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Laboratory of Liptakov
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A clear example is ETN, which ignites and burns with a long, narrow flame when heated from above. It almost always detonates when heated from below on
alu foil....
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Hey Buddy
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Quote: Originally posted by pdb  |
OK, so the explanation lies in the testing method. Although the bottom heating test is widely used on this forum, in my opinion, it is biased for
evaluating DDT. Heating samples of different energetic materials to their explosion temperatures will result in detonation much more often than if
they were exposed to a flame.
I’m not saying this test should be abandoned, but there should at least be a distinction between h(eat)DDT and f(lame)DDT. In this case, uNAP
exhibits hDDT but not fDDT, unlike some other primaries. However, these differences no longer matter when the charge is confined, as in a detonator.
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We are discussing two different examinations of a material with different purposes for the types of examinations.
Top and bottom heating are two ways to examine the response in a material to heat stimuli. Most materials (primary and secondary explosives), show a
different behavior depending on the way they are exposed to the heat stimuli.
In regards to top heating, it is a better method to use an ember from the end of a wooden punk or a hot wire, with small surface area rather than a
gas pressure torch flame that can move or throw the material. Gas torches also have a range of temperature depending on the distance of the material
to the heat source and the speed at which it is introduced to the heat. A burning ember transfers no heat until it is very close to the material, so
it is more of consistent way to probe with heat. A burning ember is a closer analogue to the spit of a fuze or hot bridgewire. The configuration of
the material when exposed to top heat affects its behavior to stimuli response. There is still a minor confinement effect going on beneath the
material where it sits on the medium being heated from above. If the material is pushed down into a depression even slightly, it affects the response
again. If the material is enclosed like in a tube or a washer, it affects the response further.
So top heating can be used to compare responses between materials as long as testing conditions are constant, but shouldnt be compared to bottom
heating, or used as the determination of the minimum masses to detonate a primary explosive. It is more accurate (IMO) to test minimum detonating
masses on a foil where their ability can be witnessed, or even better, as they are loaded into a device, such as a detonator.
The behavior of a material exposed to top heat doesn't have much correlation to how it will behave when presented to the end of a fuze spit or bridge
wire while confined in a detonator body. Top heating can't reveal minimum firing masses because materials will sometimes not detonate from top
heating, but the same material will detonate and transfer detonation to a secondary, if the same mass were loaded into a detonator.
Bottom heating (can potentially) reveal the minimum possible mass that will result in a detonation of a material. In this case, Foil or another medium
is only used to verify detonation is taking place. When the mass becomes so low that it no longer detonates, it will no longer perforate a foil. By
comparing materials in the same way, their minimum detonation masses can be evaluated.
Secondary explosives can be examined in the same way to approximate their minimum critical diameters. Such as ETN. Even if a secondary doesn't
detonate from heating but merely decomposes or deflagrates, it will usually reveal different response between top and bottom heat.
I hope that long response makes more clear my opinion. You can use any tests, to any standard you want. This is just the way I do it, or that I think
about the matter. Ultimately, these are only preliminary examinations. In application, they have to be validated in the particular detonator designs
they are intended for. The detonator design, particularly the interface from heat stimuli to primary, and interface from primary to secondary,
dramatically influences the behavior of the detonator.
Attachment: iNAP_Ember_Response.mp4 (2.6MB)
This file has been downloaded 65 times
[Edited on 8-12-2024 by Hey Buddy]
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pdb
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I hope my reply will be shorter....
I fully agree that a burning splinter disturbs the sample less than a blowtorch jet. But in this specific case, I just wanted to make a quick video
showing behaviors I was already familiar with, hence the faster choice of using the blowtorch I had on hand. Using a burning splinter wouldn't have
changed the demonstration.
Besides, this is just a hobby for me, and one that I've pursued for a long time. The xNAP interests me as a curiosity, not as a means to make
detonators, as I already have my own recipe for those. So, I'm not trying to make any elaborate correlations between these tests and xNAP's
suitability for detonator compositions.
In fact, I limit myself to comparing primaries based on two criteria: their fDDT and their power (dent in a metal plate). Nothing else (except, of
course, safety and storage), and that’s enough to keep me entertained.
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Hey Buddy
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| Quote: Originally posted by pdb | I hope my reply will be shorter....
I fully agree that a burning splinter disturbs the sample less than a blowtorch jet. But in this specific case, I just wanted to make a quick video
showing behaviors I was already familiar with, hence the faster choice of using the blowtorch I had on hand. Using a burning splinter wouldn't have
changed the demonstration.
Besides, this is just a hobby for me, and one that I've pursued for a long time. The xNAP interests me as a curiosity, not as a means to make
detonators, as I already have my own recipe for those. So, I'm not trying to make any elaborate correlations between these tests and xNAP's
suitability for detonator compositions.
In fact, I limit myself to comparing primaries based on two criteria: their fDDT and their power (dent in a metal plate). Nothing else (except, of
course, safety and storage), and that’s enough to keep me entertained. |
Understood. I always appreciate your work. I am referencing your R Salt paper you translated in another project right now. --I did not intend to frame
your research but share what I think about the topic of testing procedures. I assumed the response was invited. Apologies if out of line.
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Axt
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I'm just reiterating and reaffirming the discussion on page 7-8 here but I tried ultrasound and 800rpm precipitation. If anything the stirred solution
was slightly but negligibly smaller, I was rooting for the ultrasound as I like the novel but at least in this setup (ie. 100ml beaker placed in the
bath) it doesn't seem worth the trouble. It would be interesting to try it with other precipitates though like NTO which shows very different crystal
forms.
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Etanol
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| Quote: Originally posted by Hey Buddy |
OK, so the explanation lies in the testing method. Although the bottom heating test is widely used on this forum, in my opinion, it is biased for
evaluating DDT. Heating samples of different energetic materials to their explosion temperatures will result in detonation much more often than if
they were exposed to a flame. |
Hmm, I'm also used to evaluating DDT using the upper heating.
I repeated the tests with my NAP (without ultrasonic), which detonated from 15-20 mg at top heating.
I have to admit that with this method of testing (bottom heating), weighing less than 0.5 mg seems to be detonated. Less than 0.5 mg of the NAP makes
a dent on 0.1mm aluminum foil or a hole in the 0.015 mm foil.
[Edited on 10-12-2024 by Etanol]
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pdb
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Inspired by Axt's experiments, I wanted to see what strong stirring would do during the synthesis of DPNA in a diluted solution. By pushing my stirrer
to its maximum, 1200 rpm according to the manufacturer, I obtained a reduction in crystal size, but no change in their needle form. This is nothing
like the sand-like grains obtained with a very concentrated solution, which have the advantage of forming a free-flowing powder that is less sensitive
to mechanical stimuli compared to the needle version.
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Axt
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You should have revived the old diazonium topic for that pdb, but I like how you got it free flowing I remember that being an issue back then. Mine
was always the matted needle clumps.
What microscope are you using pdb? Mine struggles with reflected light images, it's a celestron pentaview. I'm not sure if it always struggled, I
cannot remember but it seems to be a software issue with the auto camera settings.
Bringing things back on topic here's an image of NAP from one of them cheap digital microscopes you see all over ebay and aliexpress. I used
vantablack as background on a slide, I thought it would be blacker but I like the slight shadow as it gives it depth.
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pdb
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Very beautiful image! In my opinion, with similar power, color and crystallography must have their say when collecting primaries...
I use a cheap Bresser microscope with poor lighting.
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Hey Buddy
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| Quote: Originally posted by Axt | You should have revived the old diazonium topic for that pdb, but I like how you got it free flowing I remember that being an issue back then. Mine
was always the matted needle clumps.
What microscope are you using pdb? Mine struggles with reflected light images, it's a celestron pentaview. I'm not sure if it always struggled, I
cannot remember but it seems to be a software issue with the auto camera settings.
Bringing things back on topic here's an image of NAP from one of them cheap digital microscopes you see all over ebay and aliexpress. I used
vantablack as background on a slide, I thought it would be blacker but I like the slight shadow as it gives it depth.
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This is what Im using, a cheap chinese "1500x" product. Your images are lot better than what I could produce. I would be curious what an iNAP image
would look like on your equipment.
[Edited on 13-12-2024 by Hey Buddy]
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Axt
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| Quote: Originally posted by Hey Buddy |
This is what Im using, a cheap chinese "1500x" product. Your images are lot better than what I could produce. I would be curious what an iNAP image
would look like on your equipment.
[Edited on 13-12-2024 by Hey Buddy] |
To clarify the 6 picture montage above was taken on the celestron pentaview, only the pic directly above was on the cheap "1500x" scope, with emphasis
on the quotation marks. They of course aren't 1500x unless you count opening it in an image editor and zooming into a few pixels. The montage pics are
all at 40x, if you zoom in too far everything starts looking the same and you cannot see an average size.
I had a look back through the first pages of this thread. I wouldn't be able to directly replicate what you are doing, at least not without too much
hassle. Perchlorate salts and nickel carbonate aren't available on this side of the world.
I guess there's 3 things that come to mind that could be going on in order of likelihood. 1] It's purely modifying the crystal morphology into
something less sensitive, its well known that small changes in morphology can have a dramatic effect on sensitivity. 2] It's oxidising the alcohol to
acetone and creating a hydrazone derivative by condensation with the AGu C-NH-N=C(CH3)2, partially replacing the AGu ligands. 3] IPA is able to
outweigh the dilute AGu and replace part of the ligands. Alcohols can form ligands and Ni(EtOH)6(ClO4)2 is a known complex but this is very unlikely
in aqueous solvents.
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MineMan
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Why no love for the copper QN diperchlorate? It only DDTs when confined, according to reports and is also less sensitive according to reports but
actually more brisant when confined.
During the reaction could copper oxide form making it more sensitive?
I am just shocked that primary is not getting more attention as the synth states it is done at room temp and immediately precipitates. A user posted a
few years ago showing it was more brisant than NAP.
I wonder if CAP could also be made uCAP, or not because it precipitates quite quickly according to reports.
One advantage is since it needs confinement to detonate, it would be safer for researchers to handle as any stray ignition will allow 1 gram to
deflagrate in an open cup instead of detonate like NAP, potentially saving a hand.
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Laboratory of Liptakov
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Mineman and I have the same opinion in terms of the properties of primary substances. That is, for an amateur researcher it is more advantageous (much
safer) to use deflagrating primary substances in air. Which are detonatable only in a closed metal cavity. Other researchers prefer instantly
detonating substances in paper or plastic cavities. It is a matter of opinion.
One camp is researchers who do not mind storing instantly detonating substances. Where 1g can cause permanent hearing damage. The other camp is
researchers who refuse to store even 1g of such a substance. That is me, MineMan, and we are certainly not alone in this opinion. After 1 month of
storing 0.1g of SA-DS, I disposed of this popular substance. I could not accept the fact that I was storing an instantly detonating primary substance.
From this fact arised CHP, Lithex, Cu8 and others substances. ....
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite and KC primer (2024)
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MineMan
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| Quote: Originally posted by Laboratory of Liptakov | Mineman and I have the same opinion in terms of the properties of primary substances. That is, for an amateur researcher it is more advantageous (much
safer) to use deflagrating primary substances in air. Which are detonatable only in a closed metal cavity. Other researchers prefer instantly
detonating substances in paper or plastic cavities. It is a matter of opinion.
One camp is researchers who do not mind storing instantly detonating substances. Where 1g can cause permanent hearing damage. The other camp is
researchers who refuse to store even 1g of such a substance. That is me, MineMan, and we are certainly not alone in this opinion. After 1 month of
storing 0.1g of SA-DS, I disposed of this popular substance. I could not accept the fact that I was storing an instantly detonating primary substance.
From this fact arised CHP, Lithex, Cu8 and others substances. ....
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CAP, according to reports will detonate in a plastic cavity, even in 20mg quantities. But open in the air or a jar, it has been reported that even 1
gram deflagrates. The question is could it be made into uCAP, would need someone’s opinion like micotek. From the pictures I saw the grains look
like small sugar. Maybe .1mm. The color of beauty rivals NAP.
But yes that is my philosophy LL, and not only for researchers but industry as well, why not be as safe as possible, when it is easy??
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Microtek
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I experimented a little with CAP, but found that it lost its potency over time. It may be that it was improperly dried or that some impurity made it
less storage stable, but I never investigated further. Then I got distracted by the carbohydrazide complexes.
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Explosive Socks
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Hello
I'd be grateful for some sources for CAP synthesis
I'm having trouble finding the abovementioned topic about CAP
Thank you gentlemen
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Etanol
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| Quote: Originally posted by Explosive Socks | Hello
I'd be grateful for some sources for CAP synthesis
I'm having trouble finding the abovementioned topic about CAP
Thank you gentlemen
|
Apparently, this refers to copper-aminoguanidine-perchlorate complex.
Analogy Nickel Aminoguanidine perchlorate (NAP) =>Copper Aminoguanidine Perchlorate (CAP).
The copper complex is dangerously unstable and for this reason cannot have practical application.
It decomposes with the release of nitrogen in hot water.
Violet substance is not a CAP, but mainly an intermediate product of the decomposition. Next, the decomposition occurs to yellow copper monoxide.
Even if it is possible to synthesize the CAP in a cold solution, based on its thermal instability, it can spontaneously explode when drying or
storage.
The problem of this substance is a combination of Cu(2+) and -N-NH2, not anion ClO4- or IO4-.
| Quote: Originally posted by Etanol |
Thank you. But apparently this is Fake. Copper aminoguanidine perchlorate cannot exist.
When trying to synthesize, aminoguanin perchlorate slowly oxidizes copper perchlorate in a Cu2O in an hot acidic environment and instantly does this
in a slightly alkaline environment. |
[Edited on 20-12-2024 by Etanol]
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Hey Buddy
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| Quote: Originally posted by Explosive Socks | Hello
I'd be grateful for some sources for CAP synthesis
I'm having trouble finding the abovementioned topic about CAP
Thank you gentlemen
|
The author of this granted permission to share:
"...I performed the copper synthesis, and even though it doesn't posses the performance of the nickel variants, I would argue it is the easiest of
them all to make (with the exception of the precursor copper perchlorate, which I want to share a simple method of manufacture with (since I already
had ammonium perchlorate)).
How I make ACP and the copper perchlorate for it.
To make the copper perchlorate: I used electrolysis. I made a divided cell using a terracotta pot to hold the anodelyte, in it is 200ml of distilled
water, 35g NH4ClO4 (all mixed together beforehand), and of course a copper pipe for the anode. For the cathodelyte, I simply used epsom salt, dH2O,
and a stainless steel cathode. Run the cell for 5 hours at 1.5A.
At this point there is a nice solid blue solution in the pot, filter it to get any particles out, and you're left with a roughly 16% (estimated)
solution of copper perchlorate.
Now for the ACP:
Measure out 12g of the copper solution made above, put it aside.
Measure out 1.5g of aminoguanidine bicarbonate, make sure the material is as fine as possible (no clumps, moves freely) add to this 10g of distilled
water, and stir well.
Now add the measured out copper solution to the AGBC solution (while the still stirring), start a timer. (all done at room temp)
At the end of 5 minutes, pour the solution thru a coffee filter, then rinse it a couple times with some IPA to cleanse any unreacted material and rid
most of the water.
THe resulting crystals are tiny, dark violet, pour very well, but I don't press them, merely put them in the end of a plastic straw initiated with an
electric match. In the open the powder just tends to burn, but with slight confinement, it will DDT. I've been using between 50-100mg..."
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MineMan
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| Quote: Originally posted by Etanol | | Quote: Originally posted by Explosive Socks | Hello
I'd be grateful for some sources for CAP synthesis
I'm having trouble finding the abovementioned topic about CAP
Thank you gentlemen
|
Apparently, this refers to copper-aminoguanidine-perchlorate complex.
Analogy Nickel Aminoguanidine perchlorate (NAP) =>Copper Aminoguanidine Perchlorate (CAP).
The copper complex is dangerously unstable and for this reason cannot have practical application.
It decomposes with the release of nitrogen in hot water.
Violet substance is not a CAP, but mainly an intermediate product of the decomposition. Next, the decomposition occurs to yellow copper monoxide.
Even if it is possible to synthesize the CAP in a cold solution, based on its thermal instability, it can spontaneously explode when drying or
storage.
The problem of this substance is a combination of Cu(2+) and -N-NH2, not anion ClO4- or IO4-.
| Quote: Originally posted by Etanol |
Thank you. But apparently this is Fake. Copper aminoguanidine perchlorate cannot exist.
When trying to synthesize, aminoguanin perchlorate slowly oxidizes copper perchlorate in a Cu2O in an hot acidic environment and instantly does this
in a slightly alkaline environment. |
[Edited on 20-12-2024 by Etanol] |
Do you have a source on this? Because it is not noted in the paper too which I unfortunately do not have a link on.
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MineMan
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I can’t find the post via the search engine. But someone in the last 5 years did a sand crush test of NAP vs CAP and CAP came out on top with higher
brisance. I believe they also compared the sensitivities. Does anyone remember this post, I want to say it was twell, but maybe he just showed
interest in these compounds.
I remember LL commenting on how it was a quality well done test.
I thought it was stand alone post, but maybe in a topic.
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Laboratory of Liptakov
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Let me remind you that if you already have Cu(ClO4)2, it is enough to mix it with 20% hexamine. This will give you a high-performance substance
designated as LL8. Later designated as Cu8. Hexamine is certainly more accessible than aminoguanidine carbonate. However, for research purposes (in
the sense of basic amateur research), CAP or NAP is just as interesting as Cu8.
http://www.sciencemadness.org/talk/viewthread.php?tid=158259
[Edited on 21-12-2024 by Laboratory of Liptakov]
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Laboratory of Liptakov
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Damn.....All the videos from the DUG channel are gone. There were nice tutorials on NAP and also on R - salt and much more. Too bad. But that happens
sometimes with chemistry channels on YouTube.
https://www.youtube.com/@duganashley1337/featured
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underground
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https://odysee.com/@DuganAshley:e?view=content
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Laboratory of Liptakov
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Thanks for the link, Underground. Unfortunately, the videos on this platform are almost worthless to me. Automatic translation doesn't work there.
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ManyInterests
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I am going to make my PbO2 anode tomorrow (everything is ready, I hope nothing goes wrong) to make perchlorates so I can have a steady supply of very
pure ammonium perchlorate, but given just how cold it is outside I don't think I can do an electrolysis at the moment, this means I need to improvise
to get this out of the way.
I got 20g of lithium perchlorate in order to make Lithex, but I learned that I can make ammonium perchlorate from it using ammonium carbonate. So I
used 5g of my LiClO4 to make 2.8g of ammonium perchlorate (I made some mistakes) that should be pure enough for anything.
I will be trying again for uNAP. I will try Dug's formula as is before doing anything else since I am certain that my previous attempt failed was due
to impurites of my ammonium perchlorate. Right now I am very confident in this perchlorate for it to work properly.
If anything else happens... I will have to try alternatives.
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