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Morgan - 6-5-2021 at 03:34

On eBay teflon tubing is described as S, T, or L from Chinese sellers. They sometimes list it as a size or sometimes as a type. Any ideas?

I just discovered it pertains to wall thickness in Teflon tubing. L is the thinnest and S is the thickest wall diameter. So something with an inside diameter of 1mm for example, choosing L,T, or S indicates which wall thickness although outside diameters were also stated in the description.

[Edited on 7-5-2021 by Morgan]

Jebby - 14-5-2021 at 09:14

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]

MineMan - 16-5-2021 at 13:26

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

ManyInterests - 16-5-2021 at 20:50

(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.

Oxy - 17-5-2021 at 00:51

I would not use drain cleaner for any reaction without purification. Inhibitors can affect the reactions in unpredictable ways

Sulaiman - 17-5-2021 at 06:12

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)

ManyInterests - 17-5-2021 at 13:20

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.

Jebby - 30-5-2021 at 12:40

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

MineMan - 31-5-2021 at 00:37

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.

B(a)P - 31-5-2021 at 01:12

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


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.

math - 2-6-2021 at 18:22

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]

MineMan - 3-6-2021 at 05:52

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

kweiny - 7-6-2021 at 23:48

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]

densest - 12-6-2021 at 20:34

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.

Runic7 - 18-6-2021 at 21:30

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]

ManyInterests - 9-11-2021 at 19:37

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?

DraconicAcid - 9-11-2021 at 19:55

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.

walruslover69 - 10-11-2021 at 07:20

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.

DraconicAcid - 10-11-2021 at 08:26

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.

Bert - 10-11-2021 at 12:18

Quote: Originally posted by DraconicAcid  
I don't think a water aspirator would work for vacuum distillation


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]

SWIM - 10-11-2021 at 20:41

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.

karlos³ - 11-11-2021 at 00:00

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.

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 :o

DraconicAcid - 11-11-2021 at 10:34

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.

ManyInterests - 19-11-2021 at 21:40

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.

Microtek - 21-11-2021 at 03:11

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.

ManyInterests - 26-11-2021 at 14:16

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?

katyushaslab - 27-11-2021 at 05:01

No, the hydrazine in solution with unreacted urea, unreacted NaOCl, and all the side products is not going to be clean enough to work with.

You need to extract it as hydrazine sulfate, then freebase. This step will ensure that you have a clean enough starting material, no weird fucking side reactions, etc.

ManyInterests - 27-11-2021 at 19:38

OK that makes sense.

So I think this will likely be my final question for a good while... when making the nickel nitrate. I've seen everyone react nickel metal (I have 99.6% pure nickel metal. It's very shiny and extremely clean) that's been cut to tiny pieces. The process I've seen is to add around 30% hydrogen peroxide to it as a catalyst and 68% nitric acid in a flask and then to reflux it gently for several hours. (I plan on using a hot water bath for this and never let the water reach a rolling boil around 90C or so should be sufficient).

After refluxing for hours, can this mixture be added directly to the hydrazine or would it need to be filtered? If the hexahydrate needs to be vacuum filtered, what is the optimal way of cleaning the buchner funnel? Just distilled/tap water or any other solvent is necessary? I heard that that Nickel Nitrate hexahydrate is hard to filter as it is a very fine particulate. Would it go through several layers of coffee filters?

Just getting info for the NHN synthesis. The HDN/RDX/Keto-RDX seems simple as all I need for that is fuming nitric acid at this point.

katyushaslab - 29-11-2021 at 05:34

I can't really answer to the "making nickel nitrate" question authoritatively, given I just buy my nickel nitrate.

I would, however, strongly advise filtering the nickel nitrate solution, boiling it down, and maybe recrystallizing from distilled water - just to remove any unreacted nickel, etc. If I recall correctly, nickel might be one of those metals that can cause hydrazine to decompose.

More steps cleaning up your reactants will result in a safer, more reliable product. Taking shortcuts is inadvisable (though sometimes oh so tempting).

As for the HDN/RDX: a good efficiency tip is to use any weak nitric (say, created from traps while distilling - see the NurdRage videos) to make the HDN. As for the RDX part - you want white fuming nitric instead of red fuming nitric, bubbling dry air through RFNA will clear it up. Some people add a small amount of urea to clear their nitric, but I've had mixed results with that, dry air bubbling has been more reliable.


ManyInterests - 29-11-2021 at 06:06

I have a small palm-sized 12v air pump (works for blowing and vacuum) and some clear PVC tubing. I did heard that vinyl plastic doesn't get destroyed easily by highly concentrated nitric acid, so I will cut a short length to bubble out the NO2 when I make some more nitric acid. I know that the specific gravity of the acid must be 1.49 or 1.50 at room temperature it for it to be WFNA and work for RDX or Keto-RDX. I think I might try doing keto-RDX as it seems more powerful and still retains the stability of RDX. Also it would require a nitrating mixture of H2SO4 that will let me use up my remaining H2SO4 and stretch my WFNA supply.

Lomax - 17-4-2022 at 14:16

I have a question, can i use sodium bisulfate as a dehydration agent for Nitrourea or Nitroguanidine?

Rainwater - 17-4-2022 at 14:46

Quote: Originally posted by ManyInterests  
I have a small palm-sized 12v air pump (works for blowing and vacuum) and some clear PVC tubing. I did heard that vinyl plastic doesn't get destroyed easily by highly concentrated nitric acid, so I will cut a short length to bubble out the NO2 when I make some more nitric acid.


I have noticed considerable vacuum formation inside of a sealed apparatus connected to a bubblier, resulting in water sucking back into my collection flask. The best method I have discovered is by using a cold trap with dry ice to solidify the gas. After the no2 generating reaction is complete, I add an equal volume of ice to the cold trap and allow the apparatus to slowly warm up. The reaction produces a consentrated nitric acid

MineMan - 17-4-2022 at 17:57

Quote: Originally posted by Lomax  
I have a question, can i use sodium bisulfate as a dehydration agent for Nitrourea or Nitroguanidine?


Instead of sulfuric acid?

Lomax - 17-4-2022 at 20:41

Quote: Originally posted by MineMan  
Quote: Originally posted by Lomax  
I have a question, can i use sodium bisulfate as a dehydration agent for Nitrourea or Nitroguanidine?


Instead of sulfuric acid?

Yes sience sulfuric acid can be replaced with sodium bisulfate for a number of reactions (Nitric Acid) for example. I thought it can be used as a dehydration agent for Nitrourea or Nitroguanidine sience Conc. Sulfuric Acid is very regulated in my country.

MineMan - 18-4-2022 at 06:05

Quote: Originally posted by Lomax  
Quote: Originally posted by MineMan  
Quote: Originally posted by Lomax  
I have a question, can i use sodium bisulfate as a dehydration agent for Nitrourea or Nitroguanidine?


Instead of sulfuric acid?

Yes sience sulfuric acid can be replaced with sodium bisulfate for a number of reactions (Nitric Acid) for example. I thought it can be used as a dehydration agent for Nitrourea or Nitroguanidine sience Conc. Sulfuric Acid is very regulated in my country.


Someone on here will know. It may be better to post in general chemistry. Can you try it yourself as well… everyone would be very interested in this answer

Lomax - 18-4-2022 at 06:19

Quote: Originally posted by MineMan  
Quote: Originally posted by Lomax  
Quote: Originally posted by MineMan  
Quote: Originally posted by Lomax  
I have a question, can i use sodium bisulfate as a dehydration agent for Nitrourea or Nitroguanidine?


Instead of sulfuric acid?

Yes sience sulfuric acid can be replaced with sodium bisulfate for a number of reactions (Nitric Acid) for example. I thought it can be used as a dehydration agent for Nitrourea or Nitroguanidine sience Conc. Sulfuric Acid is very regulated in my country.


Someone on here will know. It may be better to post in general chemistry. Can you try it yourself as well… everyone would be very interested in this answer

Ok

Morgan - 20-6-2022 at 12:51

I have a cylinder-shaped pencil holder like thing consisting of a tower of spaced aluminum rings and at the base a disc of clear glass bonded to the bottom aluminum ring. It looks like a clear glue of some sort so I tried heating it as much as I dared to break the bond and also acetone for the heck of it. Maybe it's an epoxy glue but what typically is used to glue glass and is there something that might break the bond? Maybe it's silicone.


[Edited on 20-6-2022 by Morgan]

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