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twelti - 7-4-2019 at 14:12

Quote: Originally posted by snooby  
Why are you sure you have failed? Most nitro esters just burns, but only detonate from inpact. Thats why its called secundary explosive. So in case if you havent tried it, go do some hammerblowntests. Maybe the etn is just fine.


Hi, yes I did try that. Melted it a little, then whack. I did manage to get maybe 1 out of 5 to go that way. I did see on YT where he was just laying some on a piece of foil and with flame , getting high order dets. Mine just defllag so far. I wonder if it is not fully dry? Gonna try another synth, this time letting temp go up to 25 for é0 min. And dry in dessicator.

UPDATE: repeated it but this time added 30 min letting the mixture slowly to up to 27 C and stay. Yield looks to have doubled, at least the before reX yield. 5.5 g E gave 15.5 g moist (pressed) neutralized product. Guessing alot of that is water, but still... Now for the reX.

[Edited on 8-4-2019 by twelti]

Laboratory of Liptakov - 8-4-2019 at 21:10

We are curious on your pure yield with " 27 C and stay".....:cool:...LL
next: My question for an Great scientist of this forum.: I do not find concentration for HClO4 according his boiling point. Especially for 140 Celsius.
Thanks for anyone....:cool:....LL

[Edited on 9-4-2019 by Laboratory of Liptakov]

underground - 9-4-2019 at 03:47

Anhydrous perchloric acid is an unstable oily liquid at room temperature. Perchloric acid forms an azeotrope with water at 203°C, consisting of about 72.5% perchloric acid

ETN strangeness

twelti - 9-4-2019 at 11:53

OK, I'm a bit stuck here. I realize there is a TON of stuff on these forums about ETN synth, but actually 90% seems to be about nitrate salt method(s). I really like the HNO3 idea since i have a bunch and it stirs easily.
Using a longer and warmer nitration period of 30 minutes at around 27 degree C, I did get a bigger yield from my first attempt. Everything looks like it should have been a success, final yield of around 8 g from 5.5 g of erythritol. Also, this time I added ice cubes during the reX to "seed" the crystalization. Material looks pretty much like the first time tough. Pressed between paper towels after final filtration, it is more of a cake. i was hoping for better crystals, using the "add water to EToH" method, but it is same as before.

Small piece on foil heated: deflag and no residue.
Small piece melted and then wrapped in foil and whacked: after several attempts, it did sort of detonate,(i.e. sparks) but not very loud. Strangely, if I whacked it again I often got a second spark. It did not all go off?
It has been drying for a day and a half now. Is it not dry? Should I give up and go nitrate salt method? I have some KNO3.... It is driving me nuts though. What else can it be but ETN?!


20190407_111738.jpg - 4.4MB 20190407_183045.jpg - 3.4MB

johnmay - 9-4-2019 at 12:23

Hello twelti,

Maybe you should check it the other way - wrap it in alluminium foil and put it in the candle flame (not in your hand of course!), it should detonate if it is okay.
ETN is not primmary material so I wouldnt expect it to go off from smacking it on the floor (I saw a yt video of some guys pounding it with big hammer and for no go.

Take care,
Regards

underground - 9-4-2019 at 14:56

Are you 100% that what you use for nitration is pure erythritol ?

C6(NO2)5CH2CH(CH3)N(NO2)2 - 9-4-2019 at 15:28

If it detonated even once, then I think you've got some ETN! The yield may not be as good as it could be, but you succeeded, I think. The rest would probably go if it was dry and was triggered by a primary.

Now my own (probably dumb) question. Has anyone recovered H2SO4 from a nitration? Or is that just an altogether bad idea (eg. traces of explosive product)

twelti - 9-4-2019 at 19:16

Oh, Joy of Joys! As we speak, little fine bits of foil confetti are lazily floating down to the floor in my workspace! Not sure if if was the extra drying, or the more aggressive confinement suggested, but I got nice high order dets now. Still not sure how that one guy on YT (https://youtu.be/ETs1pkz1Umk) got his to det, open on a piece of foil, but I guess the fact that it deos not go off ease with a hammer, or from simple heating of small amounts is a GOOD thing. I also made a small straw with around 60 mg of ETN and 15 mg of SADS and that went off nicely too. I guess it worked. Yield has a little room for improvement I guess. In my reX I also added some urea, I hope that works well. So far testing neutral with a moist litmus. Will retest every week or so.

Speaking of that, it makes more sense to me to add the urea or whatever stab you are using in the solvent (EToH in my case). That way it has time to work. I've seen others adding it in the crash solution. But in that case it wouldn't have vary long to act before new crystals are formed, seems to me...?

[Edited on 10-4-2019 by twelti]

underground - 10-4-2019 at 01:06

Quote: Originally posted by C6(NO2)5CH2CH(CH3)N(NO2)2  
If it detonated even once, then I think you've got some ETN! The yield may not be as good as it could be, but you succeeded, I think. The rest would probably go if it was dry and was triggered by a primary.

Now my own (probably dumb) question. Has anyone recovered H2SO4 from a nitration? Or is that just an altogether bad idea (eg. traces of explosive product)


I was thinking about the same and i have made a topic about this subject. My idea was to use AN/H2SO4 for nitration. After crashed and filtered, the water will contain h2so4/ammon. sulphate maybe AN and unnitrated / partly-nitrated esters. During concentration of crude h2so4 all ammonia salts would evaporate and the remaining unreacted esters would become carbon. In theory you will end with concentrated h2so4 with a little bit of carbon. I dont thik so carbon would have any effect in final yields

Herr Haber - 10-4-2019 at 03:39

Quote: Originally posted by C6(NO2)5CH2CH(CH3)N(NO2)2  

Now my own (probably dumb) question. Has anyone recovered H2SO4 from a nitration? Or is that just an altogether bad idea (eg. traces of explosive product)


Depending what you plan to do with that H2SO4 it might be a bad idea.
Spent acid from TNT manufacture can be fortified again and used for the mono nitration.
Spent acid from nitroglycerine is mostly useless.

Urbanski should give you a few good ideas of what is doable but in most lab setups it's not practical to recover the spent acid.

Laboratory of Liptakov - 12-4-2019 at 12:32

For example was tested using nitration mixture firstly for nitrocellulose (14%N) and follow for ETN with yield 50%. Because NC is possible get out as one piece of material of out.

FeedMe94 - 13-4-2019 at 07:13

I was looking for a synthesis for nitration of erythritol and im a bit confused. The one synthesis i found was : 185ml of 68% Nitric Acid + 270ml Sulfuric Acid 96 + 75g erythritol and the other was 395 grams ( not ml ) NA 68% + 756 grams of SA 96%
+ 75 grams of erythritol. Any help about how should i proceed ?

Laboratory of Liptakov - 13-4-2019 at 11:18

60 ml H2SO4 (96%) 40 ml HNO3 (65 - 68%) + 10g E. = 300 ml Nitric Acid + 450 ml Sulfuric Acid + 75g E. 1 ml SA = 1,85g
1 ml NA = 1,4g. On 10g E we need 111g SA + 56g NA. From this can be output 21 - 22g pure recrystallized ETN.

FeedMe94 - 13-4-2019 at 11:39

Quote: Originally posted by Laboratory of Liptakov  
60 ml H2SO4 (96%) 40 ml HNO3 (65 - 68%) + 10g E. = 300 ml Nitric Acid + 450 ml Sulfuric Acid + 75g E. 1 ml SA = 1,85g
1 ml NA = 1,4g. On 10g E we need 111g SA + 56g NA. From this can be output 21 - 22g pure recrystallized ETN.


Thank you very much Dr. My head was a mess before that

Laboratory of Liptakov - 13-4-2019 at 12:09

OK.....:cool:....PE is possible dissolve in NA only, and drop this transparent solution into SA. Advantage 1: Nothing crushing PE before adding into NA+SA mixture. Advantage 2: Comfort adding, maximal yield. For E is this process impossible. Arises zero yield....:cool:...LL

FeedMe94 - 16-4-2019 at 04:47

I recrystalized my ETN using acetone. When i poured it into ice water the ETN participated as big chunks and not flour consistency as before. Does it look ok ?

https://ibb.co/dB0mYDS

By the way whats ETN solubility in acetone cause i may use too much

Laboratory of Liptakov - 16-4-2019 at 12:24

Best results are usually from methanol, because has ideal solubility effect and because is usually pure. Ethanol contents impurities against consumation and acetone also contents impuritires, usually some as the fat. Pure ETN should by look as mica platelets.

FeedMe94 - 16-4-2019 at 23:42

Quote: Originally posted by Laboratory of Liptakov  
Best results are usually from methanol, because has ideal solubility effect and because is usually pure. Ethanol contents impurities against consumation and acetone also contents impuritires, usually some as the fat. Pure ETN should by look as mica platelets.


I used acetone because its 99.9%. I cannot obtain methanol and the ethanol i have is 95%

FeedMe94 - 18-4-2019 at 13:25

Tomorrow I'm going to try some Red Phosphorus with KCLO4 , KCLO3 , KMnO4 and NH4NO3 mixtures. Ofcourse not more than 100mg each. Could you give me some ratios please? I know for KCLO4 and KCLO3 is 70/30.

underground - 15-5-2019 at 13:41

Which one is more sensitive urea nitrate or ANFO ? If UN is more sensitive, with what energetic its sensitivity can be compared ?

FeedMe94 - 15-5-2019 at 20:47

Quote: Originally posted by underground  
Which one is more sensitive urea nitrate or ANFO ? If UN is more sensitive, with what energetic its sensitivity can be compared ?


Urea Nitrate
Melting Point: 152 ° C
Detonation velocity 3400 m/s at density
0.85 g/cm3
Lead block test 270 cm3
Impact Sensitivity: no reaction to 50 Nm
Friction Sensitivity: no reaction up to 353N

Nitrourea
(prepared by dehydration of urea nitrate with concentrated sulfuric acid)
Detonation velocity: up to 7000 m / s
Melting point: 159 ° C, decomposition
Lead block: 310 cm 3
Mildly sensitive to heat and shock

ANFO
Bulk density: 0.8 gr./cm3
Relative weight strength: 75%
Velocity of detonation: 3,000 m/sec
Strength (Trauzl Lead block test): 335 ml
Brisance (Hess test): 5,3 mm
Energy of explosion: 920 Kcal/Kg
Gas volume: 970 It/Kg
Explosion temperature: 2600oC
Friction sensitivity: >360N
Impact sensitivity: >50J



underground - 16-5-2019 at 11:52

So ANFO more sensivite than UN. Interesting.

Metallus - 23-5-2019 at 07:39

I'm interested in the chemistry (theory) behind the synthesis of RDX from methenamine + HNO3 and the reasons behind all the temperature adjustments during its synthesis or how impurities affect the synthesis (eg NOx concentration, presence of sulfates or other salts, etc).

It's likely that there is already a thread with all this information, but looking for it proved to be difficult, considering the huge mole of forum posts on this subject. Most posts are about the procedure or recipes, without an in-depth explanation of the reasoning behind all those parameters.

1) Patent US2859215A on RDX synthesis gives a temperature range between -10 and +40°C. Some other recipes found in the web employ an ice-salt bath (-30°C). What changes with the temperature? The reaction is exothermic, so with lower T the theoretical yield increases at the expense of kinetics. In this sense, I assume the suggested 20-30°C operational temperature is a compromise between thermodynamics and kinetics. Is that correct?

2) The addition of methenamine to WFNA has to be carried slowly. Is it because the reaction is dangerously exothermic and so it's necessary to let the mixture cool down a bit between each addition in order to easily maintain the temperature < 30°C?

3) After the two reactants are mixed, the temperature is quickly raised to 80°C. Is it to speed up the reaction? Why the temperature must be raised so quickly? What happens if it's raised gradually? Also why all that care to maintain it below 30°C in the first step if then you have to quickly raise the temperature?

4) In order to precipitate the RDX crystals, the acid mixture is washed with cold water. Is it to counter the exothermic reaction between the leftover HNO3 and water? Or is it to more easily allow the precipitation of the crystals? Or both?

5) How do impurities affect the reaction? Especially NOx dissolved in HNO3 or the presence of sulfates or other salts.

6) What is the most critical and dangerous step of this synthesis and why?

Thanks

Simoski - 23-5-2019 at 11:20

Are any copper salts fat soluble?

May not seem like an energetic material type of question, but if there are any I will disolve it is lard or tallow, add potassium chlorate and have me a new blue / green pyrotechnic star mix



[Edited on 23-5-2019 by Simoski]

Laboratory of Liptakov - 23-5-2019 at 11:40

You can use caramelit...... https://www.youtube.com/watch?v=nMfCzjMLz3w ......:cool:...LL

Simoski - 23-5-2019 at 11:49

Quote: Originally posted by Laboratory of Liptakov  
You can use caramelit...... https://www.youtube.com/watch?v=nMfCzjMLz3w ......:cool:...LL


I will, thanks LL, will make great flare mix!

Daffodile - 23-5-2019 at 17:25

Does anyone know a viable way to remove the methoxy and acetyl groups without having to reattach the amino group?

I really don't know where to go here and any help would be hugely appreciated.


Aniline.jpg - 8kB

MineMan - 7-6-2019 at 06:25

What type of propellant do you think is being used? The brown smoke in the beginning I believe is from metal oxides.... but the thick white smoke seems peculiar... ?

Any chance they are using a EM we are not familiar with in the west.... my understanding is the Russians are ahead in explosive science.

https://www.foxnews.com/world/see-it-russia-test-launches-ne...
And here is a better video.

https://m.youtube.com/watch?v=qLV1Ao9QkpE

[Edited on 7-6-2019 by MineMan]

maldi-tof - 16-6-2019 at 13:58

Quote: Originally posted by Simoski  
Are any copper salts fat soluble?

May not seem like an energetic material type of question, but if there are any I will disolve it is lard or tallow, add potassium chlorate and have me a new blue / green pyrotechnic star mix



[Edited on 23-5-2019 by Simoski]


Should organocopper compounds do the trick?

Boffis - 17-6-2019 at 12:58

I have noticed that some old primary charges in detonators etc contain lead thiocyanate. I have made a little of this compound and it is not the least bit energetic so what is its purpose in these compositions? An exotic fuel?

underground - 20-6-2019 at 08:33

From wikipedia

"Lead(II) thiocyanate is a compound, more precisely a salt, with the formula Pb(SCN)2.It is a white crystalline solid, but will turn yellow upon exposure to light. It has use in small explosives, matches, and dyeing. Like other metal cyanides, Lead thiocyanate explodes on heating when mixed with sodium nitrite. Lead thiocyanate is used in explosives, specifically an ingredient in primers for small-arms cartridges, safety matches, and to reverse aniline black dyeing (Gideon)."

underground - 21-6-2019 at 12:17

I just found few AAAA Batteries from few 9v Batteries. I want to use their cases for caps, anyone have any idea how to remove everything and clean them inside ? It looks quite tricky.

James Ikanov - 26-7-2019 at 14:00

Quote: Originally posted by underground  
I just found few AAAA Batteries from few 9v Batteries. I want to use their cases for caps, anyone have any idea how to remove everything and clean them inside ? It looks quite tricky.


What kind of 9V battery? Do the AAAA's have tabs welded together between them?

C6(NO2)5CH2CH(CH3)N(NO2)2 - 5-8-2019 at 15:55

I have been reading about chlorate based explosives in Chemistry of Powder and Explosives by Tenney Davis. I noticed that sodium chlorate based compositions were said to be slower and less powerful than their potassium counterparts. That is inspite of sodium chlorate having similar heat of decomposition to potassium chlorate, and 11 or 12% more oxygen per unit mass.

Were the sodium chlorate mixtures damp, or is their some other factor I am not taking into account here?

Laboratory of Liptakov - 6-8-2019 at 12:07

Sometimes energetics materials behave strangely, despite assumptions based on their basic properties. Nothing humidity of NaClO3. Similarly as ice which is lighter than water. And only attempt and watching showes the truth...:cool:...LL

underground - 6-8-2019 at 16:03

Quote: Originally posted by James Ikanov  
Quote: Originally posted by underground  
I just found few AAAA Batteries from few 9v Batteries. I want to use their cases for caps, anyone have any idea how to remove everything and clean them inside ? It looks quite tricky.


What kind of 9V battery? Do the AAAA's have tabs welded together between them?


Here is an example



[Edited on 7-8-2019 by underground]

snooby - 8-10-2019 at 15:41

Can i make basic cobalt carbonaten from the nnitrate? I cant Find a supplier..

Microtek - 8-10-2019 at 22:22

It seems likely that the basic carbonate has a rather low solubility and that the nitrate has a high solubility. If that is the case it is probably quite easy to do a simple metathesis, although you may need to adjust pH.

Herr Haber - 6-11-2019 at 04:11

I currently have a disagreement with people working in the oil industry but I trust Sciencemadness a bit more on this. Specifically since some of you have done this kind of fractionnal distillation.

Is there or is there not benzene (C6H6, I know there is toluene, xylenes and others) in diesel fuel ?

Specifically diesel fuel. I know it's present in crude and in regular gasoline. Any details will be welcome.

markx - 7-11-2019 at 01:08

As far as I can perceive the continuous fractionation process used for crude oil separation, there is in principle no possibility or completely removing components via this method or getting a very delicate separation. And it is not really needed for the end purpose of the oil industry.
The feed is entering the tower at about middle height and then proceeds to reditribute itself on the plates under reflux according to boiling points of the fractions. Inexorably the components of the mix have to move through the plates in the column continuously since the feed is entering the column continuously. Thus the fractions taken off from the various plates are always somewhat contaminated with the components that are still migrating through the column to "find their place in the system".
On the other hand a batch fractionation has no constant infeed and therefore one can deplete the boiler contents one by one according to rising boiling points as far the separation of the column allows for it. Thus a much finer separation of components can be achieved.

But of course the continuous fractionation of crude oil is not the only method that is used in oil refining and I'm sure it is possible to separate benzene from diesel fuel by other means if needed to do so.

Hydrogen peroxide / urea

underground - 10-11-2019 at 11:50

Has anyone any expirience with ?

https://en.m.wikipedia.org/wiki/Hydrogen_peroxide_-_urea

It is not a primary but can be detonated. I have no idea for its properties, sensitivity VoD e.t.c. It may be a good way to use some peroxide.

Bert - 11-11-2019 at 20:31

Quote: Originally posted by underground  
Has anyone any expirience with ?

https://en.m.wikipedia.org/wiki/Hydrogen_peroxide_-_urea

It is not a primary but can be detonated. I have no idea for its properties, sensitivity VoD e.t.c. It may be a good way to use some peroxide.


No experience, but I was interested when I first learned of this too.

From the fact you can ship an lb. of it without HazMat fees in the US mail, I would guess it's pretty insensitive...

https://www.firefox-fx.com/ChemU-Z.htm

underground - 12-11-2019 at 02:34

Quote: Originally posted by Bert  

No experience, but I was interested when I first learned of this too.

From the fact you can ship an lb. of it without HazMat fees in the US mail, I would guess it's pretty insensitive...

https://www.firefox-fx.com/ChemU-Z.htm


Yea, it is actually a mixture of urea and 100% HP by 1:1 Not even a new material. I guess it would be at the range of +5000m/sec VoD and seems like a good way to use some HP. Most of the peroxides are super sensitive but UHP is not.



[Edited on 12-11-2019 by underground]

Herr Haber - 12-11-2019 at 04:44

Quote: Originally posted by markx  
As far as I can perceive the continuous fractionation process used for crude oil separation, there is in principle no possibility or completely removing components via this method or getting a very delicate separation. And it is not really needed for the end purpose of the oil industry.
The feed is entering the tower at about middle height and then proceeds to reditribute itself on the plates under reflux according to boiling points of the fractions. Inexorably the components of the mix have to move through the plates in the column continuously since the feed is entering the column continuously. Thus the fractions taken off from the various plates are always somewhat contaminated with the components that are still migrating through the column to "find their place in the system".
On the other hand a batch fractionation has no constant infeed and therefore one can deplete the boiler contents one by one according to rising boiling points as far the separation of the column allows for it. Thus a much finer separation of components can be achieved.

But of course the continuous fractionation of crude oil is not the only method that is used in oil refining and I'm sure it is possible to separate benzene from diesel fuel by other means if needed to do so.


Thanks Marks.
That answers and goes beyond my question.

In the meantime I found this very interesting paper:
https://www.researchgate.net/publication/288133039_The_compo...

Quite interesting to compare the results of what goes in the tanks with what comes out of the exhaust.

Hydrogen Peroxide Urea can haz detonations?

Bert - 12-11-2019 at 05:02

On a quick look, someone thinks this is a "sleeper", awaiting the first major industrial accident where regulators are forced to notice that yes, indeed, it can go "boom"- As was ammonium nitrate before the Oppau disaster and nitro methane before the two 1958 Niagara NY and Pulaski IL railroad tank car explosion disasters.

https://onlinelibrary.wiley.com/doi/abs/10.1002/prep.2016001...

Quote:

It is not sensitive to impact and friction. However, we demonstrated that UHP (ρ=0.93 g cm−3; packed into a steel pipe with inner diameter of 206 mm) detonates with experimental velocity of detonation (VOD) of 3780 m s−1. Moreover, for UHP with maximal theoretical density (ρ=1.43 g cm−3), the calculated VOD reaches 5219 m s−1. Based on our findings, we recommend that present regulations regarding the handling, storage and transportation of the UHP should be revised, especially in cases, where UHP is kept on a large scale, under confinement and at places where the temperature can reach above 60 °C.


From other information on industrial uses, I suspect that a sample of this contaminated with a suitable decomposition catalyst (Sodium tungstate?) might be more inclined towards "friskiness".



[Edited on 11-12-2019 by Bert]

[Edited on 11-12-2019 by Bert]

MineMan - 12-11-2019 at 22:49

Quote: Originally posted by Bert  
On a quick look, someone thinks this is a "sleeper", awaiting the first major industrial accident where regulators are forced to notice that yes, indeed, it can go "boom"- As was ammonium nitrate before the Oppau disaster and nitro methane before the two 1958 Niagara NY and Pulaski IL railroad tank car explosion disasters.

https://onlinelibrary.wiley.com/doi/abs/10.1002/prep.2016001...

Quote:

It is not sensitive to impact and friction. However, we demonstrated that UHP (ρ=0.93 g cm−3; packed into a steel pipe with inner diameter of 206 mm) detonates with experimental velocity of detonation (VOD) of 3780 m s−1. Moreover, for UHP with maximal theoretical density (ρ=1.43 g cm−3), the calculated VOD reaches 5219 m s−1. Based on our findings, we recommend that present regulations regarding the handling, storage and transportation of the UHP should be revised, especially in cases, where UHP is kept on a large scale, under confinement and at places where the temperature can reach above 60 °C.


From other information on industrial uses, I suspect that a sample of this contaminated with a suitable decomposition catalyst (Sodium tungstate?) might be more inclined towards "friskiness".



[Edited on 11-12-2019 by Bert]

[Edited on 11-12-2019 by Bert]


Yes, Bert thus has been on my radar too... was actually hoping it wouldn’t pop up on the form because it is essentially a insensitive secondary that can be shipped without any ATF or hazmat.... afraid even posting on here can change that. I thought it would have good potential for a binary... such as mixed with NM. 5200m/s isn’t too bad. And it’s cheap too! So wish thus was still my secret, but cats out of the bag!

Bert - 13-11-2019 at 20:47

Nitromethane is a tad low on Oxygen. The urea peroxide is too.

How 'bout trying it in a mixture with an oxidizer or an oxygen positive HE.

In very small quantities, mind you!

My first thought was how it might behave towards admixture of a nice thin NC/NG jelly. My second thought was, I like my hands too much to find out.

Microtek - 17-11-2019 at 23:32

I experimented with urea peroxide many years ago. The synthesis was easy and high yielding, and the product was surprisingly insensitive. It burned in a manner that made me think "propellant" so I experimented a little with it as an alternative to NC.

Bert - 18-11-2019 at 06:07

Quote: Originally posted by Microtek  
It burned in a manner that made me think "propellant" so I experimented a little with it as an alternative to NC.


Did you get it to perform in a rocket motor? The source I posted is, of course, a high power rocketry materials supplier.

MineMan - 18-11-2019 at 11:34

Quote: Originally posted by Microtek  
I experimented with urea peroxide many years ago. The synthesis was easy and high yielding, and the product was surprisingly insensitive. It burned in a manner that made me think "propellant" so I experimented a little with it as an alternative to NC.


Alternative to NC... so can it be used as a binder?

ETN vs PETN

underground - 26-12-2019 at 09:43

I did some tests with both ETN and PETN and for some reason, ETN was always more powerfull-brisant than PETN. ETN got a few % of vaseline too. The containers were exactly the same and i hand-pressed them as much as i could. I thought PETN was more powerfull but ETN just did more damage and penetrate even further. It was a small scale test like 4g, maybe ETN is more bristant than PETN but PETN may be better in bigger quantities.



[Edited on 26-12-2019 by underground]

Microtek - 27-12-2019 at 08:28

Have you checked the purity of the two? Melting point and TLC are good places to start.

underground - 27-12-2019 at 10:49

I just remembered that PETN was not recrystallized while ETN was. I just recrystallized a few gr of PETN and now it's drying. I will give it a try again.

Methylhydrazine as a ligand?

georgef2545 - 6-1-2020 at 06:29

I appreciate that methylhydrazine, dimethylhydrazine etc are horrible flammable and toxic, react hypergolically with oxidisers, but I was wondering if using it as a ligand in a metal complex explosive would make a good primary explosive? For example complexing it with nickel nitrate or chlorate?

I do acknowledge that organohydrazine compounds are often very dangerous and this is probably stupid.

Herr Haber - 6-1-2020 at 07:43

Quote: Originally posted by georgef2545  
I appreciate that methylhydrazine, dimethylhydrazine etc are horrible flammable and toxic, react hypergolically with oxidisers, but I was wondering if using it as a ligand in a metal complex explosive would make a good primary explosive? For example complexing it with nickel nitrate or chlorate?

I do acknowledge that organohydrazine compounds are often very dangerous and this is probably stupid.


Search the forum for nickel hydrazine nitrate / perchlorate
You'll see there is quite a lot of interesting compounds in addition to NHN.

FeedMe94 - 7-3-2020 at 07:15

Is there any subreddit for energetic materials?

B(a)P - 7-3-2020 at 11:19

Quote: Originally posted by FeedMe94  
Is there any subreddit for energetic materials?


The youtube channel explosions and fire has one r/ExplosionsAndFire

B.D.E - 14-3-2020 at 13:07

nevermind, please delete.
apologies.

[Edited on 14-3-2020 by B.D.E]

Brightthermite - 21-3-2020 at 19:59

Could not find this in any of the other threads, is ETN hygroscopic at all? Has anyone else had experience with it taking multiple days to dry? Humidity was below 60 % and other things dry just fine.

Detonating Tannerite/Ammonal

Katie - 15-4-2020 at 11:50

Hi, long time lurker first time poster here!

Can ammonium nitrate / aluminum powder (Tannerite/Ammonal) be detonated with dextrinated lead azide? I’m using commercial brand Tannerite©. Also, will this be effective in clearing tree trunks and boulders (with tannerite filled boreholes).

I cannot test anything safely in my current location, but I have a vacation home. Unfortunately, I need to blast in the woods and I can’t be at a safe distance without losing my sight line, so detonating it with a 5.56 round isn’t an option.

I’ve made 2g dex. lead azide blasting caps based on commercial
cap design. This is my first post so I’ll mention that I have taken an explosives safety course approved by ISEE and have lab experience as well. I use electric blasting caps and a remote firework igniter so I can be at least 100 meters away from any explosion, with surrounding trees completely on securing the blast site. I’ve also gone through my “kewl bombz” phase when I was younger, and now my interests are in the synthesis and testing of energetic materials. I hope to eventually work as a chemical engineer designing products that use energetic materials.

Etanol - 17-4-2020 at 06:25

Quote: Originally posted by Katie  
Hi, long time lurker first time poster here!
Can ammonium nitrate / aluminum powder (Tannerite/Ammonal) be detonated with dextrinated lead azide?
...
I’ve made 2g dex. lead azide blasting caps based on commercial
cap design.


Yes of course.
What is the density of your lead azide in the blasting cap? Is it more than 2,0 g/cm3 ?

MineMan - 18-4-2020 at 15:47

Quote: Originally posted by Katie  
Hi, long time lurker first time poster here!

Can ammonium nitrate / aluminum powder (Tannerite/Ammonal) be detonated with dextrinated lead azide? I’m using commercial brand Tannerite©. Also, will this be effective in clearing tree trunks and boulders (with tannerite filled boreholes).

I cannot test anything safely in my current location, but I have a vacation home. Unfortunately, I need to blast in the woods and I can’t be at a safe distance without losing my sight line, so detonating it with a 5.56 round isn’t an option.

I’ve made 2g dex. lead azide blasting caps based on commercial
cap design. This is my first post so I’ll mention that I have taken an explosives safety course approved by ISEE and have lab experience as well. I use electric blasting caps and a remote firework igniter so I can be at least 100 meters away from any explosion, with surrounding trees completely on securing the blast site. I’ve also gone through my “kewl bombz” phase when I was younger, and now my interests are in the synthesis and testing of energetic materials. I hope to eventually work as a chemical engineer designing products that use energetic materials.


Why LA... so many safer options. Which ISEE course.... are you a student?

How are you going to drill the boreholes. And lastly... why tannerite... think OB.

Katie - 21-4-2020 at 16:45

Quote: Originally posted by MineMan  
Quote: Originally posted by Katie  
Hi, long time lurker first time poster here!

Can ammonium nitrate / aluminum powder (Tannerite/Ammonal) be detonated with dextrinated lead azide? I’m using commercial brand Tannerite©. Also, will this be effective in clearing tree trunks and boulders (with tannerite filled boreholes).

I cannot test anything safely in my current location, but I have a vacation home. Unfortunately, I need to blast in the woods and I can’t be at a safe distance without losing my sight line, so detonating it with a 5.56 round isn’t an option.

I’ve made 2g dex. lead azide blasting caps based on commercial
cap design. This is my first post so I’ll mention that I have taken an explosives safety course approved by ISEE and have lab experience as well. I use electric blasting caps and a remote firework igniter so I can be at least 100 meters away from any explosion, with surrounding trees completely on securing the blast site. I’ve also gone through my “kewl bombz” phase when I was younger, and now my interests are in the synthesis and testing of energetic materials. I hope to eventually work as a chemical engineer designing products that use energetic materials.


Why LA... so many safer options. Which ISEE course.... are you a student?

How are you going to drill the boreholes. And lastly... why tannerite... think OB.


The ISEE course was their practical blasting fundamentals course as well as online certificate program. They are great safety classes but mainly focused on safely using commercial explosives in mining and construction rather that the chemistry behind everything.

I chose dextrinated LA because the reagents were readily available to me and because it has been used in commercial blasting caps. Tannerite because I have a lot of it for target shooting. What are the safer alternatives for an initiator? I’d like to know for future projects as I will probably make this a hobby. For the boreholes I have a 1” and 2” by 16” long drill bit and a large two hand power drill. I believe the 1” is a stone bit designed to work with the hammer drill function. I know they will work on wood but drilling the natural stone will be interesting.

I’m no longer a student but I’ve taken 2 years of general and organic chemistry as well as 2 years of lab based general chemistry, orgo, biology, and physics courses. I took the ISEE courses in preparation of getting my federal and state explosives manufacturing license for fireworks and black powder.

I’m definitely interested in the safest primaries that can be made from chemicals available online that will ship to individuals (or synthesized with hot plates and glassware). So please give me some suggestions!

“Best” primaries

Katie - 21-4-2020 at 17:36

What do YOU think the “best” primary is in terms of safety, stability, and ease of synthesis? I recently made dex. lead azide but I understand there are safer alternatives out there that are just as easy to make and just as effective. I’ve seen many mentioned on these forms but I’m having trouble deciding on which one to use to create a supply of blasting caps that will be stored for up to a year before use (in a proper magazine, of course!)

B(a)P - 22-4-2020 at 01:27

Quote: Originally posted by Katie  
What do YOU think the “best” primary is in terms of safety, stability, and ease of synthesis? I recently made dex. lead azide but I understand there are safer alternatives out there that are just as easy to make and just as effective. I’ve seen many mentioned on these forms but I’m having trouble deciding on which one to use to create a supply of blasting caps that will be stored for up to a year before use (in a proper magazine, of course!)


There are a few really good threads on this already.
https://www.sciencemadness.org/whisper/viewthread.php?tid=99...
https://www.sciencemadness.org/whisper/viewthread.php?tid=81...
https://www.sciencemadness.org/whisper/viewthread.php?tid=25...

I would also recommend checking out threads on NHN and CHP

https://www.sciencemadness.org/whisper/viewthread.php?tid=15...
Also search for CHP by Laboratory of Liptakov you can also check out their youtube channel

Katie - 26-4-2020 at 19:14

Thank you everyone for the replies and I apologize for the redundant thread. I’m new here and not used to working with search engines that don’t have all the magic that google has!

MineMan - 29-4-2020 at 07:40

Where is the thread discussing silicone as an alternative to PIB for ETN... ? I think it was discussed recently.

FeedMe94 - 13-5-2020 at 05:55

Is there a way to remove impurities from SADS?

darolf26 - 31-5-2020 at 03:48

Are there any usable primaries containing KClO3 ?
I heard of K3(CN)6Fe mixtures and Armstrong’s mix for insane guys.”, but are there any other.

j_sum1 - 31-5-2020 at 04:17

Quote: Originally posted by darolf26  
Are there any usable primaries containing KClO3 ?
I heard of K3(CN)6Fe mixtures and Armstrong’s mix for insane guys.”, but are there any other.

I'm no EM expert but I do have some (negative) experience with Armstrong's mix.
My understanding is that chlorates are to be avoided. While they have historical significance, I believe in every application they have been hazardous and have been superceded by compounds that are less twitchy and perform better.

Someone more knowledgeable will be by soon to confirm or correct me.

Herr Haber - 31-5-2020 at 11:34

Quote: Originally posted by darolf26  
Are there any usable primaries containing KClO3 ?
I heard of K3(CN)6Fe mixtures and Armstrong’s mix for insane guys.”, but are there any other.


10% with mercury fulminate

Explosive Storage

Brightthermite - 25-6-2020 at 15:02

Is there a threaded dedicated to the storage of explosives and the likes of? Such as container designs and ideas on how to store multiple detonators. If not would there be and interest in starting one?

monolithic - 25-6-2020 at 18:52

Are there any good books that cover practical syntheses and applications of energetic materials? I've downloaded a few books but they're more general and academic in nature. They don't discuss practical considerations like weight ratios for AMMONAL and the importance of aluminum mesh sizes; PLX type energetics, etc.

RogueRose - 26-6-2020 at 07:20

Quote: Originally posted by monolithic  
Are there any good books that cover practical syntheses and applications of energetic materials? I've downloaded a few books but they're more general and academic in nature. They don't discuss practical considerations like weight ratios for AMMONAL and the importance of aluminum mesh sizes; PLX type energetics, etc.


I second this. I was looking for some good books on this and some books, manuals or guides on fireworks from fire crackers to mortars to rockets. I'd be interested in all of them.

Belowzero - 26-6-2020 at 07:27

Urbanski has lot of good info, in depth stuff.
Problem with many of the practical books is that they tend to lean towards cooking instead of science.

This is such an example: http://index-of.es/Miscellanous/Field%20Manufactured%20Explo...

Also a lot of material here: http://pyrobin.com/files.php



[Edited on 26-6-2020 by Belowzero]

aromaticfanatic - 6-10-2020 at 17:28

Quote: Originally posted by FeedMe94  
Is there any subreddit for energetic materials?


Yes my friends and I run one.

r/energetics

mekanochemical - 15-12-2020 at 06:37

hello, is it possible to synthetize cobalt and manganese nitrate from the oxides? I didnt find carbonates.

Thanks

Etanol - 15-12-2020 at 11:49

Is exists Cu acetylenide-nitrate? Bubnov "initiating explosives" written : under the action of acetylene on copper salts in acidic solutions, double compounds of acetylene with copper salts are formed.
Sorry, I don t find Thread with Acetylenides

B(a)P - 15-12-2020 at 13:59

Quote: Originally posted by mekanochemical  
hello, is it possible to synthetize cobalt and manganese nitrate from the oxides? I didnt find carbonates.

Thanks


Manganese nitrate is possible from the oxide not sure about cobalt.
Nurdrage did a good video on it.
https://www.youtube.com/watch?v=KSIeCbv4jlM
For cobalt I think you could try nitric acid directly with oxide.

Hey Buddy - 4-1-2021 at 00:50

Does anyone know of any research of urea condensation derivative explosives beyond biuret? Particularly triuret, tetrauret and pentauret? Nitrate salts, amines or perchlorates? I've looked, can't find anything. Closest I've found is mentions of tetra and penta in ag patents which only mention them as unwanted byproducts. I can't even locate methods to isolate them out of batch condensation. The only thing I've found related to separating is biuret, via solubility in H20

[Edited on 4-1-2021 by Hey Buddy]

Jome - 4-1-2021 at 01:47

If I'm going to use CaCl2 to help separating an ester from remaining alchohol, will presence of MgCl2 have any negative effect? When I look for solubilities I find that with EtOH, both CaCl2 and MgCl2 are soluble, though MgCl2 less so.

teodor - 4-1-2021 at 07:13

As far as I know "Calcium chloride combines with alcohols, phenols, amines, amino-acids, amides, ketones, and some aldehydes and esters, and thus cannot be used with these classes of compounds." (citation from Vogel).
See also https://chemistry.stackexchange.com/questions/84921/why-cant...
So, why not MgSO4?
I tried to use CaCl2 for separation of n-butyl eTHer, but without success.

Some (most?) esters are not soluble in saturated NaCl but EtOH & MeOH are soluble.


[Edited on 4-1-2021 by teodor]

Jome - 5-1-2021 at 01:56

I was referring to the use of CaCl2-solution specifically to remove remaining lower mw alcohols, like isopropyl and ethyl alcohol, like f.ex here

Sorry if I was unclear. There is for some unknown reason roughly half or so MgCl2 in the commonly avaliable "dehumidifier ball" powder bags in my little country, and it would be convenient not having to separate the CaCl2 from this, iff it'd work in procedures such as the above.

ETN Smell

Brightthermite - 16-1-2021 at 20:06

Can anyone describe what there ETN smells like? Mine after multiple washing and 2 recyst still has a slight vinegar odor to it when left in a sealed container, which makes me a bit uneasy. No noticeable signs of decompositions or fumes after several months tho.

Laboratory of Liptakov - 18-1-2021 at 06:04

Yes, pure ETN has slight smell always a like vinegar. After one year is smell a same. Without changes of properties. Very slightly smell, but yes, is there.

Jebby - 11-3-2021 at 06:49

Anyone here know how an average Joe could get an explosives manufacturer permit or license? I have read federal laws and from my understanding you have to have an actual lab or warehouse and a catalog of what you make and how much. I only ask because I think energetic materials would be an awesome career to pursue, but if anyone here has experience that says otherwise I’m all ears.

MineMan - 14-3-2021 at 03:57

Jebby

You apply.... get to know the local agents

densest - 15-3-2021 at 13:16

In the US: The biggest concern seems to be keeping the product, precursors and preparation area under strict supervision and "good citizen" operators to prevent product leaving the factory/storage/authorized users. Technical competence 2nd.

Some substances are exempt under some (very small) quantity limits or have tiers of requirements. This changes from time to time.

Expect to need storage magazine built to spec. There's a pamphlet from ex-BATF. Walls, locks, doors, floors, etc. Also distance from habitations - can be many (50? more?) yards/meters and inspected every 3 days. Production area has other requirements. Both must either be in regular use or frequently inspected. Some agencies will accept remote video, etc. monitoring. Alarm systems have to meet requirements and opinions. Strict records of quantities in, out, used, destroyed. Some substances must be traced at gram level.

Personal Type 20 license for at least low (gunpowder, firework stars, etc) dunno what type for high exp. Requirements are online.

In the US expect Federal, State, and local supervision. Differs from state to state: some it's under fire marshal, some it's under police. Any of them can be very nice ----- until you mess up. They get very upset. Get letters from the agencies involved giving their opinions about your setup.

All this -can- be met with planning and care with simple and (relatively) inexpensive work areas. Check with fireworks clubs - they don't do high explosives but many of the legal requirements are the same.

Association with the New Mexico School of Mines would be a big plus. They do lots of research.

Canada varies by province. I expect some places it's impossible.
Europe? Probably more strict - finding a site with sufficient separation might be a problem.

Asia/S.America/Central Am/Mexico? no clue

krot - 9-4-2021 at 13:13

Is it possible for a partial detonation to occur with ammonal (AN/AL) if too little booster is used? (ETN in my case)
P.S. I have planned 10 kg of ammonal

Johnny Cappone - 10-4-2021 at 08:42

Is the [Cu(NH3)3]+ ion also called tetraamminecopper? This would be the complex formed by ammonia and Cu (I).
I researched several sources and almost couldn't find anything about it, maybe it's just the cuprous tetramine complex and I'm just stupid.
By the way, in english are oxidation states pronounced as numerals? That is, can I pronounce Cu (II) as "copper two"?

outer_limits - 10-4-2021 at 09:39

How can it be tetraminecopper as there are only three, not four amine groups?

Johnny Cappone - 10-4-2021 at 09:47

Quote: Originally posted by outer_limits  
How can it be tetraminecopper as there are only three, not four amine groups?


I realized this right after posting, but I was too lazy to point out my reasoning failure and hoped that no one would notice (a silly hope, given the number of skilled chemists here). However, my doubt still persists. What is this complex called? Triamminecopper?

DraconicAcid - 10-4-2021 at 09:49

Quote: Originally posted by Johnny Cappone  
Is the [Cu(NH3)3]+ ion also called tetraamminecopper? This would be the complex formed by ammonia and Cu (I).
I researched several sources and almost couldn't find anything about it, maybe it's just the cuprous tetramine complex and I'm just stupid.
By the way, in english are oxidation states pronounced as numerals? That is, can I pronounce Cu (II) as "copper two"?

If you react ammonia with Cu(I), I'm pretty sure you get [Cu(NH3)2]+, diamminecopper(I) ions.
And, yes, they are pronounced as numerals, so copper(II) chloride is pronounced copper-two chloride. When you're typing it, there's no space between the copper and the bracket, so it's copper(II), not copper (II) or copper ( ii ).

Yes, I teach intro chemistry- how did you guess?

Johnny Cappone - 10-4-2021 at 10:40

Quote: Originally posted by DraconicAcid  
If you react ammonia with Cu(I), I'm pretty sure you get [Cu(NH3)2]+, diamminecopper(I) ions.
And, yes, they are pronounced as numerals, so copper(II) chloride is pronounced copper-two chloride. When you're typing it, there's no space between the copper and the bracket, so it's copper(II), not copper (II) or copper ( ii ).

Yes, I teach intro chemistry- how did you guess?


Thank you, Draconic Acid!
I have been reading some literature on copper acetylide recently. An ammoniacal solution of a cuprous salt - typically, chloride - is often used in the synthesis of this compound (or as a test for the presence of acetylene). Some doubts arose and, among them, the name of the complex formed was the only one that I was unable to answer alone. Thank you again!

Johnny Cappone - 10-4-2021 at 20:33

What is the role of oxygen and other oxidizing agents in the oxidation of CuCl to CuCl2?

Today I experimented with cuprous chloride emulsions in water and, at one point, reacted this solution with hydrogen peroxide. As expected, H2O2 was decomposed with a large production of O2 and the whitish CuCl solution turned green, indicating the formation of CuCl2. I started to think about it.

I know that: CuCl <--> CuCl2 + Cu.

But I can't figure out how oxygen could help with that. In addition, I was wondering if peroxide promotes oxidation as a compound (H2O2) or if it is just a convenient source of oxygen when it is decomposed by copper, with the gaseous oxygen produced being responsible for the oxidation.

pyrochemsource.com

Elemental Phosphorus - 16-4-2021 at 09:48

Has anyone here used pyrochemsource.com?

I am about to place a pretty big order with them and was wondering if anyone has used them before. It looks fine, but I just wanted to check before I ordered. So does anyone have good/bad experiences with them?

Laboratory of Liptakov - 16-4-2021 at 11:09

You can try small testing order. It seems they have all. It seems a like dream for any researcher...:cool:

RogueRose - 16-4-2021 at 13:47

Quote: Originally posted by Elemental Phosphorus  
Has anyone here used pyrochemsource.com?

I am about to place a pretty big order with them and was wondering if anyone has used them before. It looks fine, but I just wanted to check before I ordered. So does anyone have good/bad experiences with them?


It looks like they are OK. They seem to also have an Amazon store:
https://www.amazon.com/s?k=Pyro+Chem+Source&ref=bl_dp_s_...

I also saw posts about the company going back at least 6 years, so I'm assuming it's legit. I didn't find any bad reviews or claims of a scam site. Their domain is almost 10 years old as well.

From everything I'm seeing, I think you will be safe ordering from them.

Elemental Phosphorus - 1-5-2021 at 11:02

Quote: Originally posted by RogueRose  
Quote: Originally posted by Elemental Phosphorus  
Has anyone here used pyrochemsource.com?

I am about to place a pretty big order with them and was wondering if anyone has used them before. It looks fine, but I just wanted to check before I ordered. So does anyone have good/bad experiences with them?


It looks like they are OK. They seem to also have an Amazon store:
https://www.amazon.com/sk=Pyro+Chem+Source&ref=bl_dp_s_w...

I also saw posts about the company going back at least 6 years, so I'm assuming it's legit. I didn't find any bad reviews or claims of a scam site. Their domain is almost 10 years old as well.

From everything I'm seeing, I think you will be safe ordering from them.




Well, today I just received my order from them, 7 pounds of different chemicals. It arrived on time, well packed and in a surprisingly compact container. The chemicals are packed in thick plastic bags, and they come in 2 of them. Here’s a photo of about half of the order:



80237284-C74E-4824-A255-C0C787E0E4BB.jpeg - 2.2MB


Edit: Also, I picked up that barium carbonate since it's a basic barium salt. Now that I have perchlorates I can prepare some perchloric acid and then make some barium perchlorate. I was intrigued by Laboratory of Liptakov's barium perchlorate primary, so with any luck I'll be able to do that experiment soon.

[Edited on 1-5-2021 by Elemental Phosphorus]

Laboratory of Liptakov - 3-5-2021 at 12:28

Barium perchlorate can be not reliable as primary. Was tested only a few attempts. Of course, interesting salt. But when you have NH4ClO4, you can do it easy TACP.
https://www.youtube.com/watch?v=cfOZfhwKHjg
It is reliable as primary. 1:1 with ETN works always. In solid cavity. TACP has OB + 14,5 on CO2. Therefore can be added some quality fuel. Especially hexamine. And arises popular CHP.
https://www.youtube.com/watch?v=F94UpYRczkc
CHP is primary and secondary 2 in 1. Has easy DDT from hot wire up to speed 7500m/s. And detonation pressure 25 GPa. Enough big pressure for starting any secondary material. Pure cast ETN has 31 GPa. But without easy DDT.
Any way, if you have NH4ClO4, you have fun for months and maybe years. It is a completely universal salt..Easy color flames of all colors, minimal smoke, differents salts with metals.
With NH4ClO4 is easy anything...:cool:

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