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Jebby
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Anyone know where I could find detailed information on the properties of ETN like at what temperature it DDT’s? I know where to look to find the
boiling and melting points.
I’m just trying to figure out how I could get ETN to detonate reliably by thermal decomposition without wasting a lot of it.
Nvm I Utfse
[Edited on 14-5-2021 by Jebby]
[Edited on 14-5-2021 by Jebby]
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MineMan
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Quote: Originally posted by Jebby  | Anyone know where I could find detailed information on the properties of ETN like at what temperature it DDT’s? I know where to look to find the
boiling and melting points.
I’m just trying to figure out how I could get ETN to detonate reliably by thermal decomposition without wasting a lot of it.
Nvm I Utfse
[Edited on 14-5-2021 by Jebby]
[Edited on 14-5-2021 by Jebby] |
It can’t just be a temperature. I would look into catayliztz
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ManyInterests
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(I was going to start a thread, but I figured it might be more appropriate to post my questions here).
So I have numerous questions regarding making nitrates and energetic materials. I just want to make very small batches of this stuff just as a proof
of concept and for fun. I am not experienced in making energetics except for black gunpowder and nitrocellulose, both of which I’ve made a few times
with great success (but no more than 10 grams of powder and 2 cotton balls at a time), and I wanted to try my hand at making small quantities of the
following: RDX, ETN, Picric acid, Ammonium Picrate, Nickel Hydrazine Nitrate, and (possibly) DDNP. I wanted to try to make PETN, but getting some of
the chemicals is a bigger headache than I care to go through.
I looked through the forums and some of the threads regarding many of these materials, and I still have quite a few questions to ask about these.
Primarily about safety (I believe in safety first, second, and third. Results last and I will sacrifice an optimal yield for added safety), and
secondly about making sure I have everything setup to make them successfully. I figured I’d make a big question dump in one go to get all the info I
need. Chemistry is something I got into recently and most of the stuff I have been doing is fairly safe (extracting chemicals from random store
products, crystalizations and recrystalizations, electrolysis, concentrating chemicals, etc, etc).
1: Sensitivity: I once thought about making TATP, but after seeing several videos on how insanely sensitive it is I decided to wisely heed the warning
you had on the wiki and steer as clear of all peroxide-based energetics. I value my fingers far too much to even dream of making that stuff.
But that being said, I do have other questions concerning sensitivity. I know RDX is considered super stable, so I am not worried about that. But what
about ETN? ETN, as I’ve read, is three times more sensitive than PETN. What does that mean exactly? Just how sensitive are we talking about here?
I mean if I wanted to make blasting cap and I put 1 gram or 0.75 grams as a booster and gently pressed it with a wooden dowel, would there be any
chance of detonation? What about fire in that regard? Can someone please tell me what ‘three times more sensitive’ means exactly.
Also I’ve seen some people make blasting caps and use small bits of cotton as a spacer between the booster, the primary, and the ignition mixture.
If I wanted to make a blasting cap using ETN, NHN, and black powder, and if I decided to use nitrocellulose in place of the regular cotton, would that
possibly cause problems? I’m just asking because I thought of doing that and I don’t want to end up doing something bad. (I figure the
nitrocellulose would give the blasting cap a bigger kick).
Regarding Picric acid. I know it should be kept stored in a wet state (as normally all explosives when not in use) but the wiki makes it look like it
is a lot more dangerous than others. Is ammonium picrate more or less stable?
Finally, about DDNP, I saw on the thread about it that its impact sensitivity is 1,5 Nm (150g from 1 meter or 1,5 kg from 10 cm). That means dropping
a 1.5 kilo weight from 10 cm will cause it to detonate? How dangerous is softly pressing it into a cap is? Redundant I know, but I really need to ask.
2: Nickel Nitrate:
I’ve read that nickel nitrate can be made by mixing nickel oxide in nitric acid. Would nickel metal suffice? I don’t have nickel oxide or nickel
chloride, but I do have a good supply of 99.6% pure nickel strips. I’ve seen videos where some guys let the metal dissolve in a 65-68% HNO3
solution. Would 90+% fuming HNO3 also produce a similar result? The results would have a green solution. According to the thread on NHN, the formula
states to mix both the hydrazine sulfate and nickel nitrate in 95% ethanol before mixing. If the nickel nitrate is already in a liquid state, would
addition of ethanol be necessary at that point?
Also how much nickel metal to acid is needed for an optimal result? How important is the addition of 30% hydrogen peroxide is to the solution (I’ve
seen videos were some use it and others don’t).
3: Fenton’s reagent.
Yes I know it isn’t an energetic, but I will need it to dispose of the picric acid/ammonium picrate I most likely will be making, but the exact
proportion of hydrogen peroxide to iron chloride is unclear to me. Can someone just give me a quick ratio?
4: Sulfuric acid, diluting and measuring.
When diluting sulfuric acid. If I diluted drain cleaner grade (93% estimated, with inhibitors) would this cause any difference in the reactions I need
in projects (Hydrazine sulfate for example). Or would it have to start off as reagent grade? Would it make much of a difference?
I would measure the mass/volume of my acid to find out the percentage, but sadly my scale doesn’t go beyond 0.01 grams. What other way is there for
testing the percentage without any special equipment?
I think these are all the questions I have for now.
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Oxy
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I would not use drain cleaner for any reaction without purification. Inhibitors can affect the reactions in unpredictable ways
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Sulaiman
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If a fountain type firework uses a mixture of potassium nitrate with sulphur and iron powders,
in a humid environment, is it likely or possible that people downwind may smell hydrogen sulphide?
(considering testing... just curious)
CAUTION : Hobby Chemist, not Professional or even Amateur
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ManyInterests
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| Quote: Originally posted by Oxy | | I would not use drain cleaner for any reaction without purification. Inhibitors can affect the reactions in unpredictable ways |
I used drain cleaner to make my nitrocellulose and it worked quite well. I made 3 small batches... I discovered that if you undernitrate the cotton
balls they become LESS flammable than normal cotton balls!
No joke. When I made my first attempt. I looked at the small container with the nitrating mixture and I figured 'I can fit 4 balls in there' and I put
four cotton balls instead of two. What happened is that the end result was practically flame resistant than flammable. My 2nd attempt had 3 balls, and
they burned well, but not as fast as you would expect. My 3rd and latest attempt (little more KNO3 than the formula called for) with 36 hours of
nitration instead of my usual 24 resulted in a super fast burning nitrocellulose.
I used drain cleaner grade acid for all of those attempts, as I didn't have the apparatus for purifying sulfuric acid just yet. Right now I'm
concentrating some store 3% hydrogen peroxide to 30+%. It takes forever and I am doubtlessly losing due to using the evaporation method, but it works
for my purposes and for the amounts I need.
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Jebby
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Anyone know if it would be possible to set off 5 to 10g of melt cast etn with little confinement with a 75/25 1g det cap that has .25g of melt cast
etn with .25 of powdered etn on top. I’m just wondering if anyone has an idea if it would work or not because I don’t really want to waste etn
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MineMan
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Jebbayyyyy
Many are going to be reluctant to answer because this forum is built off of experimenting.
When it comes to explosives. Follow your gut even if it does not make sense.
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B(a)P
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| Quote: Originally posted by Jebby | | Anyone know if it would be possible to set off 5 to 10g of melt cast etn with little confinement with a 75/25 1g det cap that has .25g of melt cast
etn with .25 of powdered etn on top. I’m just wondering if anyone has an idea if it would work or not because I don’t really want to waste etn
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Some more info would be useful. Is you det cap proven to be reliable? Are you sure that the melt cast etn component of your cap is detonating? What
makes up the other 0.5 g of your cap? There are some good threads on SM on this very subject, I would post the links but I have terrible reception and
am using a phone.
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math
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What are some ideal energetic materials, in terms of being low in manufacturing costs, ease of synthesis, good thermodynamic properties and having low
shock and friction sensibility? Thanks
[Edited on 3-6-2021 by math]
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MineMan
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| Quote: Originally posted by math | What are some ideal energetic materials, in terms of being low in manufacturing costs, ease of synthesis, good thermodynamic properties and having low
shock and friction sensibility? Thanks
[Edited on 3-6-2021 by math] |
DAUN
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kweiny
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| Quote: Originally posted by math | What are some ideal energetic materials, in terms of being low in manufacturing costs, ease of synthesis, good thermodynamic properties and having low
shock and friction sensibility? Thanks
[Edited on 3-6-2021 by math] |
Well in my experience there is no "ideal" energetic material. They all have thier pro's and con's
Take TATP as an example: Its easy to synthesize but stupidly sensitive.
RDX is another example: relatively easy to make (if you got the precursors) but quite hard to detonate. You cant just stick a fuse in it.
For my needs i find that ETN will probably do the job. I can get everything that is needed to synthesize it quite easily Online. Its stable enough to
be worked with (meaning it doesnt detonate when you just lightly touch it eg. TATP) and i found a plan for a detonator from someone on here that uses
ETN as main charge and Silver acetylide as Primary.
My suggestion is you browse the forum for a while and evaluate different energetic materials and thier pro's and con's and find the one hat suits your
situation the best. If i got something wrong fel free to correct me.
Cheers 
[Edited on 8-6-21 by kweiny]
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densest
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| Quote: Originally posted by Sulaiman | If a fountain type firework uses a mixture of potassium nitrate with sulphur and iron powders,
in a humid environment, is it likely or possible that people downwind may smell hydrogen sulphide?
(considering testing... just curious) |
KNO3 + S + fuel reactions are interesting. Gunpowder has been researched pretty thoroughly. As usual I don't have the reference on hand. Among other
products KNO3 + S produce complex sulfides of potassium which can react with water to make H2S. Gunpowder charcoal contains enough volatiles to
produce H2S directly.
I'm curious that the firework described will be a fountain because relatively little gas will be produced. I'd expect some charcoal or other
gas-producing fuel.
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Runic7
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| Quote: Originally posted by Sulaiman | If a fountain type firework uses a mixture of potassium nitrate with sulphur and iron powders,
in a humid environment, is it likely or possible that people downwind may smell hydrogen sulphide?
(considering testing... just curious) |
Unlikely, out of all the testing I have done with fountains outdoors, I have never run into a problem with the smell of hydrogen sulfide. As long as
pure chemicals are used, I don't think this will be a issue for you.
[Edited on 6-19-2021 by Runic7]
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ManyInterests
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I have a question about freebasing hydrazine sulfate for nickel hydrazine nitrate synthesis. How many grams of sulfate to how much 95% ethanol and
sodium hydroxide? Also add the hydroxide first or ethanol first?
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DraconicAcid
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Steam distillation- what is it good for purifying? What kind of impurities is it good for getting rid of?
I get the idea that it is good for purifying organic liquids with high boiling points and that are immiscible with water, and would be good for
getting rid of materials that are either completely non-volatile, or are significantly water-soluble at 100 oC, but I haven't found a more detailed
description than that. I'm thinking it might be a good way to separate, say, an amide from an ester.
Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
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walruslover69
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With a few exceptions, vacuum distillation is usually superior to steam distillation, as it is much quicker and doesn't involve further purification
and drying.
The only times that I have ever steam distilled was when I reduced a nitro compound with zinc, and had my amine mixed with a large solid mass of zinc
oxide. Worked great, but is a little bit of a hassle. It's not the best at getting good separation of compounds (in my experience). I think It's a
popular way to extract essential oils fragrances and terpenes from plant material without using solvents.
It could work, you might want to be slightly weary of hydrolyzing your ester in the presence of boiling water.
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DraconicAcid
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Sadly, I don't have a vacuum pump (and I don't think a water aspirator would work for vacuum distillation), so I'm still looking into steam.
Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
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Bert
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Not a given.
This depends on how much vacuum you want, how sensitive to water your process is and how cold you can keep your water supply...
https://www.amazon.com/HNZXIB-Laboratory-Distillation-Equipm...
[Edited on 11-10-2021 by Bert]
Rapopart’s Rules for critical commentary:
1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it
that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.
Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).
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SWIM
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For years a water aspirator was all I had for vacuum distillations.
It worked okay as long as you didn't need too high a vacuum.
I'd put a filter flask in the line from aspirator to still as a vacuum trap to ensure I never sucked a bunch of water into my reaction mixtures.
I've made diethylsulfate that way, and a few other things.
I was only getting down to 50 Torr or so because the tap water on the San Francisco peninsula isn't d very cold.
I bet the tap water is a lot colder in your neck of the woods, and you can always use recirculated ice cooled water if needs be. And if you have a
pump.
Using the tap won't work well if you have pressure fluctuation in your plumbing, but if the pressure is fairly constant it does work okay.
Older organic lab manuals have good advice on setup and use of aspirators for distillation.
I like Organic Experiments, by Feiser and Feiser.
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karlos³
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| Quote: Originally posted by DraconicAcid | | Sadly, I don't have a vacuum pump (and I don't think a water aspirator would work for vacuum distillation), so I'm still looking into steam.
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Oh wait what?
Nonono, it suffices, not for everything but it does.
I agree with mostly everything SWIM said about them.
Its a good alternative.
There is a video of nurdrage or the other guy, boiling water at rt with an aspirator.
I bought a few of the cheap(very cheap) pump he used in there directly from india after trying it out.
Or was it from china and the video how to put the cables in came from india?(that sounds more realistic)
I am still on my second, because the first needs to be taken apart for cleaning etc, but still worked.
Oh, I bought those pumps in 18 or even 17 
verrückt und wissenschaftlich
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DraconicAcid
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Not sure how stable my water pressure is, but I can hook up a trap easily enough. I may very well give it a try. I can always keep the receiver in
an ice bath, and I don't have to worry about water-sensitivity (or I wouldn't be considering steam distillation).
One reason I'm considering steam distillation for this is that I'm usually keeping almost everything I do as a possibility for my students to use. I
could have them do steam distillation, but all the water aspirators running at once for vacuum distillation? Yikes. Half the sinks would flood.
Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
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ManyInterests
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| Quote: | | I have a question about freebasing hydrazine sulfate for nickel hydrazine nitrate synthesis. How many grams of sulfate to how much 95% ethanol and
sodium hydroxide? Also add the hydroxide first or ethanol first? |
To answer my own question, it appears to be 80% hydroxide to however much hydrazine sulfate you put in, and it appears to be best to dissolve the
sulfate in ethanol first, only using exactly what is necessary.
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Microtek
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Hydrazine sulfate is not very soluble in ethanol. I suggest you use 1 mol HS to one mol sodium hydroxide, with enough ethanol added to cover the
entire mass. Then triturate this (ie. grind it under the fluid surface) until a blob of white slurry has formed. In my experience, this blob doesn't
really mix with the ethanol, so I like to add a second mol of NaOH to convert the NaHSO4 to Na2SO4 to make it separate more cleanly as a crystalline
precipitate. There may be a drying effect as well, since Na2SO4 can form stable hydrates.
Then decant the ethanol solution of hydrazine, and extract the remainder with a few more portions of ethanol. There's a trade off here between product
recovery and concentration, so consider your requirements.
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ManyInterests
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That sounds good. It will need maybe some experimentation for it to work. But I got other question related to NHN synthesis.
For the hydrazine, when making it using the Hoffman degradation of urea (how I made hydrazine sulfate) would the hydrazine that is made before the
addition of sulfuric acid and cooling to extract the hydrazine sulfate be adequate to make nickel hydrazine nitrate? As in just adding the nickel
nitrate solution to the hydrazine at 65 C be enough? That seems much easier than making the sulfate then freebasing it again. I can make the hydrazine
and use it on the spot instead of storing it for later.
Also about the nickel nitrate hexahydrate. I saw people make it with nickel metal, nitric acid, and hydrogen peroxide as a catalyst. Do we need to dry
it or boil it down to extract the hexahydrate, or would simply refluxing the three reagents for a few hours be enough? And the resulting solution
added to the hydrazine as prepared above?
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