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MineMan
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Quote: Originally posted by KFeNAT  | | I used a homemade drop hammer for the test, relying on the impact of a steel ball fixed to the end of the shaft to sample, and the drop height was
determined by calipers, and the mass of the entire drop weight was exactly 600g. Unfortunately, there was no significant reduction in the sensitivity
of PVA-NAP in this test method. |
I don’t understand how it is the same sensitivity as HMTD and LA is even less so?
Reading papers CAP has a sensitivity of impact 20 less than LA which is reported at .1joules.
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KFeNAT
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| Quote: Originally posted by MineMan | | Quote: Originally posted by KFeNAT | | I used a homemade drop hammer for the test, relying on the impact of a steel ball fixed to the end of the shaft to sample, and the drop height was
determined by calipers, and the mass of the entire drop weight was exactly 600g. Unfortunately, there was no significant reduction in the sensitivity
of PVA-NAP in this test method. |
I don’t understand how it is the same sensitivity as HMTD and LA is even less so?
Reading papers CAP has a sensitivity of impact 20 less than LA which is reported at .1joules. |
As far as I know, there is only one case where LA is so sensitive, that is, the solution is prepared with little stirring, so that a LA with
significant needle-like crystals is obtained, which is not only extremely sensitive but also has a risk of self-explosion. But in fact, the
sensitivity of LA is not high when the process is correct, the LA I used in the control test above is just a product that always maintains high-speed
stirring during preparation, without adding any crystal control agent, and I have also tested the product with dextrin, and its sensitivity is lower
than that of pure LA
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Microtek
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IIRC, LA is not very sensitive to impact, but has quite high friction sensitivity.
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Clay Buster
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| Quote: Originally posted by Etanol | | Clay Buster, these tests do not show the NAP power/brisance relative to the LA, but the deflagration to detonation transition. Apparently, the NAP did
not detonate in all your tests. It is classic deflagration. |
All of the tests did easily transition to detonation. Those NAP tests that did not perforate the flashing did detonate.
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Clay Buster
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| Quote: Originally posted by MineMan | | Quote: Originally posted by Clay Buster |
Nickel Acetate from Nickel Carbonate. Have you tried this yet?
[Edited on 20-5-2025 by Clay Buster]
[Edited on 20-5-2025 by Clay Buster] |
I do not understand the use of Ni carbonate. It seems users here always report non reacted solids. I think the acetate form is superior from listening
to others. I assume if you start out with acetate there will be acetic acid… but maybe not enough for optimal yields. For carbonate I would expect
the addiction of acetic acid to help substantially. |
I tried the NAP water based synthesis with a small (5 ml) acetic acid. All I got was a nice green transparent solution that would not precipitate
upon cooling.
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Clay Buster
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Acetic Acid Addition
| Quote: Originally posted by Etanol | to KFeNAT,
Hmm, Its correctly that you were able to get NAP in a slightly acidic environment of acetic acid and then recrystallize it from acetic acid without
decomposing of NAP?
This is strange for me, because I tried to get NAP in the aqueous solution with ways:
Ni(ClO4)2+2AGu&CH3COOH=[Ni(AGu)2](ClO4)2+2CH3COOH
and
Ni(ClO4)2+2AGu&CH3COOH+2NH3=[Ni(AGu)2](ClO4)2+2CH3COOH4N
But both reactions do not go. Instead of NAP I received a green solution of NI(CLO4)2 in a slightly acidic environment and a blue solution of a nickel
complex with acetic acid in a neutral environment.
I tried the NAP synthesis with small amounts of acetic acid and got the same green solution with no crystallization.
[Edited on 31-5-2025 by Etanol] |
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Etanol
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Add 3-5% NaOH solution to pH8.
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qwerty
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Following on my theory of the forced precipitation of NAP from IPA i did the following experiment.
Prepare a batch of NAP from salts:
NiCO3 0,43gr
NH4ClO4 0,86gr
AG 1gr
Use 27ml of water for the boil.
After 10min of boiling I decanted the liquor from the unreacted nickel carbonate into 380ml of IPA previously chilled to ±5°C under stirring at
600rpm. Solution turned a salmon orange colour and immediate precipitate was observed. I let it sit for an additional 10minutes in the freezer then
filtered. Washed the filtrate with an addition 40ml of IPA and let it dry. Final yield was ±0,48gr.
The colour is almost identical to the INAP I previously prepared. Behaviour is identical to other NAP variants I prepared. So it may not be conclusive
that the IPA complexes but I personally doubt it.
[Edited on 18-6-2025 by qwerty]
  
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Axt
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I've posted this before, but I think it's plausible that boiling nickel perchlorate with IPA will result in some oxidising to acetone and thus forming
a hydrazone complex by condensing with aminoguanidine. If a chemical change is taking place that results in a lowering of vehemicity/sensitivity this
seems most likely. Thus, you wouldn't expect to see this effect from precipitation from cold IPA.
There is supporting evidence for this in the case of carbohydrazide, as attached. The low sensitivity hydrazone complex is formed by adding acetone to
the reaction. In the case of NAP the contaminating species would be H2N-C(=NH)-NH-N=C(CH3)2.
[Edited on 18-6-2025 by Axt]
Attachment: Copper carbohydrazide acetone complexes as colorants.pdf (139kB)
This file has been downloaded 136 times
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qwerty
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Interesting article Axt. I think I have missed that somewhere in the thread.
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sulfuric acid is the king
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Hey guys, how are yours Cu version tests going?
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Clay Buster
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Acetic Acid Addition with pH Pushed to ~8
So, to be clear on what you are suggesting. Do the NAP synthesis using water with a small amount of acetic acid, enough to get the NiCO3 to dissolve.
Once the synth is complete, adjust the solution to pH = 8 with NaOH.
Is this what you are suggesting?
Have you tried this approach? If so, what was your result?
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Etanol
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Yes, I tried this approach. However, I would like to wait for the evidence of other experimenters who would confirm or refute my opinion.
My opinion is the product is contaminated with [Ni[AGu]2] diacetate. It is weaker and has a longer DDT than clear NAP.
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Clay Buster
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NAP Produced with Acetic Acid
| Quote: Originally posted by Etanol |
Yes, I tried this approach. However, I would like to wait for the evidence of other experimenters who would confirm or refute my opinion.
My opinion is the product is contaminated with [Ni[AGu]2] diacetate. It is weaker and has a longer DDT than clear NAP. |
I was partially successful in producing small crystal NAP using acetic acid to convert the insoluble Nickel Carbonate to soluble Nickel Acetate on the
front end of the synthesis followed by addition of NaOH to pH= 9/10 on the back end. The wet NAP I produced shows the same appearance as the water
produced NAP I've prepared previously. A more detailed of the process I followed is provided below.
I weighed out 0.43 g Nickel Carbonate and 0.86 g Ammonium Perchlorate and placed both into a tall form 200 ml beaker with 25 ml of DH2O. I placed the
tall form beaker into a water bath on the hot plate and put a stir bar into the beaker. I set the temp at 99 C.
Sidebar: I use a hot water bath because, in a few of my previous NAP runs I've had the unfortunate experience of the boiling NAP solution "burp" with
some of the burps violent enough to eject the solution from the beaker. This usually occurs near the end of the boil as the solution is turning very
dark green. I believe there some type of reaction occurring at the interface of the beaker bottom and the boiling solution. My hot plate has a
temperature thermocouple but no rheostat; just full on or full off. So, the hot plate surface and the bottom of the beaker are getting pretty hot
near the end of the boil. The hot water bath provides enough thermal inertia to prevent the bottom of the beaker getting too hot.
Back to the synthesis: As the hot water bath and solution in the beaker are getting up to temperature I weighed out 1 g Aminoguanidine Bicarb (AGB)
but held off adding the AGB to the reaction beaker. I dripped in a weak solution of acetic acid into the reaction beaker until I got the pH down to
about 5. At this pH, the Nickel Carbonate begins to dissolve and the hot solution becomes almost transparent green. I let the Nickel Carbonate and
Ammonium Perchlorate get up to a light boil and slowly add the 1 g AGB. There is a reaction that occurs as the solution foams up to about 2/3s of the
beaker but quickly dies down back to a light boil. I boiled the solution for about 6 min and then added a NaOH solution dropwise to a pH of 8/9.
At 7.5 minutes, I turned off the heat and gravity filtered the hot solution collecting the filtrate in a 50 ml beaker. I placed a stir bar in the 50
ml beaker and placed the beaker into an ice bath with the stirrer running fast. I've found that aggressive stirring of the filtrate in an ice bath
causes the NAP to crash out of solution quickly in the form of very small crystals.
I got a very healthy NAP yield on this run. Photo of wet NAP below. I said above I was "partially successful" because I still had some unreacted
Nickel Carbonate in the filter paper from filtering the hot NAP solution. For my next attempt, I will use a bit more acetic acid and see if I can get
all of the Nickel Carbonate to go into solution as Nickel Acetate along with the Ammonium Perchlorate. I should see the green solution go completely
transparent at that point.
After the NAP dries, I'll test it to see if it is as forceful on aluminum flashing as the NAP I've produce previously.
NAP dried out and I tested it. I weighed out 10 mg and placed it on 0.010" aluminum flashing. Heated from underneath with a propane torch. Full
detonation and blew through the aluminum like the standard NAP I've produced. Photos below. I also compared this batch of NAP to the standard NAP I
have on the shelf. In all appearances, it is identical.
 
[Edited on 8-8-2025 by Clay Buster]
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Etanol
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It seems, aminoguanidine perchlorate is soluble in hot ethyl alcohol and acetone. Na2SO4, NaCl, Agu-sulphate and AGu-chloride is not.
How about this way?:
NiCO3+H2SO4(37%,water solution to pH5...4)=>NiSO4+CO2+H2O
NiSO4+2NaClO4*H2O(in water solution)=>Ni(ClO4)2+Na2SO4
=>(drying)=>(hot extraction with C2H5OH or acetone)=>Ni(ClO4)2(organic solution)
2AGuH2CO3+H2SO4(37%,water solution to pH5...4)=>(AGu)2H2SO4+H2O+CO2
(AGu)2H2SO4+2NaClO4*H2O(water solution)=>2AGuHClO4+Na2SO4
=>(drying)=>(hot extraction with C2H5OH or acetone)=>Ni(ClO4)2(organic solution)
Ni(ClO4)2+2AGuHClO4(10-20% excess)+2NaOH (to pH7,5...8)=>NAP+2NaClO4
Hot AGuHClO4 is dangerous! It do not form crystall, but melts. At high temp its melt explodes!
[Edited on 11-8-2025 by Etanol]
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Clay Buster
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NAP Produced from Perchlorate Reactants
| Quote: Originally posted by Etanol | It seems, aminoguanidine perchlorate is soluble in hot ethyl alcohol and acetone. Na2SO4, NaCl, Agu-sulphate and AGu-chloride is not.
How about this way?:
NiCO3+H2SO4(37%,water solution to pH5...4)=>NiSO4+CO2+H2O
NiSO4+2NaClO4*H2O(in water solution)=>Ni(ClO4)2+Na2SO4
=>(drying)=>(hot extraction with C2H5OH or acetone)=>Ni(ClO4)2(organic solution)
2AGuH2CO3+H2SO4(37%,water solution to pH5...4)=>(AGu)2H2SO4+H2O+CO2
(AGu)2H2SO4+2NaClO4*H2O(water solution)=>2AGuHClO4+Na2SO4
=>(drying)=>(hot extraction with C2H5OH or acetone)=>Ni(ClO4)2(organic solution)
Ni(ClO4)2+2AGuHClO4(10-20% excess)+2NaOH (to pH7,5...8)=>NAP+2NaClO4
Hot AGuHClO4 is dangerous! It do not form crystall, but melts. At high temp its melt explodes!
[Edited on 11-8-2025 by Etanol] |
I believe the route you propose will work and produce NAP. NAP has already been produced from a solution of Nickel Perchlorate and Aminoguanidine
Perchlorate. While the route you propose above should produce NAP, I think it is the long way around to produce NAP. You'll be using additional
reagents plus added processing steps that will result in losing some intermediate products along the way to NAP. I don't see any advantage in what
you propose.
What would be the advantage of preparing the perchlorate based reactants to get to NAP?
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Etanol
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Clear NAP without other anions impurity (CH3COO-),
without using of rare HClO4,
without using of rare Ni(ClO4)2,
regeneration of ClO4(-)
[Edited on 11-8-2025 by Etanol]
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Axt
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Thats essentially the same method I've used to make copper ethylenediamine bromate. Although the complex is formed before the ethanol extraction.
CuSO4.5H2O + 2NaBrO3 + 2C2H8N2 --> Cu(C2H8N2)2(BrO3)2.H2O + Na2SO4
Make a saturated solution, add ethanol, bring to boil, filter the sodium sulphate and cool to precipitate Cu(en)2(BrO3)2. It works with KClO3 too, but
in Cu(en)2(ClO3)2's case its very soluble in ethanol and needs to be evaporated out.
I think you are right in that for NAP, you'd want to form the complex after extracting the Ni(ClO4)2. Although you could try adding H2SO4/AGB/NaOH to
the initial slurry and see what gets extracted.
[Edited on 11-8-2025 by Axt]
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Clay Buster
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| Quote: Originally posted by Hey Buddy |
You can boil NH4ClO4 and NiX for a long time to produce Ni(ClO4)2*6H2O, the reaction for NAP doesnt begin until AGu ligand is added.
The whole thing is really simple.
[Edited on 29-5-2025 by Hey Buddy] |
I attempted to make iNAP again and, while somewhat successful, my yield was very poor. My experience with using IPA (91%) to synth NAP has been hit
and miss. Today was another miss.
I read through most of the 16 pages on this topic and ran across Hey Buddy's post above. I decided to try a slightly modified approach to the
aqueous NAP synth which appears to have been very successful. I made three batches using the process summarized below.
45 ml DH2O in a 150 ml tall form beaker placed on a hot plate with strong stirring. Temperature set to 97 degrees which on my hot plate gives a
continuous lightly rolling boil.
Add to the beaker 0.86 g Nickel Carbonate and 1.72 g Ammonium Perchlorate and boiled without AminoGuanidine Bicarb (AGB).
First synth boiled the first two components for 3 min then added 2 g AGB.
Second synth boiled the first two components for 5 min then added 2 g AGB.
Third synth boiled the first two components for 7 min then added 2 g AGB.
Prior to adding the AGB, the Nickel Carbonate and Ammonium Perchlorate in water make a minty green solution that is constant in color.
After adding the 2 g AGB, the reaction is very quick and the solution quickly turns darker green going to almost black within 2-3.5 min. The first
synth took the longest time to turn black at about 3.5 mins. The second synth took between 2.5 and 3 minutes to turn black. The third synth took
only about 2 min to turn black.
After adding the AGB I continued the boil for only 3.5 to 4 minutes as the solution color did not appear to darken further. I removed the beaker from
the hot plate and filtered the hot solution through a coffee filter into a 100 ml standard beaker.
The filtrate and 100 ml beaker with magnetic stirrer was placed into a cold water bath (2 - 5 C) and stirring was turn up to high speed (just below
splashing).
I'm pretty sure I pulled the 100 ml beaker out of the cold bath and stopped stirring too early. I placed the beaker into the fridge to further cool
and crystalize. Rather than getting the small crystal form of NAP, I got medium sized long needle crystal NAP on this first synth. But, the yield
was good and the color looks good. I tested an ~15 mg pile on some aluminum roof flashing and it detonated with sharp crack and shredded the
flashing.
The second synth, I left the beaker and solution in the cold water bath with very strong stirring until I saw the small NAP crystals form in the
solution (about 2-3 mins). I removed the beaker and placed it into the fridge.
The third synth was stirred and cooled as in the second synth.
I've found that with strong stirring in a cold water bath, I get a very small grain crystal NAP that appears to have the same power and detonation
characteristics of the large needle crystal NAP. Of course, than only works out if you leave the beaker in the bath with stirring long enough for the
small crystal formation (somewhere between a temp of 20 - 25 C).
I've also found that, once I see the small crystals form in the cooled stirred solution, I get a higher NAP yield if I place the solution beaker in
the fridge for 30 - 45 min. After the short stay in the fridge, I filtered the contents through another clean coffee filter to capture the NAP. I
also use a light IPA wash to clean out all the NAP crystals from the beaker and help dry the filtered NAP crystals a little quicker. The second and
third synths final filtrate was nearly colorless clear with only a very slight hint of color.
I still found residual Nickel Carbonate on the hot solution filter paper, Interestingly, the 3 minute pre-boil residual was still minty green but the
longer pre-boil residual was a much darker green on the 5 minute boil and nearly black on the 7 minute boil. It also appeared there was less residual
on the hot solution filter paper for the 7 min pre-boil.
Once the NAP dries out (tomorrow), I'll weigh the result and see what I got for a yield. If nothing else, pre-boiling the Nickel Carbonate and
Ammonium Perchlorate appears to speed up the reaction with AGB and the quick distinct color change provides some certainty that the NAP reaction has
completed.
 
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Clay Buster
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NAP Yields After Pre-Boiling Nickel Carbonate and AP
| Quote: Originally posted by Clay Buster |
Once the NAP dries out (tomorrow), I'll weigh the result and see what I got for a yield. If nothing else, pre-boiling the Nickel Carbonate and
Ammonium Perchlorate appears to speed up the reaction with AGB and the quick distinct color change provides some certainty that the NAP reaction has
completed.
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I weighed the dried NAP from the second and third synths and got the following.
5 min pre-boil 0.992g
7 min pre-boil 0.928 g
I was surprised by this result as the pile of NAP from the 7 min pre-boil, despite weighing less, was visibly larger by volume than the 5 min
pre-boil. Upon closer inspection of the two piles of NAP, it was apparent that the 7 min pre-boil NAP was a much finer grain almost powder compared
to the 5 min pre-boil NAP. Since both are crystallizations from true solutions, I attribute the grain size and density differences to the speed and
maybe duration of stirring while cooling/crystallization occurred. I did have strong/fast stirring on both but I purposefully had the stirring as
high as possible w/o splashing out the solution on the 7 min pre-boil batch. Takeaway here is that the crystallization and bulk density of the NAP
you produce is impacted by the energy you put into the solution as it is cooling/crystallizing. I believe this will be true whether you use strong
stirring or an ultra-sound bath. The photos below show the two batches side by side in identical glass bottles. The lower volume batch is the
heavier of the two, 5 min pre-boil batch.
On to the yield calc with a caveat. I've been retired for several years now and I'm a nuclear physicist not a chemist. However, I question if the
yield calcs I've seen in previous postings here are correct. One post I ran across by Hey Buddy said the following.
"Yield is ~.91 g which is low compared to other procedures, a 100% yield would be 2.96 g"
I'll summarize mine below and please show me where I'm wrong if I'm off base here.
The chemical formula for NAP is Ni(CH6N4)2(ClO4)2
Note this formula is slightly different than in the first posting of this thread. There are two aminoguanidine molecules in the formula above.
However, the chemical formula above is consistent with the patent linked below.
https://patents.google.com/patent/EP2450330A2/en
and it is consistent with the chemical name in the patent.
nickel (II) di(monoaminoguanidine) diperchlorate
I calculate the molar mass at 405.81 g/mol
Using Nickel Carbonate, Ammonium Perchlorate, and Aminoguanidine Bicarb (AGB) to produce NAP should therefore look something like the following.
Ni(CO3) + 2(NH4ClO4) + 2(CH6N4H2CO3) = Ni(CH6N4)2(ClO4)2 +2(H2CO3)
In the reaction, the bicarb may remain in solution or may break down to water and carbon dioxide. Given the pH values I've measured, I suspect much
of the bicarb remains in solution. I believe most of the NH4 off gases during the reaction.
Calculating the yield based on 2 g AGB should look like this.
2 mol of AGB produces 1 mol NAP at 100% yield
AGB molar mass = 136.11 g/mol
I used 2 g AGB and got 0.992 g NAP
(2 g AGB)/(136.11 g/mol) = 0.014694 mol AGB
(0.992 g NAP)/(405.81 g/mol) = 0.002444 mol NAP
Since I need two mol of AGB to produce one mol of NAP, my molar yield is
(2 x 0.002444)/0.014694 = 33.3%
Doing the math in mass (vs mols) results in 1 g of AGB = 1.491 g NAP at 100% yield.
Let me know if I didn't get this correct.
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ExcerptSix
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Seeing that synth reports are still a thing on the subject I'll write up my last two synths using HClO4 since I have it.
I'm looking at my reagents the following way:
-Basic Nickel Carbonate (most nickel carbonate is basic, and mine being from the chem store it's stated as such) - Ni4CO3(OH)6(H2O)2 - 432.852 g/mol
-Aminoguanidine bicarbonate AGB - C2H8N4O3 - 136.11 g/mol
-HClO4 - 70% lab grade - 100.46 g/mol
For the first try I was going for 20mmol scale
A - Ni4CO3(OH)6(H2O)2 + 8HClO4 = 4Ni(ClO4)2
so for 20mmol of Ni(ClO4)2 I used :
-5mmol(2.164g) Ni4CO3(OH)6(H2O)2
-40mmol(4.018g) HClO4 and since mine is 70% - 4.018/(0.7*1.6713) = 3.434ml
B - AGu perchlorate 40mmol
-AGB 40mmol - 5.444g
-HClO4 - due to a typo during calculations I used 2.339ml
-A and B were carried out in two beakers with 50ml RO water each. A was clear green liquid after addition of acid and for once i didn't have any
undissolved nickel carbonate.
-After addition mixture is light green to dark green
-Under stirring and hotplate set at 160C pH balancing with 25% aq ammonia to 7.5-8 pH the mixture turned black.
-Boiled under stirring for 10minutes
-Crystallization under ultrasonic bath with addition of ice to keep the temp of the bath from getting too hot.
-Yield was 4.797g. Crystals look darker and seem to be larger than previous synthesis with ammonium perchlorate which yielded under 500mg per synth.
I'm theorizing that my ultrasonic bath was underpowered for the mass of crystallization going on or perhaps it crystalized too fast?
Second attempt at 10mmol
-basic nickel carbonate - 1.082g
-HClO4 70% - 1.717ml
-25ml water
-AGB - was to be 2.722g but i read somewhere in the thread that a little excess would be good so I used 3g
-HClO4 70% - 1.7ml
-25ml water
-When adding acid to AGB not all seemed to dissolve. When added to the nickel beaker CO2 was released so it seemed that there wasn't enough acid in
the AGB beaker and there was some unreacted AGB which reacted when combined.
-ph balanced to 7.5-8 pH mixture turned dark green then black
-boiled under stirring for 8minutes
-Ultrasonicated in water, after a minute or two with no precipitation i noticed what looked to be undissolved nickel carbonate at the bottom.
-I decanted the still hot/warm black liquid to a new beaker. I could not see the undissolved solid in either beaker. maybe i was imagining?
-Continued the ultrasonic bath and the precipitation formed.
-Yield was 2.7938g. Crystals look slightly lighter in color and a bit finer than the first try but no real way to measure.
Comparing to my previous sub 500mg ultrasonicated yields it looks as if the smaller yields had a lighter color and are perhaps finer crystals.
Colors of the photo came out a bit wonky but the sample containers are as follows from left to right - Oldest batches , 20mmol , 10mmol.
Would a higher power sonication risk breaking the beakers?
Seems like I always need to add aq ammonia to turn the mixture dark. Is it the same for the rest of HClO4 users?
Would slower or faster cooling in the sonication be better for finer crystals?
I also noticed changes of the vibration of the beaker in relation to the position in the bath so the whole thing is a little fiddly for repeatability.
Perhaps I'm not always getting the excitation of the mixture in the same way.
I think the next attempt I'll try to cool under fast stirring in an ice bath and compare since I don't have a stronger ultrasonic cleaner.
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ExcerptSix
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Looking at salt synth, 20 mmol and 10mmol through a microscope with the same magnification:
Salt:
 
20mmol scale:
 
10mmol scale:
 
Taken through x40 objective and x10 eyepiece.
Salt synths yielded around 300-400mg. Clearly with a smaller scale sonication worked better although the largest crystals in all samples looked to
have around the same diameter. I'm trying to think up a good empirical way to test friction sensitivity between the samples.
[Edited on 4-10-2025 by ExcerptSix]
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pdb
Hazard to Others
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Registered: 8-4-2004
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A new publication on NAP
Articles on NAP are rare enough that they're worth pointing out. Here is one that came out a month ago and thus is unfortunately not available online
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https://onlinelibrary.wiley.com/doi/10.1002/prep.70039
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Axt
National Hazard
Posts: 945
Registered: 28-1-2003
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Supporting info presents their preparation, there's also raw VOD data but that's too hard to decipher. I'm sure someone will buy it heh.
The synthesis procedure was as follows:
For each batch, 1.4g (10mmol) of Aminoguanidine bicarbonate was dissolved into 25ml of distilled water into a beaker with continuous stirring, at room
temperature. 2g (12mmol) of 60% perchloric acid was added to the solution, and stirring kept until the CO2 formation stopped and the solution was free
of visible gas bubbles. Then 1.6g (4.4mmol) of Nickel perchlorate hexahydrate were added.
At this point, the patent mentions that crystals start to form “in a few hours”. However, for us this was not the case, and adjusting the pH of
the solution was the only thing that seemed to make the crystals form. The pH adjustment was made by adding dilute NaOH solution dropwise, and
checking the pH at each level. The adding of NaOH changes the solution’s color from green to blue, and, when a pH of 7 is achieved, red crystals
start to immediately precipitate. The formation of the crystals raises the pH of the solution again, which self-limits the quantity of final product
obtained, if no subsequent pH adjusting is done. The yields were always greater than 70% (1.2g of NAP). To get the maximum yield without overshooting
the pH and start favorizing the formation of Ni(OH)2, multiple filtrations of the crystals were made and then readjustments of the pH for the filtered
solution. Using this method yields as high as 90% were obtained.
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ManyInterests
International Hazard
Posts: 1019
Registered: 19-5-2019
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I want to mention that I did use some of the iNAP I made a few months ago for a few more detonators to test, and they worked perfectly. While this
isn't much on their synthesis, It does appear that NAP is quite stable for storage.
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