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pdb
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Nitrobenzenediazonium perchlorate vs NAP
Following a series of tests, here is my assessment:
Without confinement, nitrobenzenediazonium perchlorate is more "vehemic" than NAP (in fact, it is more vehemic than all other primaries I have
prepared). However, under confinement, NAP surpasses it in power, in terms of mechanical effects (though I cannot comment on its brisance).
Both compounds excel in initiating HE. NAP is therefore a serious alternative for detonators: its synthesis does not require exotic reagents, and it
is reputed to be remarkably insensitive to mechanical stimuli for a primary, which is a significant characteristic. However, this is based on the
experience of us amateurs, and I am unaware of any publications providing quantitative measurements. That said, al least it does not have the
sensitivity of the diazonium compound, which is not far from that of AgCNO (this is why I switched to AgN3).
On the other hand, questions arise regarding its long-term stability, given that NAP is a relatively new compound and is known to have a weakness in
the presence of water and air. I still have diazonium from about fifteen years ago that remains unchanged. Reproducibility is also an issue. Even when
sticking to a single synthesis method (water, NiO and HClO4), one can never be entirely certain of obtaining the same product from one batch to
another. Neutralizing HClO4 with NaOH causes NAP to precipitate instantly, but dosing is challenging (pH): too much leads to partial decomposition
(and the NAP is contaminated with a black substance), while too little reduces the yield. NH4OH has a more controllable, gradual effect, but it’s to
the point where it’s unclear when the reaction is complete: sometimes, the filtrate obtained after 4 hours or more continues to produce NAP in
substantial quantities. The same questions arise for methods starting from salts..
To summarize, NAP is an extremely interesting new primary, but it still requires rigorous feedback and more experience to build confidence
definivively.
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Clay Buster
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Large Crystal NAP Synthesis
I am a new member on this board. However, I've been reading postings on this board for about a year. I finally decided to attempt synthesis of NAP a
few days ago and thought I'd share that experience and the results.
I found the synthesis, using the approach outlined by "Hey Buddy", to be very straight forward. I successfully prepared large crystal NAP, small
crystal NAP (stirred), and iNAP (IPA) using Nickel Carbonate, Aminoguanidine Bicarb, and Ammonium Perchlorate in stoichiometric quantities.
I prepared large crystal NAP by placing all three reactants into 30 ml of boiling dH2O. The initial foaming was significant almost to the point of
overflowing the beaker. The mixture immediately turned light green, then to a dark green, and near the end of the 7 minute boil, to a dark nearly
transparent liquid with some non-reacted material swirling around the bottom. I gravity filtered the mixture hot. I noted there was a significant
amount of non-reacted material on the filter paper. The non-reacted material appeared to be nickel carbonate with a few pills of amino guanidine
bicarb. I allowed the dark reddish filtrate to stand w/o stirring or agitation with one deviation from Hey Buddy's approach. I forced the NAP to
crystallize quickly by placing the filtrate in a refrigerator at 3-4 degrees Celsius. Understanding long exposure of NAP to liquid water would likely
reduce yield and introduce non-reactive degradation products, I chose to speed up the crystallization of NAP out of solution. Quick crystallization
may also produce smaller crystals than would slow crystallization. Seen with my naked eyes (admittedly old), the resulting NAP crystals are small
pointed rods with the largest being on the order of 1mm in length. The first photo below shows the large crystal NAP on filter paper. I did not
weigh the resultant NAP to determine a yield.
I did test the large crystal NAP after drying by placing a small amount on a piece of aluminum roof flashing. The flashing is 0.010" in thickness,
substantially thicker than aluminum foil. Hence, the quantity of NAP tested was roughly the size of the head of the Q-Tip shown in the second photo
for reference. Heated from underneath the flashing, the NAP detonated with a loud crack and made a substantial sized hole in the flashing as shown in
the third photo. Note the third photo is turned 180 degrees from the second. Yes, I was wearing PPE (welding gloves, face shield, and muffs).
I could find no residue around the hole in the flashing or on the curled fingers on the underside of the flashing. Very clean detonation.
I'll add the small crystal NAP synthesis and the iNAP synthesis results in separate posts to prevent this from getting too long.
  
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Clay Buster
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Small Crystal NAP Synthesis
In the first synthesis (Large Crystal NAP), I noted significant non-reacted reagents remaining on the filter paper with some of it in small
pills/clumps. For this synthesis, I first ground/crushed and fully mixed the three reactants together dry hoping to more fully react the reagents in
the process. In addition, I started the synthesis with the dH2O at 85 degrees Celsius (not boiling) with intent to get a more complete reaction.
When I added the reagents, there was fizzing but no appreciable foaming. With vigorous magnetic stirring, the solution initially turned light green
as before but turned to a darker green very slowly. After 7 mins at 85 degrees, I reset the temperature to 100 degrees and boiled the solution for
another 5 minutes and the mixture turned to a dark semi-transparent liquid with some non-reacted components swirling around.
As before, I gravity filtered the mixture hot. The filtrate was a dark reddish almost black transparent liquid. Non-reacted solids on the filter
paper appeared to be almost entirely green Nickel Carbonate with only very small traces of white pills of what I assume was Aminoquanidine Bicarb.
I forced the crystallization again with the beaker in an ice water bath this time with vigorous stirring using the magnetic stirrer. I don't know the
rpm as my hotplate/stirrer has a simple rheostat for stirrer speed. Fine red crystals formed shortly after placing the beaker in the ice water bath.
After about 10 minutes of vigorous stirring I placed the beaker in the refrigerator for about 10 minutes. I removed the beaker from the refrigerator
and found the NAP crystals had all accumulated on the bottom with a nearly colorless aqueous solution on top. I decanted most of the water then
filtered the NAP and remaining water. I used a small amount of IPA to rinse the remaining NAP from the beaker and wash the filtered NAP.
The first photo below shows the resultant small crystal NAP on the filter paper. The crystals appear to have a very fine sand like texture. Almost a
powder consistency but under a strong light, there is some reflecting of light that indicates at least some of the material is crystalline.
I did weigh the NAP produced in this synthesis and got a net of 0.78 g. Not a great yield as I know others have gotten 1 g or more.
I also tested this small crystal NAP again using aluminum roof flashing (0.010"). The second and third photos below show the pre test and post test.
This small crystal NAP detonated with the same sharp crack as the large crystal NAP test and left a hole in the flashing. The hole and the aluminum
flower petals on the reverse had no visible residue from the detonation.
  
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Clay Buster
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Acetic Acid
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]
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Clay Buster
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INAP Synthesis
I followed essentially the same process using 91% IPA instead of distilled water up to the point of the iNAP dropping out of solution. Near the end
of the 7.5 min boiling period, iNAP began to form on the top of the boiling IPA. Using IPA, there is no solution to filter and no filtrate to cool
for crystallization. After 7.5 min I took the beaker of the heater/stirrer and let it set to cool to room temp. The salmon colored iNAP settled in
the bottom of the beaker. I decanted off most of the liquid sitting on top then put the iNAP and remaining IPA through a gravity filter. The first
photo below shows the wet iNAP on the filter paper. Because of the IPA used as the solvent (reaction medium?), the iNAP dries quickly and did require
crushing the mass into powder gently with a toothpick. There was some non-reacted Nickel Carbonate and a few white pills of aminoguanidine bicarb
mixed in with the iNAP. The iNAP yield was much higher than the NAP prepared with water. I'd estimate double the yield I got for the water based
NAP.
I tested a portion of the iNAP after drying. The second photo below is pre-detonation and the third photo post detonation. I did not weigh the iNAP
amount tested but I'd estimate around 50 mg. Since this synthesis and test, I did get a better scale that reads out in milligrams. I'm planning to
test the three NAP forms against equivalent amounts of lead Azide in the next couple of days
  
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Clay Buster
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NAP vs LA
After testing the three types of NAP I synthesized (large crystal, small crystal, and iNAP), I questioned whether NAP provides the same power/brisance
as Lead Azide (LA) which I've synthesized previously. The iNAP I prepared seemed noticeably low on power. I made up a few test coupons out of
0.010" aluminum roof flashing. I started by testing small quantities of LA to find the minimum quantity of LA that would penetrate the test coupons
in open air. Unfortunately, I failed to find the minimum. My scale will read down to 1 mg but I'm pretty sure the accuracy for determining an
absolute mass fades below 10 mg. The first 9 photos below show the test coupons using 25 mg, 12 mg, and 6 mg of LA. The 6 mg charge had no trouble
perforating the aluminum flashing.
Photos 10 and 11 show the pre and post test using 6 mg of large crystal NAP. The detonation left a sizeable dent in the test coupon but did not break
through.
Photos 12 and 13 show the pre and post test using 10 mg of small crystal NAP. Again a sizeable dent, slightly deeper than photo 11, but did not break
through the coupon.
Photos 14 and 15 show the pre and post test using 20 mg of iNAP. The iNAP detonation left a larger diameter dent in the test coupon of roughly the
same depth as the other two NAP tests.
Making any concrete conclusions based on these simple tests is tough. But I'll go out on a limb and present what I believe I can take away from this.
1. On an equivalent weight basis, it appears the Lead Azide delivers more power and brisance than does NAP in any form.
2. The iNAP I prepared is significantly lower in brisance/power compared to Lead Azide as a 20 mg charge of iNAP would not penetrate the test coupon
while 6 mg of LA did so easily.
I'd like to know if anyone else has made back to back comparisons of NAP performance vs other common initiators or primary explosives. If so, please
share.
           
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Etanol
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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.
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Microtek
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I've said this before, but will repeat here:
The usual purpose of a primary is to initiate a base charge, so the value of primaries should be based on minimun priming charge to set off a standard
secondary in a standard blasting cap configuration. I realize perforation tests are much easier to do, but I think it somewhat misses the mark
(although there is a decent correlation between micro scale power and initiation performance).
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Laboratory of Liptakov
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Although there is a correlation between micro scale power and initiation performance, testing on thin aluminium plate are irelevant.
For example mixtures with oxidizers on base NaH2PO2 or base lead phosphite as reduction agent show incredible hole in thin aluminium plate. But in
thick steel cavity at 300 mg is impossible initiation ETN with them. Therefore are important words from Microtec. Reliability in the assembly
(cavity) is crucial as the NAP will be used to initiate secondary materials. The same applies to CHP and many other primary-secondary mixtures. On air
almost nothing, but in cavity initiation properties are observed....
Development of primarily - secondary substances: CHP (2015) neutral CHP and Lithex (2022) Brightelite (2023) Nitrocelite and KC primer (2024) Diper
60 (2025)
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MineMan
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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.
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ManyInterests
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I tested out several detonators using various grades of iNAP that I made, and all worked quite well to fully detonate various charges in the blasting
caps. I used ETN:RDX, ETN ETN, plain ETN, and an ETNETN:RDX charge(65:17.5:17.5 ratio) in the tube, they all worked very well, blasting
apart the fence brackets I used for witness plates. I deleted the pictures, but I am very satisfied with the result.
the mention that lead azide would be superior might be true. But I never found any NAP complex, whether it is the native form or uNAP or iNAP to
simply not detonate. iNAP is not as powerful or brisant as uNAP, but iNAP is MUCH safer to handle than uNAP and also a world of safety from handling
an extremely sensitive material such as lead azide.
I used 0.075g of what I considered the 'better' grade of iNAP for my detonators, and 0.10g of poorer grade, but both worked perfectly to fully
detonate the secondaries in the cap, and that is what is important. I was able to tightly pack (by hand, I tried to use a makeshift press, but I am
not sure if it worked all that well) 1.5g of secondary, which should be enough for any charge.
So while LA is probably the superior overall, in terms of ease of manufacture and safe handling I would put uNAP or iNAP above it, and it isn't weak
by any stretch of the imagination.
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Kwentino
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Amount of vinegar?
Hello,
What would, in your opinion, be a good proportion of acetic acid instead of water? I have glacial acetic acid.
And I can confirm some unreacted Ni Carbonate is nearly always present.
Thanks in advance
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Hey Buddy
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The whole purpose of using nickel carbonate is to make NAP from commercially available and cheap reagents, which are dry-state, which can be ordered
in the mail (in USA). NiCO3, NH4ClO4, AGuHCO3. There is no benefit to using salts to produce it, if it requires an operation to prepare the salts in
the first place. The perchlorate anion is already mandatory to produce NAP. It is much higher yielding and equally time consuming to just use
perchloric acid or prepare Ni(ClO4)2*6H2O, with an acid or metathesis. If you are going to take the time to prepare an acetate, it would be more
logical to prepare a perchlorate. 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. There is no reason to overcomplicate things, unless it's for novelty. If you must use salt method, understand it is
just for simplification, it isnt efficient or high yield. People complaining about NAP yields or undissolved nickel is just confusing. They are
missing the point. It's is a high power primary that can be prepared in the field with boiling water in a procedure simplified beyond even crude
peroxide production and with less time in the operation. Just a mix of salts boiled and dried in short time. There isn't anything else like that Im
aware of. HMTD takes even longer to prepare. If not doing NAP in the expedient method, why not take the time to prepare with perchloric acid instead
of attempting other anions that arent in the target complex?
[Edited on 29-5-2025 by Hey Buddy]
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KFeNAT
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Perhaps crystal control agents could be used to alter the crystal morphology
By using a solution containing PVA and acetic acid to recrystallize NAP, or by adding PVA to the solution during preparation, sand-like and
short-rod-like crystals can be obtained. Compared with ordinary NAP, iNAP or ethanol solution NAP, it has better fluidity and is easier to charge
non-standard-sized micro-detonators. The sensitivity is also reduced. The amount of PVA added is 0.1%-0.01% of the solution mass. The specific process
needs to be further explored. In principle, other crystal controllers for needle-shaped crystals are likely to be effective.
         
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MineMan
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| Quote: Originally posted by KFeNAT | | By using a solution containing PVA and acetic acid to recrystallize NAP, or by adding PVA to the solution during preparation, sand-like and
short-rod-like crystals can be obtained. Compared with ordinary NAP, iNAP or ethanol solution NAP, it has better fluidity and is easier to charge
non-standard-sized micro-detonators. The sensitivity is also reduced. The amount of PVA added is 0.1%-0.01% of the solution mass. The specific process
needs to be further explored. In principle, other crystal controllers for needle-shaped crystals are likely to be effective. |
This is really interesting! Can you share more on your findings?! For industry bulk density and flow ability are the two bigs for primary explosives!
Perhaps if 1 percent was used it would coat the crystals even more and make them far less sensitive! Can you try it with 1 percent and also try
rapidly cooling the solution with stirring and an ice bath?
[Edited on 30-5-2025 by MineMan]
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KFeNAT
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| Quote: Originally posted by MineMan | | Quote: Originally posted by KFeNAT | | By using a solution containing PVA and acetic acid to recrystallize NAP, or by adding PVA to the solution during preparation, sand-like and
short-rod-like crystals can be obtained. Compared with ordinary NAP, iNAP or ethanol solution NAP, it has better fluidity and is easier to charge
non-standard-sized micro-detonators. The sensitivity is also reduced. The amount of PVA added is 0.1%-0.01% of the solution mass. The specific process
needs to be further explored. In principle, other crystal controllers for needle-shaped crystals are likely to be effective. |
This is really interesting! Can you share more on your findings?! For industry bulk density and flow ability are the two bigs for primary explosives!
Perhaps if 1 percent was used it would coat the crystals even more and make them far less sensitive! Can you try it with 1 percent and also try
rapidly cooling the solution with stirring and an ice bath?
[Edited on 30-5-2025 by MineMan] |
What we know now is that when the PVA content exceeds 0.3%, if the precipitation speed is fast, cotton-like products may appear. This may be caused by
the small crystal particles and the adhesion between each other. Too high a concentration of PVA will inhibit the growth of crystals in all
directions, and only very small particles may be obtained, which will make the fluidity of the product very poor.
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Etanol
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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.
[Edited on 31-5-2025 by Etanol]
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KFeNAT
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| 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.
[Edited on 31-5-2025 by Etanol] |
Actually, you are only a little away from success. The essence of recrystallization in acetic acid solution is to disassemble NAP into Ni(ClO4)2 and
aminoguanidine acetate, and then add alkali to make aminoguanidine recombined with Ni2+ to generate NAP. However, it is important not to use ammonia
to neutralize acetic acid, because the alkalinity of NH3 is not significantly greater than that of aminoguanidine. Secondly, the concentration of
commercial ammonia water is not very precise, which is not conducive to accurate control of dosage, and the solubility of Ni(NH3)6(ClO4)2 is not
particularly high. Therefore, if ammonia water is used for neutralization, NH3 is very easy to act as an impurity and compete with aminoguanidine for
the binding of Ni2+, resulting in a large amount of nickel-ammonia complex in the product. Therefore, NaOH must be used to obtain a purer product, and
the amount of NaOH required should be slightly less than the amount of acetic acid in the solution. Avoiding excessive alkalinity is the key to
preventing the solution from oxidizing to produce black substances. At the same time, additional perchlorate can also be added to the solution to
reduce the solubility of NAP in it.
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Axt
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I have formed the acetate, but for the reason of producing a "universal solution" that can be used to precipitate whatever counterion one wishes just
by adding its neutral salt, whether it be NaClO4, NaNO3, NaBrO3 etc. The acetate does seem to be significantly more soluble than the rest. I aimed to
try chlorate and periodate, but I only tested bromate successfully.
Ni4CO3(OH)6⋅4H2O + 8CH6N4⋅H2CO3 + 16CH3COOH + 8NaOH →
4Ni(CH6N4)2(CH3COO)2 + 8CH3COONa + 9CO2 + 23H2O
4Ni(CH6N4)2(CH3COO)2 + 8NaBrO3 → 4Ni(CH6N4)2(BrO3)2 + 8NaOOCCH3
Assumed Solubility
BrO3 < NO3 < Cl < ClO4 < OOCCH3
But I'd have to test perchlorate.
I cannot say I've noticed ammonium complexes interfering with the actual quality of the product, but rather definitely slows the precipitation, and
any excess does hold it in solution preventing precipitation completely; thus, implying it's significantly more soluble that the AGu complex.
They are some nice and neat crystals KFeNAT. If you had to do it would this be best from recrystalisation or integrated into the reaction liquor? I
think I have PEG 4000 somewhere.
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Etanol
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| Quote: Originally posted by KFeNAT |
and then add alkali to make aminoguanidine recombined with Ni2+ to generate NAP. However, it is important not to use ammonia to neutralize acetic
acid, because the alkalinity of NH3 is not significantly greater than that of aminoguanidine. ... Therefore, NaOH must be used to obtain a purer
product, and the amount of NaOH required should be slightly less than the amount of acetic acid in the solution.. |
To what pH did you add the NaOH?
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KFeNAT
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To what pH did you add the NaOH?[/rquote]
It is usually controlled between 8-9, which is related to the amount of acetic acid used and the concentration of the solution. The pH of the solution
when the "excess" acetic acid in the solution is completely converted into sodium acetate is the pH that needs to be achieved in theory, and it is
also the upper limit of the pH value. For example, in a solution of 0.6g acetic acid added to 30ml water, the pH value of the solution is about 8.5
when the acetic acid is completely neutralized.
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KFeNAT
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| Quote: Originally posted by Axt | I have formed the acetate, but for the reason of producing a "universal solution" that can be used to precipitate whatever counterion one wishes just
by adding its neutral salt, whether it be NaClO4, NaNO3, NaBrO3 etc. The acetate does seem to be significantly more soluble than the rest. I aimed to
try chlorate and periodate, but I only tested bromate successfully.
Ni4CO3(OH)6⋅4H2O + 8CH6N4⋅H2CO3 + 16CH3COOH + 8NaOH →
4Ni(CH6N4)2(CH3COO)2 + 8CH3COONa + 9CO2 + 23H2O
4Ni(CH6N4)2(CH3COO)2 + 8NaBrO3 → 4Ni(CH6N4)2(BrO3)2 + 8NaOOCCH3
Assumed Solubility
BrO3 < NO3 < Cl < ClO4 < OOCCH3
But I'd have to test perchlorate.
I cannot say I've noticed ammonium complexes interfering with the actual quality of the product, but rather definitely slows the precipitation, and
any excess does hold it in solution preventing precipitation completely; thus, implying it's significantly more soluble that the AGu complex.
They are some nice and neat crystals KFeNAT. If you had to do it would this be best from recrystalisation or integrated into the reaction liquor? I
think I have PEG 4000 somewhere. |
I recommend adding it directly to the reaction solution, and the significance of recrystallization is more about correcting the existing unsuitable
product.
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Etanol
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| Quote: Originally posted by KFeNAT |
To what pH did you add the NaOH?[/rquote]
It is usually controlled between 8-9, which is related to the amount of acetic acid used and the concentration of the solution. The pH of the solution
when the "excess" acetic acid in the solution is completely converted into sodium acetate is the pH that needs to be achieved in theory, and it is
also the upper limit of the pH value. For example, in a solution of 0.6g acetic acid added to 30ml water, the pH value of the solution is about 8.5
when the acetic acid is completely neutralized. |
Thank you
I still don't understand why ammonia works with an ClO4 but not in a mixture of ClO4 and CH3COO. But NaOH seems to work.
I evaporated ammonia from my solution preserving pH8 with NaOH.
Indeed, after cooling the ice, red energy crystals, similar to NAP, settled.
However, I'm not sure how much it contain ClO4 and CH3COO. It seems to me that these crystals are more soluble than NAP.
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KFeNAT
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tried to use dextrin with lower solution viscosity as a crystal control agent, and tried adding amounts of 0.2% and 1%. But the effect was not good,
no obvious crystal morphology could be seen, and the product was not ideal.May be a mixture of products with various morphologies.
 
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KFeNAT
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Regarding the sensitivity of sandy PVA-NAP
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.
       
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