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Author: Subject: Quantitative NHN synthesis without Hydrazine hydrate
ManyInterests
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[*] posted on 14-12-2021 at 20:22


so... hurray! I appear to have succeeded.

Bad news? I seem to have a problem cleaning my buchner funnel. The frit is contaminated with minute amounts of NHN and since I am putting sodium hydroxide through it to neutralize it, it is turning green from nickel oxide... Is my buchner funnel done for? I planned on giving it away for someone to use to make food grade stuff. I figure it is kinda useless now for that purpose?
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fredsci93
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[*] posted on 14-12-2021 at 20:33


nah, it's fine just wash it with sodium hydroxide then hydrochloric acid, the hydrochloric acid cleans off any nickel oxide
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[*] posted on 14-12-2021 at 20:54


That's good to know. How dilute does the HCl need to be?
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fredsci93
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[*] posted on 14-12-2021 at 21:44


maybe 10-5% it doesn’t matter much, just enough to dissolve the small amount of nickel oxide
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[*] posted on 14-12-2021 at 22:07


OK, so my HCl is around 31.5%, so to 1 part of that, add 2.5 parts of water. simple enough.

[Edited on 15-12-2021 by ManyInterests]
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[*] posted on 15-12-2021 at 00:58


yea, it's not an exact science, anywhere between 15% and 5% would probably work
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[*] posted on 17-12-2021 at 15:23


Here is my end result! 8 grams (wow! I wasn't expecting that much!) of clay like NHN. I did burn the filter paper and I did hear the snap and crackle that is characteristic of small NHN deflageration.

That being said. It seems like I added too little dextrin to the nickel nitrate, or the dextrin should have been added to the hydrazine. At any rate. I will need to very carefully grind them up with a rubber spatula, just like the documentation said.

Edit: After grinding I had apparently lost 0.2 grams (enough for a cap!) that got stuck to the containers.

I hate to throw them away. But after this... well, I'm soaking them in sodium hydroxide solution to neutralize the NHN. I will throw the water after and throw them in the trash. I can always get more glass baking pans.

Nhn.jpg - 1.9MB

[Edited on 17-12-2021 by ManyInterests]
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[*] posted on 17-12-2021 at 15:56


Yea, you’ll always lose a bit to mechanical loses, but 8g is a very nice amount, enough for 40 detonators which should last a very long time, in confinement does the NHN strongly detonate? (Don’t test to much, I usually use remote detonator for my first test or two, just to get a feel of how much I can test at a time)
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[*] posted on 17-12-2021 at 16:56


40 detonators? That's quite a lot. I was thinking around 16. The reason is I was using the improvised munitions manual as a guide on making improvised detonators.

They recommend 1 gram of a booster (RDX, picric acid, or ETN/PETN) combined with anything from 3 grams of lead picrate to one gram of TACC, 0.5 grams of DDNP, or 0.75 grams of mercury fulminate, HMTD, or double salts.

I mentioned it several times before that I am using a pen body for a detonator casing. How much ETN and NHN should I put in? How much black powder for the ignition mix? ( I will be using an electric match. I will seal the other end with hot glue.

Edit: I was planning on usnig 0.5 grams of NHN, using the same amount as DDNP (albeit NHN has a det velocity of 7000mps, while DDNP is around 5500).

[Edited on 18-12-2021 by ManyInterests]
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[*] posted on 17-12-2021 at 17:17


I use about 200mg NHN to set off ETN, so long as the ETN is dry and medium/low density 200mg is fine and ~>90 explosive yield compared to using 500mg NHN, since ETN is quite easy to set off, how much explosive you want to use depends on what you want to set off, you won’t need any more than a gram for nearly all secondarys, between 1g and 10g is needed for tertiarys, although all this depends on what explosive you use, DDNP would be fine for a detonator, not sure how much NHN you would need though, maybe 500mg would be required for it, although 0.5g of DDNP might not be sufficient for all secondarys (something like nitrourea which is arguably a tertiary explosive might not be set off)

3g lead picrate is not ideal and you only need that much since lead picrate sucks, if you use a stronger primary like NHN, CHP, AgNTZ, CuNTZ, Ni(NTZ)NO3 etc then you will only need max 500mg (depending on the booster you chose) , but all that depends on what you want to set off, but I would recommend increasing the amount of booster rather than the amount of primary if you want to set off more insensitive explosives since you can separate the primary and the secondary prior to detonations so as to reduce the danger (dealing with 1g primary + 10g secondary separated is much safer than 10g primary + 1g secondary separated or either mix on their own)

For a NHN/ETN pen detonator the amount of black powder is not super crucial, maybe ~1cm worth, just enough to get it all to burn at the same time, for initiating ETN you only need 200mg NHN lightly compressed (LIGHTLY being an important stipulation) ontop of 200mg powdered ETN and however much cast ETN you want depending on what you need the detonator for (minimum 500mg for secondary up to maybe 5g maximum for setting off tertarys, but take that with a grain of salt as I don’t work with tertiarys)

[Edited on 18-12-2021 by fredsci93]
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[*] posted on 17-12-2021 at 18:31


That sounds good. Detonators are an interesting thing. The reason why lead picrate and the other stuff is use is because the improvised munitions manual was written in 1969 and back then things were a little different... on top of that, the laws regarding obtaining reagents was very different back then, and the manual assumes the munitions maker has no chemistry equipment.

The reason why they made the detonator so strong (I believe) is that they wanted to make a detonator that could set off almost all explosives, like dunnite (ammonium picrate, a very stable explosive) or composition B or TNT, which require a booster like tetryl, RDX, or picric acid in order to detonate in addition to the primary.

But right now I'm not really looking to set anything off other than the detonator. So I guess I'll make a few with various compositions... or maybe make them just before I know I will get an opportunity to set them off. I don't think it's a good idea to have blasting caps lying around, especially with the electric match inserted.

When I do get around to setting stuff off I will be making a plasticized ETN/RDX mix (I would have that now, but as you know, my K6/RDX synth went awry) as well as a cheddite explosive (potassium chlorate mixed with petroleum jelly in a 9:1 mixture).

I also made a system of getting the energetic powder into my pen body before pressing.

https://www.youtube.com/watch?v=62kPi5kpbcg&list=WL&...

This video makes a very nice cone that fits well into the inner diameter of my pen but also flares up that it makes loading quite easy. I will be hand pressing, but I will put the pen body in my 5 gallon, sawdust filled bucket with a pair of needle-nosed pliers (away from my hand) and press with the wooden dowel that I will also hold with a pair of pliers.

I won't press too hard. I will gently increase pressure but not give it a ram. No tamping either.

My black powder I believe will work. But maybe in the future I might want to attempt to make faster burning black powder. I tried the wet method (using alcohol and trying to cake and grate the grains) but it didn't work well. The powder still burns well when I put an electric match in it, but it doesn't react when I use a barbique lighter. It's weird that way. So I need to make sure that when I insert the electric match, the match must be enveloped in the black powder to insure ignition.
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[*] posted on 19-12-2021 at 11:27


@fredsci93

Quote:

I use about 200mg NHN to set off ETN, so long as the ETN is dry and medium/low density 200mg is fine


What confinement was used in this case?
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[*] posted on 19-12-2021 at 11:57


The NHN is lightly pressed into a PP tube and takes up ~5mm of the tube, a fuse mix is added above it with a fuse inserted, this assembly is then sealed with hot glue and electrical tape.

So the confinement is a PP tube with a hot glue lid, the NHN sits directly ontop the ETN (except for a thin layer of cling film to stop the ETN mixing with the NHN)
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[*] posted on 19-12-2021 at 12:50


Quote: Originally posted by fredsci93  
The NHN is lightly pressed into a PP tube and takes up ~5mm of the tube, a fuse mix is added above it with a fuse inserted, this assembly is then sealed with hot glue and electrical tape.

So the confinement is a PP tube with a hot glue lid, the NHN sits directly ontop the ETN (except for a thin layer of cling film to stop the ETN mixing with the NHN)


Have you tested this? I would be surprised if lightly pressed 200 mg of NHN would reliably set of ETN.
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[*] posted on 19-12-2021 at 13:40


Now I'm even more suspicious ;)
What does the witnessplate say to this?

Just a bang or at least a dent?
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[*] posted on 19-12-2021 at 15:44


For reliable DDT, respectively for DDT segment with low density was necessary do mix ETN /NHN 1:1. A like two dry powders, respectively
grains ETN + fine powder NHN. And it even in solid steel cavity. Thats my experiences. Output segment of course cast ETN or high pressed ETN. This described mix is pressed on 5 Kg in cavity 6 mm. With central bridge wire in mix. As plug can be used warm plastic glue. The assemble cast ETN + slightly pressed NHN only, can be not reliable always. Especially in plast cavity.
300 mg high pressed ETN as output segment must deflorate 2 mm steel plate of diameter minimal 6 mm, usually 7 mm.




Safety explosive Alfred Nobel 1867. Safety ecologic detonator Dr. Liptakov 2015, inventor CHP and Lithex
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[*] posted on 19-12-2021 at 17:13


I haven’t extensively tested it (I did a couple detonations, 3 with one misfire where the NHN wasn’t defligrated/detonated due to a bad fuse + I detonated some ETN with the cap), it's not the greatest design, I'll look at improving it I've just not had a burning need to have a high yield detonator cap right now so the potentially poor explosive yield and overall power has never phased me enough to look into it, but it sounds like it's sub optimal

below is a diagram (not the greatest quality, but you get the idea)

[Edited on 20-12-2021 by fredsci93]

Cool.png - 6kB
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[*] posted on 20-12-2021 at 00:49



Quote:

I haven’t extensively tested it (I did a couple detonations


Can you explain these "detonations"? Did you set anything of with you cap or was it just the caps itself?
Like Doc Liptakov wrote, can you punch through metal?

If the cast ETN is set of properly, that should be no problem. If it is blasted to pieces the whole assembly can still make a hell of a bang but it will initiate nothing.

But thank you for sharing your synthesis, like others, I got frustrated with the sulfate. But I happen to have some dichloride I got as a gift a long time ago and never bothered since ;)
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[*] posted on 20-12-2021 at 01:15


I didn’t test with any metal plates, I have done 3 detonations with just the cap underground and one with the cap and ETN (10g), all but one showed subjectivity good results based off what I expected from prior detonations, the one bad result being one cap which didn’t get properly initated for some reason, I should have tested it's penetrating power on some aluminium or steel, maybe next time I suppose.
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[*] posted on 20-12-2021 at 08:17


Witness plate test is necessary for confirmation. All others are only speculations. CHP works a like primary - secondary energetic material.

CHP05.jpg - 86kB

[Edited on 20-12-2021 by Laboratory of Liptakov]




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[*] posted on 21-12-2021 at 04:52


When I test energetics for performance, I use the following setup:

- 1.000 +- 0.002 g of the material is pressed into a brass tube of 8mm OD and 0.5 mm wall thickness. The tube is bottomless to avoid errors from varying material thickness. The pressure used is substantial, but unmeasured - I use a vice or my small hydraulic press, so around 100 kg, or 570 psi.

- 0.300 +- 0.002 g of PETN is pressed directly on top by hand.

- The charge is glued into a 3D-printed flange which is then glued onto a piece of 20 +- 0.005 mm thick aluminum bar taken from the same stock to avoid alloy variations. The point of the 3D-printed piece is to ensure an absolutely flush and square contact between the charge and the witness block.

- It is set off using a small 3D-printed cap that fits inside the tube, and contains a wad of fluffy NC. The cap is then closed at one end with a putty made of aminoguanidine nickel perchlorate and NC dissolved in acetone. The other end is closed by design, except for a hole which fits the wire I use. A 20 cm piece of wire is cut off and inserted into the hole (I've designed it to be an interference fit).

- The assembly is placed in a thermobox (ca. 30 liters) filled with crumb rubber in place of coarse sawdust, and initiated electrically using a cheap (1 dollar) boost converter which produces an arc across the end of the wire inside the cap, igniting the fluffy NC.

The dent that the explosion makes in the aluminum block is then measured using a dial indicator as the difference in height between the flat upper surface and the lowest point of the dent. This is then compared to the values I obtained for picric acid, PETN, RDX and HMX, in the same setup.

Not all energetics perform as well as they might under this protocol. Aminotetrazolium nitrate for instance, places between picric acid and PETN. This might well be caused by under initiating or by too little distance to accelerate but this reflects what I require from energetics, since I usually work at the ~1 g scale.

[Edited on 21-12-2021 by Microtek]
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[*] posted on 21-12-2021 at 11:25


Microtek: that is a *very* interesting setup, I might have to borrow some ideas from it. How well does it do with regards noise reduction? I'd imagine it muffles the sound a fair bit?
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[*] posted on 21-12-2021 at 14:31


Yes, my family doesn't notice the difference between me hitting something with a hammer in my workshop (located below the main floor) and a detonation in my thermobox. I'm sure that coarse sawdust will muffle the noise just as well as crumb rubber, but the rubber is less flammable.
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[*] posted on 22-12-2021 at 10:06


After doing a touch of work with making black powder filled caps (only black powder) and experimenting slightly with the NHN I made I came to the following.

When pressing the ETN and NHN it must be pressed very gently. Not because of the sensitivity, but one thing I noticed is that if I press something too hard into a cap it won't even burn. I've had black powder fizzle, potassium chlorate/nitrocellulose pop well when not super pressed, but fail to do anything when heavily pressed.

Also I realize that NHN is so flame sensitive that it does not an igniter like black powder. Besides... the match head I used on my electric match will produce all the flame needed to set off NHN. Given how unbelievably flame sensitive this stuff is!

Seriously. I took like a tiny pinch of NHN (My scale couldn't measure how much because of how little I put) and the flash it made after the flame so much as licked it was shocking. I was momentarily stunned by its power! My first successful batch was a fine batch indeed!

One other thing is that I apparently am terrible at making christmas light e-matches. I'd better stick to my own design. They need more power to set off, but a 9V battery made of 6 AA is quite small and I noticed will still ignite my match that is set at the end of 3 meters worth of wire. I will test it with a soldered battery pack made of 6 AAAs. But that is just out of curosity.

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[*] posted on 22-12-2021 at 15:01


@Microtek Id love some photos of the 3D printed caps your using and your box! Can you point me in the direction of some info regarding that primarily putty, it sounds interesting.

@ManyInterests its called dead pressing. Good to know the NHN can be dead pressed though, Im sure that will save someone a headache.
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