp to 22-23C max for about 30min. Always maintain vigorous stirring


[Edited on 4-7-2019 by underground]

Strange batch

twelti - 5-7-2019 at 12:22

I just did another batch of ETN, around my 4th or 5th one. I was a little distracted by wife and house guests. I probably should have just waited until next weekend but I was impatient. So, my timing and temp control was not as good as usual. I have had perfectly good results and yields before using same method, mixed acids. This time i did a larger batch, 15 g of E. 120ml SA, 75 ml 70% NA. One thing is that it takes forever, even with a salted ice bath, to add the NA to the SA without getting too hot. In my case it was kept below 20 deg or so, max, during addition. The solution does not thicken toooo much and can still be stirred using mag stirrer, though it is sometimes hard to see if it is effectively stirring when it thickens up to cream consistency and you can't see in there. I did let it go up to around 25-30 deg at the end (helped with warm water bath). It may have sat in the nitration bath longer than I usually do, as I said, I was distracted. Also noticed a small yellow spot on the top after warming, which I immediately stirred back into the rest of it.

Thing is, I got some larger chunks in here after crashing into water. Some are 3-4 mm across. I'm neutralizing and will reX tonight, but wondered if I should be concerned. I normally get fine crystals, like snowflakes.

wessonsmith - 5-7-2019 at 18:03

Quote: Originally posted by twelti  
I just did another batch of ETN, around my 4th or 5th one. I was a little distracted by wife and house guests. I probably should have just waited until next weekend but I was impatient. So, my timing and temp control was not as good as usual. I have had perfectly good results and yields before using same method, mixed acids. This time i did a larger batch, 15 g of E. 120ml SA, 75 ml 70% NA. One thing is that it takes forever, even with a salted ice bath, to add the NA to the SA without getting too hot. In my case it was kept below 20 deg or so, max, during addition. The solution does not thicken toooo much and can still be stirred using mag stirrer, though it is sometimes hard to see if it is effectively stirring when it thickens up to cream consistency and you can't see in there. I did let it go up to around 25-30 deg at the end (helped with warm water bath). It may have sat in the nitration bath longer than I usually do, as I said, I was distracted. Also noticed a small yellow spot on the top after warming, which I immediately stirred back into the rest of it.

Thing is, I got some larger chunks in here after crashing into water. Some are 3-4 mm across. I'm neutralizing and will reX tonight, but wondered if I should be concerned. I normally get fine crystals, like snowflakes.


I have made ETN about 25+ times. I usually make 300g at a time. My mixed acid method is 180g Erythritol that I first dehydrate in 440mL of 98% Sulfuric Acid. This requires some cooling with an ice bath. I can add the 180g of Erythritol to the Sulfuric Acid in about 20 min, 10min if I add AN to the ice. You will need to keep the temperature below 40°C or your Erythritol will carbonize. Once all the Erythritol has been added I then add that mixture to my Fuming Nitric acid in (4) separate additions. So approx 175mL at a time. I need to apply heat so I can get the mixed acid Erythritol mixture to 55°C reaction temperature.

Try dehydrating your Erythritol in Sulfuric Acid first, then temperature control won't be such an issue.



[Edited on 6-7-2019 by wessonsmith]

twelti - 5-7-2019 at 19:16

Quote: Originally posted by wessonsmith  
Quote: Originally posted by twelti  
I just did another batch of ETN, around my 4th or 5th one. I was a little distracted by wife and house guests. I probably should have just waited until next weekend but I was impatient. So, my timing and temp control was not as good as usual. I have had perfectly good results and yields before using same method, mixed acids. This time i did a larger batch, 15 g of E. 120ml SA, 75 ml 70% NA. One thing is that it takes forever, even with a salted ice bath, to add the NA to the SA without getting too hot. In my case it was kept below 20 deg or so, max, during addition. The solution does not thicken toooo much and can still be stirred using mag stirrer, though it is sometimes hard to see if it is effectively stirring when it thickens up to cream consistency and you can't see in there. I did let it go up to around 25-30 deg at the end (helped with warm water bath). It may have sat in the nitration bath longer than I usually do, as I said, I was distracted. Also noticed a small yellow spot on the top after warming, which I immediately stirred back into the rest of it.

Thing is, I got some larger chunks in here after crashing into water. Some are 3-4 mm across. I'm neutralizing and will reX tonight, but wondered if I should be concerned. I normally get fine crystals, like snowflakes.


I have made ETN about 25+ times. I usually make 300g at a time. My mixed acid method is 180g Erythritol that I first dehydrate in 440mL of 98% Sulfuric Acid. This requires some cooling with an ice bath. I can add the 180g of Erythritol to the Sulfuric Acid in about 20 min, 10min if I add AN to the ice. You will need to keep the temperature below 40°C or your Erythritol will carbonize. Once all the Erythritol has been added I then add that mixture to my Fuming Nitric acid in (4) separate additions. So approx 175mL at a time. I need to apply heat so I can get the mixed acid Erythritol mixture to 55°C reaction temperature.

Try dehydrating your Erythritol in Sulfuric Acid first, then temperature control won't be such an issue.

Remember, the more water you are adding the hotter the reaction is going to be. So using 70% Nitric Acid means you are adding a lot of water which means a lot of heat generation.


[Edited on 6-7-2019 by wessonsmith]

Thanks for your hints. Dang, that is a lot of ETN you have made!! I can see why yield is very important to you. I did try the other method, dissolving in SA first, on the last batch. Yield seemed about the same, though I've not controlled all variables in order to make a good comparison. I don't have FNA, and haven't felt the need yet, though I know there are some advantages.

Upon reX, I got a gram or two of material not dissolving in the EtOH. I filtered that out. It is very slightly yellow, and dull colored. The rest came through with flying colors. Bright white and twinkly like mica, just like before. My stir rod might have got stuck. I've noticed if I turn it up too fast, after the liquid gets thick, it just starts jumping around and not stirring. It is also harder to see in there as the nitration goes on. I didn't go up anywhere near 55 degrees in the nitration. Im getting around 70% yield (AFTER reX).

I bought a microscope to look at the crystals. I'm having a hard time correlating my product to others description of crystal form. My ETN comes out looking like snowflakes in suspension, and almost like a paste after final filtering. I'm doing reverse Rex in hot EtOH, using icecube "seeding" and then pouring cold dH2O slowly into vigorously stirred EtOH.

wessonsmith - 6-7-2019 at 05:15
Quote:

I did try the other method, dissolving in SA first, on the last batch. Yield seemed about the same, though I've not controlled all variables in order to make a good comparison. I don't have FNA, and haven't felt the need yet, though I know there are some advantages.



Just an FYI, my yields are based on maximizing my Fuming Nitric Acid precursor and not the Erythritol. 180g of Erythritol converted to 300g of ETN is a lousy yield when based on the theoretical maximum conversion of Erythritol to ETN. However, since the precursor Erythritol is now 10x less expensive to use than Fuming Nitric acid, I tweaked the ratios to maximize the Fuming Nitric Acid precursor.

The reason for dehydrating the Erythritol in Sulfuric Acid first is 1) Safety; no chance of a runaway once the Erythritol has dehydrated. 2) Ease of manufacture; temperature control is much easier when you are heating rather than cooling. This advice only applies to Fuming Nitric Acid. When you are using 70% Nitric Acid, you are introducing water which when mixed with the acids generates heat.

You need higher temperatures so that you can easily mix your nitration mixture with a stir bar. At the higher temperature, the ETN remains dissolved in the acids. When the mixture is allowed to cool below 45°C, ETN starts to crash out, causing the mixture to thicken up considerably, making stirring with a stir bar next to impossible. Allowing the nitration mixture to thicken up before all of the Erythritol has converted, you increase the possibility of localized excessive heat, which destroys some of the ETN.

Once you start using Fuming Nitric Acid, all of the issues you are having will go away. I can't stress enough just how easy and relatively inexpensive it is to manufacture Fuming Nitric Acid.

underground - 6-7-2019 at 05:42

Have you ever try to make RDX from that FNA?

wessonsmith - 6-7-2019 at 06:09

Quote: Originally posted by underground  
Have you ever try to make RDX from that FNA?


No. I don’t have any need for RDX, PETN since my compositions take advantage of ETN’s positive oxygen balance.

Take my Thermobaric composition. I can use 55% ETN and no Ammonium Perchlorate. If I were to use RDX, I would need 10% AP, so my composition would be less potent as compared to ETN.

My plastic also takes advantage of the synergy between the excess oxygen of ETN and the fuel richness of the HTPB binder. The first 15% of the HTPB binder is converted to energy using ETN. RDX's power is watered down immediately. So the power of two plastics both using a 12% binder one based on ETN the other on the more powerful RDX are the same due to the synergy between ETN and the fuel. Remember, RDX's power is realized at higher densities, and since plastic explosive hover around 1.55-1.62 g/cm^3, RDX's power advantage is nullified.

Considering ETN in detonators, nothing is more straightforward and easy to replicate as a melt-cast secondary.

[Edited on 6-7-2019 by wessonsmith]

underground - 6-7-2019 at 07:17

It is not everything about oxygen balance. For example you can see that PETN and RDX do perform better than ETN despite their negative OB. Very impoetant is density. C4 with12+% inerts and even worse OB from RDX itself still perform better than pure ETN.

[Edited on 6-7-2019 by underground]

wessonsmith - 6-7-2019 at 07:27

Quote: Originally posted by underground  
It is not everything about oxygen balance. For example you can see tha PETN and RDX do perform better than ETN despite their negative OP. Very impoetant is density. C4 with12+% inerts and even worse OP still perform better than pure ETN itself.


[Edited on 6-7-2019 by underground]


We are talking about a marginal difference. When you factor in the cost of precursors and difficulty of manufacture as compared to ETN, there is no contest for me. My Therombaic, however, is more potent than an RDX based version.

Here is an example of the effect that my ETN based plastic has on cold-rolled steel 6.4mm thick. I was using 5g of my plastic and one of my #8 power detonators.

https://drive.google.com/drive/folders/1BZrbD1aTIWdly4TyZZgO...


FYI. C4 only has a density advantage when in block form. Once you start to kneed it, the density drops down to approx 1.55 g/cm³.

[Edited on 6-7-2019 by wessonsmith]

underground - 6-7-2019 at 07:37

As you wish

wessonsmith - 6-7-2019 at 07:40

Quote: Originally posted by underground  
As you wish


It comes down to each his own. I am not in any way negating the general importance of either RDX, PETN just stating that they are of no interest to me based on the reasons provided.

underground - 6-7-2019 at 07:45

If i where you, i should made them both, even HMX too and try them out. After you could decide more wisely. I was thinking the same as you for PETN but when i tried it out, i changed my mind.

[Edited on 6-7-2019 by underground]

wessonsmith - 6-7-2019 at 09:12

Quote: Originally posted by underground  
If i where you, i should made them both, even HMX too and try them out. After you could decide more wisely. I was thinking the same as you for PETN, but when I tried it out, I changed my mind.

[Edited on 6-7-2019 by underground]


You make a fair point. If I were to synthesize RDX or HMX, it would be for personal edification only. In the US, buying large quantities of the precursor, Pentaerythritol will get you put on a list. I can buy 25KG of Erythritol off Amazon without any issue. When I consider the cost of the precursors and the cost manufacture and the quantity I like to play with, ETN is the only choice for me.

I will, however, stand by my assertion that my Thermobaric mixture is more powerful using ETN than using HMX or RDX. 22% more high explosive is a lot more high explosive. When you consider the power difference between the two at the densities, the Thermobaric mixture is pressed too, ETN wins hands down.



[Edited on 6-7-2019 by wessonsmith]

underground - 6-7-2019 at 09:40

Quote: Originally posted by wessonsmith  
Quote: Originally posted by underground  
If i where you, i should made them both, even HMX too and try them out. After you could decide more wisely. I was thinking the same as you for PETN, but when I tried it out, I changed my mind.

[Edited on 6-7-2019 by underground]


You make a fair point. If I were to synthesize RDX or HMX, it would be for personal edification only. In the US, buying large quantities of the precursor, Pentaerythritol will get you put on a list. I can buy 25KG of Erythritol off Amazon without any issue. When I consider the cost of the precursors and the cost manufacture and the quantity I like to play with, ETN is the only choice for me.

I will, however, stand by my assertion that my Thermobaric mixture is more powerful using ETN than using HMX or RDX. 22% more high explosive is a lot more high explosive. When you consider the power difference between the two at the densities, the Thermobaric mixture is pressed too, ETN wins hands down.



[Edited on 6-7-2019 by wessonsmith]


We or you have to test it out. I really doubt if you can actually exceed HMX with such mixture. In general AL may increase the temp of explosion but also decrease the VoD, dont trick you the sound. It is generally accepted that Al drop the performance of ETN. You have to try them all, same amount, same steel plate same detonator e.t.c. to have a clear answere.

[Edited on 6-7-2019 by underground]

wessonsmith - 6-7-2019 at 11:21

Quote: Originally posted by underground  
Quote: Originally posted by wessonsmith  
Quote: Originally posted by underground  
If i where you, i should made them both, even HMX too and try them out. After you could decide more wisely. I was thinking the same as you for PETN, but when I tried it out, I changed my mind.

[Edited on 6-7-2019 by underground]


You make a fair point. If I were to synthesize RDX or HMX, it would be for personal edification only. In the US, buying large quantities of the precursor, Pentaerythritol will get you put on a list. I can buy 25KG of Erythritol off Amazon without any issue. When I consider the cost of the precursors and the cost manufacture and the quantity I like to play with, ETN is the only choice for me.

I will, however, stand by my assertion that my Thermobaric mixture is more powerful using ETN than using HMX or RDX. 22% more high explosive is a lot more high explosive. When you consider the power difference between the two at the densities, the Thermobaric mixture is pressed too, ETN wins hands down.



[Edited on 6-7-2019 by wessonsmith]


We or you have to test it out. I really doubt if you can actually exceed HMX with such mixture. In general AL may increase the temp of explosion but also decrease the VoD, dont trick you the sound. It is generally accepted that Al drop the performance of ETN. You have to try them all, same amount, same steel plate same detonator e.t.c. to have a clear answere.

[Edited on 6-7-2019 by underground]


I would agree if it were equal amounts of HMX and ETN, that the HMX would be more powerful. However, the ETN version has 22% more high explosive, so the math says that the ETN version will be more powerful.

VOD is not a paramount issue for thermobaric's. 7,000 m/s is more than adequate for that type of explosive composition.

twelti - 7-7-2019 at 10:18

Since we are talking about ETN, I'm wondering if you guys' product is sensitive to impact? Mine is very insensitive, to the point that I thought it was not ETN when I fist made it. I find it almost impossible to detonate it wrapped in foil with hammer (steel on steel). I know it is a secondary, but descriptions I have read in literature would suggest it should be more sensitive. I'm thinking maybe it is the small crystal size I'm getting. Under a microscope, I don'e even really see any crystals. Looks kind of amorphous or maybe the crystals are just very small.

Wrapped in foil, it detonates just fine. 1 mg is quite loud. Looks very pure (reX at least once). PH tests neutral, no odor etc.

MineMan - 7-7-2019 at 10:55

Wesson. What is your thermobaric comp? Also. I am not sure I agree with your math, the 22 percent more explosive, maybe I am just not thinking right...

wessonsmith - 7-7-2019 at 12:07

Quote: Originally posted by MineMan  
Wesson. What is your thermobaric comp? Also. I am not sure I agree with your math, the 22 percent more explosive, maybe I am just not thinking right...


Here is a link to an interactive spreadsheet. At the bottom you choose the amount of the Thermobaric composition you want, the sheet will populate with the appropriate amounts of the other ingredients.

https://docs.google.com/spreadsheets/d/1UgFokDX_ikGcVIjsvubl...

FYI here are the two papers from which I got the basic formula. In the documents, they test 14 different variations settling on TBE-3, which is what I modified.

https://drive.google.com/drive/folders/1ALAn-co9H3OugWTx45Yj...

[Edited on 7-7-2019 by wessonsmith]

wessonsmith - 7-7-2019 at 12:09

Quote: Originally posted by twelti  
Since we are talking about ETN, I'm wondering if you guys' product is sensitive to impact? Mine is very insensitive, to the point that I thought it was not ETN when I fist made it. I find it almost impossible to detonate it wrapped in foil with hammer (steel on steel). I know it is a secondary, but descriptions I have read in literature would suggest it should be more sensitive. I'm thinking maybe it is the small crystal size I'm getting. Under a microscope, I don'e even really see any crystals. Looks kind of amorphous or maybe the crystals are just very small.

Wrapped in foil, it detonates just fine. 1 mg is quite loud. Looks very pure (reX at least once). PH tests neutral, no odor etc.


Dried ETN is very easy to detonate with a wack of a hammer against steel. If ETN is slightly damp it is very difficult to detonate with a hammer blow.

twelti - 7-7-2019 at 12:13

Quote: Originally posted by wessonsmith  
Quote: Originally posted by twelti  
Since we are talking about ETN, I'm wondering if you guys' product is sensitive to impact? Mine is very insensitive, to the point that I thought it was not ETN when I fist made it. I find it almost impossible to detonate it wrapped in foil with hammer (steel on steel). I know it is a secondary, but descriptions I have read in literature would suggest it should be more sensitive. I'm thinking maybe it is the small crystal size I'm getting. Under a microscope, I don'e even really see any crystals. Looks kind of amorphous or maybe the crystals are just very small.

Wrapped in foil, it detonates just fine. 1 mg is quite loud. Looks very pure (reX at least once). PH tests neutral, no odor etc.


Dried ETN is very easy to detonate with a wack of a hammer against steel. If ETN is slightly damp it is very difficult to detonate with a hammer blow.

Mine is dry I assure you. Either I need a bigger hammer, or it is possibly the crystal size. I'm going to try recrystallizing using slow cooling to try to get larger crystals, just as a test.

wessonsmith - 7-7-2019 at 12:27

Quote: Originally posted by twelti  
Quote: Originally posted by wessonsmith  
Quote: Originally posted by twelti  
Since we are talking about ETN, I'm wondering if you guys' product is sensitive to impact? Mine is very insensitive, to the point that I thought it was not ETN when I fist made it. I find it almost impossible to detonate it wrapped in foil with hammer (steel on steel). I know it is a secondary, but descriptions I have read in literature would suggest it should be more sensitive. I'm thinking maybe it is the small crystal size I'm getting. Under a microscope, I don'e even really see any crystals. Looks kind of amorphous or maybe the crystals are just very small.

Wrapped in foil, it detonates just fine. 1 mg is quite loud. Looks very pure (reX at least once). PH tests neutral, no odor etc.


Dried ETN is very easy to detonate with a wack of a hammer against steel. If ETN is slightly damp it is very difficult to detonate with a hammer blow.

Mine is dry I assure you. Either I need a bigger hammer, or it is possibly the crystal size. I'm going to try recrystallizing using slow cooling to try to get larger crystals, just as a test.


I can tell you with absolute certainty that large or small crystals will behave the same from a hammer blow. I have both, and they both act very similarly. Here is a paper showing the difference between melt-cast and powered ETN, and you will see that the sensitivity difference between the two is minimal. Powdered ETN of different crystal size , the difference will be even smaller.

https://drive.google.com/file/d/1gqDvdSuiXI6F-smxKIHlQlELWHH...



[Edited on 7-7-2019 by wessonsmith]

Microtek - 7-7-2019 at 13:25

The test for impact sensitivity using aluminum foil to contain the explosive and then hitting it with a hammer is flawed. I used it myself for a long time, but discovered that it gives a false impression of insensitivity for many substances. This tendency can to some extent be negated by using a larger amount of explosive.

Herr Haber - 7-7-2019 at 14:24

Quote: Originally posted by underground  
I nitrate ETN at max 23°C. If i go above 30°C it will decompose (kno3/h2so4 method).


Brown fumes observed around 30 degrees aswell using mixed acid (70%).
23 seems indeed a safe spot.

wessonsmith - 7-7-2019 at 14:28

Quote: Originally posted by Herr Haber  
Quote: Originally posted by underground  
I nitrate ETN at max 23°C. If i go above 30°C it will decompose (kno3/h2so4 method).


Brown fumes observed around 30 degrees aswell using mixed acid (70%).
23 seems indeed a safe spot.



I use fuming nitric and 98% Sulfuric. No fumes and 55C reaction temp.

twelti - 7-7-2019 at 14:43

Quote: Originally posted by Microtek  
The test for impact sensitivity using aluminum foil to contain the explosive and then hitting it with a hammer is flawed. I used it myself for a long time, but discovered that it gives a false impression of insensitivity for many substances. This tendency can to some extent be negated by using a larger amount of explosive.

Yes, I had wondered about that. I think the amounts I am using, a few mg, are too small for that test. Will try 20 or 50, with hearing protection.

twelti - 7-7-2019 at 15:05

Quote: Originally posted by wessonsmith  


I can tell you with absolute certainty that large or small crystals will behave the same from a hammer blow. I have both, and they both act very similarly. Here is a paper showing the difference between melt-cast and powered ETN, and you will see that the sensitivity difference between the two is minimal. Powdered ETN of different crystal size , the difference will be even smaller.

https://drive.google.com/file/d/1gqDvdSuiXI6F-smxKIHlQlELWHH...



[Edited on 7-7-2019 by wessonsmith]

If from that paper you make a blanket assumption that the form doesn't have much effect on sensitivity, then ok. They didn't actually test small crystals though (did you see the size of the crystals they did use ?! Huge). I'm not sure you can equate extremely small crystals to a cast solid. I'm gonna grow some large crystals and check. Slow cooling in saturated EtOH?