| Pages:
1
..
12
13
14 |
Microtek
National Hazard
Posts: 921
Registered: 23-9-2002
Member Is Offline
Mood: No Mood
|
|
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
International Hazard
Posts: 1033
Registered: 29-3-2015
Member Is Offline
Mood: No Mood
|
|
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
National Hazard
Posts: 921
Registered: 23-9-2002
Member Is Offline
Mood: No Mood
|
|
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
National Hazard
Posts: 969
Registered: 19-5-2019
Member Is Offline
|
|
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
National Hazard
Posts: 867
Registered: 28-1-2003
Member Is Offline
Mood: No Mood
|
|
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
International Hazard
Posts: 1447
Registered: 2-9-2014
Location: Tel Aviv University
Member Is Offline
Mood: old jew
|
|
ManyInterests......Lithex is too simple to make. There's nothing to mess with. You'll have much more trouble and fun making NAP......
Development of primarily - secondary substances: CHP (2015) neutral CHP and Lithex (2022) Brightelite (2023) Nitrocelite and KC primer (2024) Diper
60 (2025)
|
|
|
Nemo_Tenetur
Hazard to Self
Posts: 70
Registered: 13-12-2023
Location: Germany
Member Is Offline
|
|
NAP laser initiation
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.
Attachment: Laser red.mp4 (2.9MB)
This file has been downloaded 86 times
Attachment: Laser green.mp4 (2.4MB)
This file has been downloaded 85 times
Attachment: Laser blue weak.mp4 (2.8MB)
This file has been downloaded 68 times
Attachment: Laser blue strong.mp4 (1.3MB)
This file has been downloaded 113 times
|
|
|
Microtek
National Hazard
Posts: 921
Registered: 23-9-2002
Member Is Offline
Mood: No Mood
|
|
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
Hazard to Self
Posts: 70
Registered: 13-12-2023
Location: Germany
Member Is Offline
|
|
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
National Hazard
Posts: 921
Registered: 23-9-2002
Member Is Offline
Mood: No Mood
|
|
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
International Hazard
Posts: 1447
Registered: 2-9-2014
Location: Tel Aviv University
Member Is Offline
Mood: old jew
|
|
Thus principle a like excitation Cl + H gas mixture by laser
https://www.youtube.com/watch?v=BoC8LrNdnOc
Development of primarily - secondary substances: CHP (2015) neutral CHP and Lithex (2022) Brightelite (2023) Nitrocelite and KC primer (2024) Diper
60 (2025)
|
|
|
Microtek
National Hazard
Posts: 921
Registered: 23-9-2002
Member Is Offline
Mood: No Mood
|
|
Yes, something like that.
|
|
|
ManyInterests
National Hazard
Posts: 969
Registered: 19-5-2019
Member Is Offline
|
|
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
National Hazard
Posts: 969
Registered: 19-5-2019
Member Is Offline
|
|
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
National Hazard
Posts: 969
Registered: 19-5-2019
Member Is Offline
|
|
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
Harmless
Posts: 4
Registered: 10-12-2024
Member Is Offline
|
|
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
Hazard to Others
Posts: 443
Registered: 3-11-2020
Location: Bushwhacker Country
Member Is Offline
|
|
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
Harmless
Posts: 4
Registered: 10-12-2024
Member Is Offline
|
|
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 |
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). |
|
|
|
ExcerptSix
Harmless
Posts: 4
Registered: 13-4-2025
Member Is Offline
|
|
Write up of my first attempt at (u)NAP
I tried following Dug's method as seen in his videos on the matter.
Aminoguanidine bicarbonate - 1g - purchased from china. It has a slight/medium ammonia smell. Could anyone tell me if that's normal?
Ammonium perchlorate - 0.86g - Made by reacting perchloric acid with aq. ammonia 25% solution and recrystalized twice.
Nickel carbonate - 0.43g - chemical supply store grade
-reagents were mixed together in a vessel
-30ml water was boiled in tall form beaker with magnetic stirring, covered with watchglass for reflux
-reagents were dumped together into refluxing water
-Mixture was allowed to react and reflux for over 10 minutes. Initially the color was green and then very slightly muddy. I expected to only need to
react it for abour 5-7 minutes but I ended up leaving it for perhaps close to 15.
-mixture was decanted into a new beaker and placed in a ultrasonic bath at ~20C for 10 minutes.
No crystals were precipitated. No change was observed. Slightly red/purple colored liquid.
Mixture was allowed to cool to room temp and left covered for an hour. No crystals were formed.
After 2-3+ hours very small needle like crystals were observed at the walls of the beaker.
The mixture was left to crystalize for further 6ish hours and then the crystals were broken loose from the walls of the beaker by hitting them with
the ultrasonic bath. Crystals were filtered and dried.
Final yield was 162mg - way less than I originally expected.
Tests on a aluminum foil detonated with a pop but no foil perforation was noticed.
Any ideas on what went wrong?
Does the synthesis of ammonium perchlorate seem sound?
What would be a good way to purify the aminoguanidine bicarb if the ammonia smell is not supposed to be there? I see that the solubility in water
isn't great.
[Edited on 15-4-2025 by ExcerptSix]
       
|
|
|
Etanol
Hazard to Others
Posts: 220
Registered: 27-2-2012
Member Is Offline
Mood: No Mood
|
|
Oh my god. NAP is water soluble. I'm tired of repeating this. The hot red solution should be evaporated until the first crystals appear, then cooled.
There is no need to recrystallize ammonium perchlorate prepared from pure reagents if you used indicator paper to measure pH.
There is no need to make ammonium perchlorate if you have perchloric acid. It would be more efficient to prepare aminoguanidine perchlorate and nickel
perchlorate to prepare NAP from this with good purity and yield.
Ultrasonic is useful at this
and this stage:
Ultrasonic is useless at this stage
How much unreacted nickel carbonate was left in the precipitate before decantation?
[Edited on 15-4-2025 by Etanol]
|
|
|
ExcerptSix
Harmless
Posts: 4
Registered: 13-4-2025
Member Is Offline
|
|
I have some ammonium perchlorate left so i'll try a few runs like that before giving the Nickel Perchlorate and Aminoguanidine perchlorate route a go.
The point of the ultrasonication after decantation(still hot solution) was to cool down the solution leading to precipitation and to affect the
crystal morphology leading to micro crystals. At least that was my understanding.
I don't understand how I would be running an ultrasonic bath while heating to a boil and stirring the solution as your first quote suggested.
Very little nickel carbonate was left before decantation. I didn't measure it but it was in the form of a fine sludge/powder and it looked less than
some of the videos i've seen.
Could you confirm that a slight ammonia smell is normal from the Aminoguanidine bicarb?
|
|
|
ExcerptSix
Harmless
Posts: 4
Registered: 13-4-2025
Member Is Offline
|
|
I did the same synth as my previous post.
15 minutes boiling. This time the mother liquor evaporated a bunch. After decanting I introduced the hot mixture to the ultrasonication bath for 10
minutes.
IT WORKED! Yield was 370mg uNAP. When heated from below on a piece of kitchen aluminum foil it detonates and blows away the foil.
This time the leftover nickel carbonate was quite a bit.
Does the leftover nickel carbonate mean that one or more of the other reagents were lacking? The aminoguanidine bicarb feels a bit wet and is in
clumps also the ammonia smell. Is anyone aware of a good way to purify it?
|
|
|
Etanol
Hazard to Others
Posts: 220
Registered: 27-2-2012
Member Is Offline
Mood: No Mood
|
|
| Quote: Originally posted by ExcerptSix |
I don't understand how I would be running an ultrasonic bath while heating to a boil and stirring the solution as your first quote suggested.
|
Ultrasonic heats the solution. +Hot wire
Unfortunately, not every ultrasonic bath is capable of working at high temperatures.
My Aminoguanidine bicarb has a slight smell of hydrazine, no ammonia.
|
|
|
ExcerptSix
Harmless
Posts: 4
Registered: 13-4-2025
Member Is Offline
|
|
I've ran quite a few uNAP synths using the salt method.
I'm usually getting around 350mg of uNAP for ever 1g AGu carbonate run with 25min of boiling.
My uNAP detonates with a loud crack when heated from below on aluminum foil and perforates the foil reliably.
When heated from above by either a blowtorch or an ember it detonates? with a pop with no foil perforation.
I've ran a few tests using a PETN det caps as they are outlined in Dugan Ashleys videos - namely a PT100 thermocouple casing OD 6mm ID 5.2mm.
Progressively pressed with an arbor press 3x250mg PETN. With the last secondary interface layer being pressed by hand with about 1.5kg pressure. The
primary is set off by a commercial e-match. The results for the uNAP initiation are as follows:
25mg uNAP lightly pressed on top - 0/2 caps managed to transfer the detonation to the PETN
25-30mg uNAP pressed/compacted into a 5mm OD / 3.4mm ID / 3mm length 3D printed bushing inserted against the PETN - 2/5 managed to transfer the
detonation to the PETN
55-60mg uNAP pressed/compacted into a 5mm OD / 3.4mm ID / 6mm length 3D printed bushing inserted against the PETN - 5/5 managed to transfer the
detonation to the PETN
I'm finding this surprising since from what I was reading I expected the minimum initiation quantity for uNAP to be 5-10mg and it appears that even
30mg isn't enough to reliably set off lightly pressed PETN.
The uNAP I've made is otherwise visually exactly what is expected.
[Edited on 21-4-2025 by ExcerptSix]
|
|
|
Microtek
National Hazard
Posts: 921
Registered: 23-9-2002
Member Is Offline
Mood: No Mood
|
|
Well, you probably have a lot of impurities in your NAP from the nickel carbonate. As Etanol says, you should eliminate that impurity by preparing the
perchlorate salts of both aminoguanidine and nickel (there is no need to isolate them - you can just use the solutions, but avoid having an excess of
perchloric acid as the low pH may prevent precipitation).
If you do it this way, the only species that isn't extremely soluble in water is NAP.
|
|
|
| Pages:
1
..
12
13
14 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
