Sciencemadness Discussion Board - Nickel aminoguanidine diperchlorate

Nickel aminoguanidine diperchlorate

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Etanol - 17-1-2025 at 08:30

The mother liquor was clear and not black the way it often gets in the patent method for NAP. This black colouring is, AFAIK, characteristic of AQ decomposition under the influence of air. There are other decomposition modes of course.

In the case of NAP, the black color is not a sign of the decomposition of aminoguanidine. This is really the color of the saturated solution of the NAP. It is very dark red, so it looks almost black.

Quote: Originally posted by Laboratory of Liptakov

It seems, that NAP explode soon spontaneously.....

Thank you for trying to soften the atmosphere, but this comparison is inappropriate.
The ions of copper and silver are fundamentally different from nickel by the ability to quickly oxidize hydrazine and hydrazine compounds at room temperature. This reaction does not require air.

Microtek - 17-1-2025 at 14:02

No, the black color I'm talking about is not the red of the NAP in solution. You can see it more clearly if you add prepared NAP to water. The water is gradually colored black, and the NAP loses its effectiveness. If you do it with just a little NAP, the black color is quite dilute and you can easily see through the water, bu it is still unmistakeably black, not red at all.

ManyInterests - 18-1-2025 at 19:13

Ok, so I need to report my latest attempt. It is currently drying, and there was a mishap.

The first thing I did was, in order to get to cool to 0C (or close to thereabouts) I used a saturated saline solution and put it in my freezer. There was plenty of slush there, but no solid water, so it was good for my purposes. Secondly I did the ultrasonic treatment outdoors where it is close to 0C anyway.

I used 50ml of water in a 250ml beaker with a watchglass atop it to cover most of it, but still allow CO2 and water vapor to escape through the spout, and I made sure it was boiling before putting in the reagents (1:0.86:0.43g proportions of the aminoguandine bicarbonate, ammonium perchlorate, and nickel carbonate), and while I said I did want to let it boil for 25 minutes, the diminishing solution volume made me antsy as it was getting close to 35ml or 30ml and I was hearing some mild knocking sound. I wasn't sure what it was, but like I said, I got increasingly nervous, so I took it off the heat after around 18 minutes of boiling.

There was next to no nickel carbonate left over. So much that I honestly did not think that decanting should not have been done... but I tried to do it anyway, the stirbar fell out and I had to wipe my floor to make sure I didn't have any residue left. I needed to use a little more water in order to wash the NAP that did stick to my beaker. I then started ultrasonication in the cold for 13 minutes. The glass I used wasn't heavy enough to sit at the bottom and to prevent it from floating up and possibly tipping over, I had to hold it down by hand throughout the whole time.

And while adding more of the cold slush, I think I accidently had some fall in the beaker. I am hoping that this does not interfere with the end product.

I noticed I have a lot more yield than the previous times which I did this, but I won't be calling it a success until I have some holes blown in aluminum foil!

pjig - 18-1-2025 at 20:33

You could do a wash to remove chloride contaminants from the finished product , then again, some “accidents “ produce unbelievable results , or changes in industry…. :cool:

ManyInterests - 19-1-2025 at 06:45

Complete failure... it reacted no differently than the previous times. I am legitimately baffled as to what is going on. The only alternative I can see is that this method is clearly not working for me, and I don't know why. I didn't even have that many problems with NHN synthesis.

I will not do any more attempts with the these three ingredients in a similar manner. I've had too many failures and nothing even remotely suggesting that they would work another time. I will need to make in a different way. I will give one more attempt with iNAP (isopropyl alcohol), but I will have to use my other ammonium perchlorate supply that may not be 100% pure.

I should mention that when I tried it, I put a coffee filter on a regular plastic funnel and I poured it in. Some some was so fine it seeped through, I poured everything on a paper towel again and let it dry.

I am just not a very happy mad scientist right now.

ManyInterests - 19-1-2025 at 10:39

OK I decided to do the iNAP synthesis. I started with 75ml of 91% IPA and I boiled it, then added everything with strong stirring and kept the boil for 14 minutes. The amount of solvent I used was starting to run dry, well below 50ml, so after 14 minutes I stopped the heating and immediately poured out the stuff. I have a much larger 'yield' than last time I did it with iNAP. There was no nickel carbonate left undissolved, so the extended heating and stirring did its job in that regard, but right now the final answer will be whether or not I will finally have a useable product.

To test, I put some on a thin sheet of aluminum foil and I use a cheap torch lighter beneath it to heat the foil.

Edit: I put a photo of what my stuff looks like.

[Edited on 19-1-2025 by ManyInterests]

Laboratory of Liptakov - 19-1-2025 at 14:12

The path to success is often lined with a trees. Trees of failures. However, in the case of NAP, the trees seems to have no end.

ManyInterests - 19-1-2025 at 14:44

It is possible that my aminoguandine bicarbonate is no good. That is a possibility

With this case, it has a weak fizzle, but no pop. So it is a failure.

Edit: Does Aminoguandine bicarbonate degrade over time? Even if stored properly?

[Edited on 19-1-2025 by ManyInterests]

Microtek - 20-1-2025 at 00:51

My aminoguanidine*HCO3 is about 20 years old and my NAP works every time I make it. I think it's safe to say that it has a very long shelf life.

Etanol - 20-1-2025 at 01:06

Quote: Originally posted by ManyInterests

Edit: Does Aminoguandine bicarbonate degrade over time? Even if stored properly?

This progresses very very slowly, much more than 10 years.

The color of your product indicates that you have received an aminoguanidine complex, but probably with a different anion.
Are you sure your NH4ClO4 is NH4ClO4? How did you prepare it?
Mix 1 gram of sugar powder and 3 grams of your powdered perchlorate. How does this mixture burn?

pjig - 20-1-2025 at 08:06

For the ammonium perchlorate you can tell if you burn it with hexamine or other fuels . It puts off hcl gas (burns nose ) . You can also introduce a base like sodium hydroxide to release the gas to confirm your ammonium perchlorate. As for the aminoguanadine bicarbonate im sure one of the members will have a simple spot test you cold perform to confirm your material and its condition.

[Edited on 20-1-2025 by pjig]

ManyInterests - 20-1-2025 at 22:35

Quote: Originally posted by pjig

For the ammonium perchlorate you can tell if you burn it with hexamine or other fuels . It puts off hcl gas (burns nose ) . You can also introduce a base like sodium hydroxide to release the gas to confirm your ammonium perchlorate. As for the aminoguanadine bicarbonate im sure one of the members will have a simple spot test you cold perform to confirm your material and its condition.

[Edited on 20-1-2025 by pjig]

Thank you for mentioning the hexamine test. Since I have two PbO2 (one bought, one made) anodes, I will be making more sodium perchlorate and from there maybe perchloric acid.

I was advised against making perchloric acid since it is very dangerous. I want to try, but I will be as cautious as possible and gather as much information before proceeding. Perchloric acid will allow me to make the purest ammonium perchlorate possible (by neutralizing it with an excess of ammonium carbonate. Once it is nothing but perchlorate and water and carbonate, it can be boiled down to destroy the excess carbonate and leave nothing but pure ammonium perchlorate), as well as making aminoguandine perchlorate. Since I put in an order for another 100g of aminoguanadine bicarbonate, I will have enough to experiment with.

I really want to succeed at this. I want to make a packable, safe to load/lightly press NAP.

Quote: Originally posted by Etanol

Quote: Originally posted by ManyInterests

Edit: Does Aminoguandine bicarbonate degrade over time? Even if stored properly?

My 'main' supply was made in 2022 or so when I made some sodium perchlorate (before my Pt anode died in the first attempt...) and I turned what I could of it into ammonium perchlorate via a double displacement of ammonium chloride and sodium perchlorate.

I also tried to make some with a different method. Since I had some lithium perchlorate that I bought (and thus can safely assume is pure) I took 5 grams of it and mixed it with ammonium carbonate. I filtered out the lithium carbonate (which is mostly insoluble in water, and has reverse solubility, too!) and slowly evaporated the water off the remainder, leaving me with 2.8 grams of pure ammonium perchlorate. I used an excess of ammonium carbonate since even gentle heating destroys said carbonate fairly quickly.

This is the perchlorate I used in most of my tests since it is the purest I know I have.

This is why I am baffled as to why it isn't working. Maybe my other supply isn't pure enough, but the one I made from lithium perchlorate has to be pure.

[Edited on 21-1-2025 by ManyInterests]

Microtek - 21-1-2025 at 00:09

How about your aminoguanidine, is that bought or home made?

Laboratory of Liptakov - 21-1-2025 at 00:32

He has purchased bicarbonate. He writes it on line 4. It seems it. Thus I estimate.

Axt - 21-1-2025 at 01:09

I'm with Etanol on this one, the chloride looks the same as the perchlorate but is of course, inert.

Try making the nitrate it'll also look exactly the same (perchlorate, chloride, nitrate, bromate all look the same) but will deflagrate somewhat like chlorate/sugar without the white smoke. That way you'll know you are getting the complex, just not the perchlorate.

Here's the writeup for the bromate salt, nitrate is the same just don't add the sodium bromate.

Preparation: Two solutions are made, for the first 1.49g (0.02mol) of nickel oxide is dissolved into 20mL of boiling 68% nitric acid and allowed to boil dry on a 200 degree hotplate. The remaining nickel nitrate in the form of a yellowish green plate is redissolved into 50mL of water. 6.04g (0.04mol) of sodium bromate is now added and dissolved.

For the second solution 5.45g (0.04mol) of aminoguanidine bicarbonate in 50mL of water is dissolved by the addition of 3.70g (0.04mol) of 68% nitric acid with the release of carbon dioxide gas. This solution is then freebased by the addition of 1.60g of sodium hydroxide in 10mL of water, solution turns from yellow to orange.

The first solution is rapidly stirred as the second solution is slowly poured in, the mixture quickly turns dark bluish purple and within 10 seconds a brick red precipitate fills the liquid. This was left to stir for 15 min then filtered and dried, yield 7.70g (83% to bromate, 116% to nitrate).

ManyInterests - 21-1-2025 at 20:40

Just to point it out, the nickel carbonate is purchased from a chemical supplier (onyxmet), so I assume it is lab grade and not pottery grade.

Quote:

Here's the writeup for the bromate salt, nitrate is the same just don't add the sodium bromate.

Preparation: Two solutions are made, for the first 1.49g (0.02mol) of nickel oxide is dissolved into 20mL of boiling 68% nitric acid and allowed to boil dry on a 200 degree hotplate. The remaining nickel nitrate in the form of a yellowish green plate is redissolved into 50mL of water. 6.04g (0.04mol) of sodium bromate is now added and dissolved.

For the second solution 5.45g (0.04mol) of aminoguanidine bicarbonate in 50mL of water is dissolved by the addition of 3.70g (0.04mol) of 68% nitric acid with the release of carbon dioxide gas. This solution is then freebased by the addition of 1.60g of sodium hydroxide in 10mL of water, solution turns from yellow to orange.

The first solution is rapidly stirred as the second solution is slowly poured in, the mixture quickly turns dark bluish purple and within 10 seconds a brick red precipitate fills the liquid. This was left to stir for 15 min then filtered and dried, yield 7.70g (83% to bromate, 116% to nitrate).

That sounds like an interesting experiment. But I cannot do the bromate since I have no sodium bromate and it isn't something I thought about making or getting. Your first step I assume is making nickel nitrate. I already have some available, so I don't need to make any... unless an excess of For the second step I will have to make some nitric acid since I don't keep that around. But I was planning on making lots of nitric acid anyway, so it isn't an issue (I aim for WFNA, but that can be diluted with distilled water to 68%).

It'll take a bit for that to happen since I will be a bit busy with other projects. I had made some detonators with NAP in mind, but since this has been taking so long, I used an ETN:NHN filler. I hope it is enough to set off some of my overpacked RDX caps!

My experience with NAP

Nemo_Tenetur - 22-1-2025 at 17:21

Now I want to share my two cents concerning the different synthetic pathways and results.

The promising power and ease of synthesis draw my attention to this thread for more than one year and I´ve decided to give it a chance.

As I have no problems to get (almost) all precursors from commercial lab suppliers, I´ve bought perchloric acid, aminoguanidine bicarbonate and nickel acetate. I could also buy directly nickel perchlorate, but the price was a ripoff (several hundred Euro for a half kilogram). In such cases, I´m a cheapskate and I´ve bought commercially available nickel acetate, added the appropriate amount of 72 percent perchloric acid and evaporated it in the vacuum to dryness.

The much stronger and less volatile perchloric acid liberate the much weaker and more volatile acetic acid, conversion and yield close to 100% - for a fraction of the called ripoff-price.

The commercially available nickel carbonate isn´t pure nickel carbonate, it´s always a mixture with nickel hydroxide, in most cases not further specified. This makes stoichiometric calculations more difficult.

Anyway, I got the cheapskate nickel perchlorate and the aminoguanidine perchlorate in the same way (aminoguanidine bicarbonate and perchloric acid, no vacuum necessary).

Then I combined the appropriate amounts of concentrated solutions, boiled it for several minutes, cooled it down and the result was NOTHING.

Sad. No reaction, no orange crystals, just a dark green but clear solution.

Where was the mistake? I´ve repeated it twice, with more and less concentrated solutions, more and less heat and stored it even in the fridge for weeks.

Again, nothing. Sad.

Then I found a comment here from a fellow member that I should add aqueous 25% ammonia.

I decided to give it a last try and BINGO, almost immediately orange crystals appeared and settled down to the bottom of the erlenmeyer flask.

The quantity of ammonia seems not decisive, two drops with a pipette were enough. Therefore I think (just my speculation) that a catalytic amount is enough.

I´ve repeated the synthesis without boiling, just a warm water bath, and got a copious amount NAP.

No ultrasonication, no boiling necessary.

Then I started sensitivity testing. Some told here that it is less sensitive, but I could initiate it with a hammer hit out of my wrist. Is this less sensitive? Maybe less sensitive than lead or silver azide, but with a moderate hammer strike it goes off, no excessive force necessary.

The response to a flame seems difficult to predict. From my experience, small quantities (up to a matchhead) deflagrates in most cases. Sometimes it makes a sharp "whomp", but no bang.

The slightest confinement, however, produce a powerful and sharp bang. See the mpeg "NAP clamp", a quantity less than a matchhead partially covered between the tip of a clamp gave such a powerful explosion that the gas flame was blown off, whereas a larger quantity at the tip of a knife gave an intense "whomp!" but no bang - and the gas flame was not blown off.

After the first flame tests of unconfined samples (just deflagration, no detonation observed) I´ve decided to destroy the residual NAP soaked in the filter paper - the residual quantity was so small that I couldn´t scratch it off with a knife or spatula, thickness much less than a millimeter - and hold the filter paper in the flame.

To my surprise, I got an ear-ringing detonation! My assumption is that the very weak confinement in the porous filter paper was enough to promote ddt.

As a side note: the gaseous explosion by-products are very unpleasant and irritating to lungs and/or mucous membranes, even in tiny amounts.

To sum it up: yes, it´s an interesting and very powerful primary, easy to synthesize once you´ve found the way.

But there are some serious drawbacks. Nickel and its salts are always problematic, although maybe less problematic than lead or even mercury. The strongly irritating fumes after a minuscule explosion are a red flag for me.

Also there are still not fully evalutated stability issues (water sensitivity) and some other data/values are also not investigated (for example, compatibility with aluminum, copper and plastic, with secondaries, and - very important - it´s sensitivity against electrostatic discharge), unknown or at least not published.

Feedback and comments to my results are welcome.

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[Edited on 23-1-2025 by Nemo_Tenetur]

[Edited on 23-1-2025 by Nemo_Tenetur]

Microtek - 23-1-2025 at 00:18

Yes, the products of the explosion, whether it is nickelcarbonyl or just atomized nickel, and the potential (probable) health effects are the reason I'm searching for alternatives based on iron, copper or cobalt. If you're interested in that, I'm writing some of my findings in the "complex salts" thread.

Regarding the sensitivity, it does indeed seem there is some variation. In my own experiments, with quantitative tests, NAP produced by either the ultrasonication method or the rapid stirring method shows a little less sensitivity towards abrasive impact (rigid hammer pendulum oblique impact onto 180 grit sand paper backed by steel) than PETN. Your pictures seem to indicate that your crystals are quite small, so maybe something other than grain size is at play.

Laboratory of Liptakov - 23-1-2025 at 00:41

I'm also looking for copper ion alternatives to basically anything that bangs. Similar to Microtec. I observe nickel compounds including NAP thread through the user interface. For sure..... :cool:

Nemo_Tenetur - 23-1-2025 at 01:28

Copper and iron, yes. But cobalt is - as far as I know - as problematic as nickel. Many cobalt salts are classified as SVHC according to EU legislation. And, from a commercial point of view, it´s more expensive.

The "jack of all trades" primary is still not found.

For small detonators indoor, I prefer silver azide even if it´s expensive. Atomized silver isn´t poisonous in such quantities. The preparation according to the pacific scientific energetic materials company performs well, an almost granular product and good pourability.

For big detonators outdoor, NHN is still my choice. It´s safe to handle, the synthesis is also safe, easy and high-yielding. I´ve gotten enough hydrazine hydrate (from industrial water boiler treatment, a really good deal by the way ...) that I don´t need to bother with it´s synthesis.

The drawbacks (confinement and large quantities necessary) are not decisive for me.

Etanol - 23-1-2025 at 07:41

Don't worry. Nickelcarbonyl is not there. High temperature and enough oxygen do not allow this to form.
An irritating smoke consists of NiCl2 and HCl. This is unpleasant, but it is much safer than carcinogenic Co or Pb or Hg or even Zn.
Copper is as toxic as nickel.

Quote: Originally posted by Microtek

searching for alternatives based on iron,

Is the oxidation of Fe(II) noticeable the complex to Fe(III) during storage?

Microtek - 23-1-2025 at 15:01

Not so far, but it has only been a few weeks. I'm not convinced that nickelcarbonyl cannot be formed. Varying amounts of CO is produced in most explosions, and the detonation products cool quickly. You are probably correct that equilibrium concentrations of the compound will be very low, but transient concentrations may be another matter.

Regarding Co, as far as I was able to find with just a little searching, cobalt is a probable carcinogen when it is bonded to tungsten carbide (cutting tools such as end mills), but only a possible carcinogen in other contexts.

"Based on chronic toxicity data in animals [Patty 1963], the original IDLH for cobalt metal dust and fume (20 mg Co/m3) is not being revised at this time. This may be a conservative value due to the lack of relevant acute toxicity data for workers." From https://www.cdc.gov/niosh/idlh/7440484.html

"Overall, these results show that repeated exposure to copper compounds results in an acute cellular response with no associated pathology and which fully resolved after the cessation of exposure." From https://www.sciencedirect.com/science/article/pii/S0300483X2...

"The revised IDLH for copper fume is 100 mg Cu/m3 based on an analogy to copper dusts and mists which have a revised IDLH of 100 mg Cu/m3. This may be a conservative value due to the lack of relevant acute toxicity data for workers exposed to concentrations above 100 mg Cu/m3" From https://www.cdc.gov/niosh/idlh/1317380.html

"The revised IDLH for nickel compounds is 10 mg Ni/m3 based on acute inhalation toxicity data in animals [NDRC 1943]. This may be a conservative value due to the lack of relevant acute inhalation toxicity data for workers. [Note: NIOSH recommends as part of its carcinogen policy that the “most protective” respirators be worn for nickel compounds at concentrations above 0.015 mg Ni/m3.]"
From https://www.cdc.gov/niosh/idlh/7440020.html

"The available toxicological data contain no evidence that an acute exposure to a high concentration of iron oxide dust and fume would impede escape or cause any irreversible health effects within 30 minutes. However, the revised IDLH for iron oxide dust and fume is 2,500 mg Fe/m3 based on being 500 times the NIOSH REL of 5 mg Fe/m3 (500 is an assigned protection factor for respirators and was used arbitrarily during the Standards Completion Program for deciding when the “most protective” respirators should be used for particulates)."

Thus it seems that nickel is ten times as toxic as copper but only two times as bad as cobalt. Iron is expectedly non-toxic (but ideally nothing other than air should be inhaled).

Laboratory of Liptakov - 24-1-2025 at 00:44

The whole breathing is based on the oxidation of iron. So a little extra dust won't hurt anyone. If we could create a primary substance with iron ions, it would be revolutionary. After all, Fe2O3 is a reliable fire accelerator..... :cool:

pdb - 24-1-2025 at 02:21

Be my guest !

In 2007, I planned to try Na[Fe(NT)₃(H₂O)₃] from NT and FeCl₂·4H₂O (example 2 of the patent), but I didn’t for some forgotten reason. That same year, Engager conducted an extensive investigation into NT synthesis and M-NT compounds, with no clear conclusion IIRC (see https://www.sciencemadness.org/whisper/viewthread.php?tid=81... and the following pages).

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Etanol - 24-1-2025 at 07:14

Quote: Originally posted by Microtek

Thus it seems that nickel is ten times as toxic as copper but only two times as bad as cobalt. Iron is expectedly non-toxic (but ideally nothing other than air should be inhaled).

Hm. You are right. It seems inhalation toxicity is different from the oral. I focused on the values for salts:
FeCl2 LD50=450mg/kg (oral,rat)
CuCl2 LD50=140mg/kg (oral,rat)
NiCl2 LD50=105mg/kg (oral,rat)
CoCl2 (hexahydrate?) LD50=80mg/kg (oral,rat)

It would be ideal to create a non-gigroscopic, poorly soluble, waterfree Fe(III) complex with fast DDT.

Microtek - 24-1-2025 at 10:09

Yes, that would be the optimal solution to this particular problem. It seems that most researchers are focusing on Fe(II) compounds rather than Fe(III), most likely because it forms complexes that are more suited as energetics. I admit that I don't know quite enough about complex chemistry to say exactly why that should be the case.
I would be more comfortable with Fe(III) compounds since it feels like they should be more stable. On the other hand, many Fe(II) salts are very stable when not in solution, so maybe oxidative decomposition won't necessarily be a problem.

At the moment I'm working on some Fe(II) complexes:

The old "Green primaries" one from Los Alamos, and also the [Fe(4-ATRI)n](ClO4)2 one I wrote about earlier. It may be possible to mix it with something (AgNT maybe) to make it DDT faster while keeping the sensitivity low.

MineMan - 26-1-2025 at 20:20

Quote: Originally posted by Microtek

I think the route through [Ni(NH3)6](ClO4)2 is your best bet. It is also a beautiful reaction in itself. There are a number of ways in the patent, have you tried following those without attempting to alter it in some way?
Why would you boil it for 20-25 minutes? I think you would risk decomposing the aminoguanidine which is not very stable in the presence of air.

By the way, I synthesized the copper complex, simply following the directions in the patent. It works as described and produces striking violet crystals. It is not as good as NAP and it remains to be seen how storage stable it is, but I can affirm that it is definitely not fake.

A user here posted showing that the copper salt is more brisant when confided in a sand crushing test. That post must have been deleted by the user. It is also less sensitive than NAP, not sure about uNAP. One user reported it is hard to make without excess ammonium perchlorate but I am sure that is easy for you to figure out. With crystal modification I think it shows more promise than NAP, but it precipitates right away so maybe the reaction needs to be done during sonificstion… as it is a room temp reaction. From what I have read it is DDTs in as little at 20mg poorly confined in foil.

Please let us know what you come up with! I would be anxious to hear about crystal modification because in all of the pictures the crystals are about .1mm in size. Reports indicate it stores well for years but there maybe increased sensitivity… I don’t know why, or if too many unreacted byproducts were left from a non ideal synth. I suppose any amount of copper oxide would increase sensitivity greatly as it does to all pyrotechnic mixtures.

Microtek - 27-1-2025 at 12:35

For right now, my attention is firmly focused on the Fe complexes of 4-ATRI with perchlorate anions. Regarding the CAP, I haven't done extensive tests with it, though since I have it on hand I could probably investigate a little.

ManyInterests - 29-1-2025 at 14:18

I decided to buy more aminoguanadine bicarbonate and... I noticed something. There is a significant difference in texture and color between my old purchase (which as far as I know has not changed since I got it some 2 and a half years ago) and the new one.

I pictured my stuff below and marked them. The fine white powder is the new purchase, while the one to its right is the old, it is chunky and not necessarily entirely white.

I won't be able to make another synth for another week or so, but if I make another synth and it all works out fine then I will be one very unhappy mad scientist... I almost bought from my original supplier, but I am glad I didn't. If it works I will buy another from the same guy I got this batch from and it should be happy, if a little poorer.

I hope the original ammonium perchlorate supply I have is good. Or maybe I will just use some of my lithium perchlorate (I don't think I'll be making Lithex, LL. sorry...) to make more confirmed ultra pure stuff.

Axt - 29-1-2025 at 22:06

My aminoguanidine is a buff coloured clumped fine powder that's spent 20 years in a hot tin shed. It works fine. Your problem is almost certainly your perchlorate.

Bis(aminoguanidine)nickel(II) bromate (NAB) is not stable. The two week old crystalline sample is now an inert brown powder. NAP stored the same, is fine after over a month.

Laboratory of Liptakov - 29-1-2025 at 23:32

ManyInterests......Lithex is too simple to make. There's nothing to mess with. You'll have much more trouble and fun making NAP......

NAP laser initiation

Nemo_Tenetur - 31-1-2025 at 03:13

According to the German patent, NAP is laser sensitive. I´ve done some testing and would like to share my first results with you.

The laser pointers were bought from chinese suppliers. The three small are rated with 200 milliwatt , whereas the big (strong) blue is rated with 2000 milliwatt output. Beam diameter between 3 and 5 millimeter, beam not focussed.

Only the strong blue was able to initiate my NAP samples. I want to emphazise that this is just a preliminary result with two NAP samples irradiated out of my wrist. Surely more and better testing is necessary to get reliable results.

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Microtek - 31-1-2025 at 08:39

I think the term "laser sensitive primary" is a little strange. If a laser is strong enough to burn things, it should obviously be able to set off most primaries eventually. I would guess that the term involves another, faster mechanism than simple radiative heating...

Nemo_Tenetur - 31-1-2025 at 09:00

I guess that the initiation of my NAP sample isn´t just thermal heating, if you compare the initiation velocity with the thermal ignition of a piece blackmatch/quickmatch:

https://www.amazon.de/dp/B0BP26RYYM?ref=ppx_yo2ov_dt_b_fed_a...

Microtek - 31-1-2025 at 14:52

From what I've read in the papers that talk of laser sensitive primaries, it seems to be micro- or nano second response times. To me, this indicates direct excitation of the chemical bonds as when a compound selectively absorbs only some wave lengths and therefore appears coloured. I haven't read any theoretical papers on this, it is simply inferred from the remarks in experimental works.

Laboratory of Liptakov - 1-2-2025 at 00:31

Thus principle a like excitation Cl + H gas mixture by laser
https://www.youtube.com/watch?v=BoC8LrNdnOc

Microtek - 1-2-2025 at 08:34

Yes, something like that.

ManyInterests - 15-2-2025 at 18:12

OK, I am prepping to make more perchlorates (as that might well be the main culprit) but before that, I finally got around to trying to do one more iNAP synthesis.

I measured out the reagents, but this time I am using a huge excess of isopropyl alcohol. Dugan said that he would use around 35 to 40ml. The last time I tried it I used 75ml and let it run at high heat/stirring for 12 minutes until the solvent ran low.

This time I am using 100ml of 91% isopropyl, and I will be letting it run for 20 minutes or until the solvent is starting to run below 30ml. Let's see what happens.

ManyInterests - 16-2-2025 at 06:42

IT WORKS!

I was probably swindled on my original aminoguandine bicarb!

The iNAP pops like a motherfucker!

YES! IT WORKS!

Edit: I made a 2nd synth. The first picture (lighter colored stuff) is the first synth and it works. I got around 1.22g of yield. The 2nd synth is the second one and it is currently drying. It reacted a little differently... it took 20 minutes to do it instead of 17.5 minutes. I think it is because I kept the doors and windows opened that lowered the temp, but I almost ran out of solvent and I did see some of the rose colored stuff starting to form. I hope it works just as well.

[Edited on 16-2-2025 by ManyInterests]

ManyInterests - 16-2-2025 at 15:58

Decided to do it a third time (because why not?) The 2nd time after it dried up was not as effective as the first, but it still popped. I am glad I am starting to get some results. I used 100ml of 91% IPA, but I think I used too much. The run time was a little over 20 minutes since something was up with the heating. I noticed that the reaction doesn't really start to kick in until the solvent is starting to run lower, so perhaps using too much of an excess is what caused it to get a little weaker.

This one was almost (and I mean almost) 20 minutes, but I had to let it out since it was almost fully dry. the color only started to get to the reddish/salmon rose towards the absolute end, which is concerning to me. but at any rate, I will wait for it to dry before trying some more. I will wait until tomorrow because I don't want to wake up any neighbors.

qwerty - 19-3-2025 at 02:04

To test longish term properties I have made INAP, UNAP and NAP according to the NinjaChemist procedure around back in september. All preperations were done wil NickelCarbonate, NH4ClO4 and Aminoguanidine bicarbonate.

For normal NAP synthesis the cold synthesis from prepepared solutions of nickelperchlorate and aminoguanidine perchlorate seemed to be the cleanest route for me.

Hey Buddy's synthesis was the quickest, but more care needs to be taken to prevent overflow from escaping carbon dioxide and ammonia.

After 3 months I noticed already that INAP's behaviour and the cold procedure NAP product was changing.

Were it DDT'd directly, shortly after it's preperation. After 3 months this was less evident and it showed more of a deflagration. This becomes even more prone after 6 month.

Hey Buddy's one pot boil synthesis however still DDT'd in very small quantities.

Anybody else observe the same behaviour.

Hey Buddy - 19-3-2025 at 17:23

Quote: Originally posted by qwerty

Anybody else observe the same behaviour.

I monitored a sample of iNAP and NAP from 2023 for degradation in storage in closed bottles, temp range -5 F to 115 F. I think it was around a year and half total time, two winters two summers. The samples were made from salts. There was a sample of NAP that turned dark reddish brown very early on, after only a few months, IIRC it was an early sample that was heated for a really long period of time in preparation. It was visually obvious that it changed in color pretty quickly. I still have this sample. It still detonates but is really sluggish and the performance is degraded. I had other samples of standard NAP and iNAP prepared from salts in the usual way. They didn't change over approximately a year and a half. I used them in detonators after I realized they were monitored beyond a year (which was my personal interest in the test).

qwerty - 21-3-2025 at 04:18

Thank you for your experience in this matter Hey Buddy! All samples I have are also made from salts. And as far as I can tell have not changed colour. But initial colour are different between the samples. Where the UNAP seemed relatively dark red. The NAP cold synthesis was more of a light red salmon colour. And the INAP was a really light salmon colour.

As to the preperation of INAP I have a theory where I think that the isopropanol is maybe not complexing but is helping to force the precipitation of NAP more quickly and thus causing a higher yield/finer product. But I still need to think of an experiment to test this theory.

Quote: Originally posted by Hey Buddy

Quote: Originally posted by qwerty

Anybody else observe the same behaviour.

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