Sciencemadness Discussion Board

Nickel aminoguanidine diperchlorate

 Pages:  1  2  

B(a)P - 12-4-2024 at 03:51

Quote: Originally posted by Nemo_Tenetur  
Last week I tried the synthesis from nickel perchlorate (itself synthesized from commercially available nickel nitrate and soda, the precipitate was filtered, washed and redissolved in perchloric acid) and aminoguanidine perchlorate (prepared from commercially aminoguanidine bicarbonate and perchloric acid).

I´ve always used less than the theoretical amount perchloric acid, in both cases some insoluble carbonate / bicarbonate remained at the bottom of the vessel even if stirred over night.

Then I decanted the solutions from the insoluble impurities, the aminoguanidine perchlorate solution was yellow. I combined the solutions by dropwise addition of the nickel perchlorate solution to an excess aminoguanidine perchlorate solution and heated the reaction mixture until bubbles appear, then hold the temperature for several minutes and let it cool again to room temperature.

No visible reaction, no precipitate, nothing even after two days.

Disappointing.

Maybe the solutions were not concentrated enough or maybe the heating was not enough? Maybe the bubbles were simple carbon dioxide instead almost 100 degree centigrade water vapors? I didn´t use a thermometer to check the temparature, this was a mistake.

Is this reaction so temperature and/or concentration sensitive that slight alterations lead to a zero yield?



The reaction is very sensitive to water, what mass of water and reactants did you use? You should use no more water than will dissolve your reactants at an elevated temperature. I also believe the formation of the complex more readily occurs at lower pH.

Etanol - 12-4-2024 at 04:44

Quote: Originally posted by Nemo_Tenetur  
Last week I tried the synthesis from nickel perchlorate (itself synthesized from commercially available nickel nitrate and soda, the precipitate was filtered, washed and redissolved in perchloric acid) and aminoguanidine perchlorate (prepared from commercially aminoguanidine bicarbonate and perchloric acid).

I´ve always used less than the theoretical amount perchloric acid, in both cases some insoluble carbonate / bicarbonate remained at the bottom of the vessel even if stirred over night.

Then I decanted the solutions from the insoluble impurities, the aminoguanidine perchlorate solution was yellow. I combined the solutions by dropwise addition of the nickel perchlorate solution to an excess aminoguanidine perchlorate solution and heated the reaction mixture until bubbles appear, then hold the temperature for several minutes and let it cool again to room temperature.

No visible reaction, no precipitate, nothing even after two days.

Disappointing.

Maybe the solutions were not concentrated enough or maybe the heating was not enough? Maybe the bubbles were simple carbon dioxide instead almost 100 degree centigrade water vapors? I didn´t use a thermometer to check the temparature, this was a mistake.

Is this reaction so temperature and/or concentration sensitive that slight alterations lead to a zero yield?



Add water ammonia by drop after mixing Ni(ClO4)2 and AGu*HClO4 to pH=7.5...8:
Ni(ClO4)2+2AGu*HClO4+2NH3=>Ni(AGu)2(ClO4)2 (solid)+2NH4ClO4 (solution)
Then cold it to 0...5 Celsium.
Very nice and fast reaction:)
Long heating is not required in this method.

[Edited on 12-4-2024 by Etanol]

Microtek - 13-4-2024 at 14:00

I would be wary of using ammonia for adjusting pH. I think you risk substituting some of the aminoguanidine ligands.

Laboratory of Liptakov - 13-4-2024 at 21:30

I feel that will partially created Diamine nickel perchlorate. Which is relatively weak salt on energy.

Etanol - 13-4-2024 at 21:50

Quote: Originally posted by Microtek  
I would be wary of using ammonia for adjusting pH. I think you risk substituting some of the aminoguanidine ligands.


Substituting with ammoia?
I have already prepared the subs with this method. Its color, solubility and explosive properties are identical to the NAP.
May be, Ni hexaammine perchlorate is formed in excess NH3, I don't check it.

pjig - 14-4-2024 at 16:08

Gotta ask , is the initiation properties of nap reliable as something like azides ? Common method of cap manufacture (dense secondary base charge , medium pressed secondary, followed by a primary lightly pressed initiated by either ematch or fuse.
Can NAP function in that det orientation? Or as other “det trains “needs an intermediate 50/50 mix of primary and secondary to achieve this ddt transfer to the high density secondary base?

B(a)P - 14-4-2024 at 19:45

Quote: Originally posted by pjig  
Gotta ask , is the initiation properties of nap reliable as something like azides ?

Yes


Quote: Originally posted by pjig  
Common method of cap manufacture (dense secondary base charge , medium pressed secondary, followed by a primary lightly pressed initiated by either ematch or fuse.
Can NAP function in that det orientation?

Yes

Quote: Originally posted by pjig  
Or as other “det trains “needs an intermediate 50/50 mix of primary and secondary to achieve this ddt transfer to the high density secondary base?

Not required.

Have a read through this thread I think Hey Buddy has tested the effectiveness of initiation. I have also done this on a small scale and it performs well. No need for any special primary secondary mixing.

pjig - 14-4-2024 at 20:11

Awesome! Ty for the quick response. I thought I read that back a ways in the thread, but couldn’t find it anywhere….
NAP is very energetic like azides. Single crystal dets. Remarkable for such a simple synth.
It begs the question why it isn’t used more in an industry standard . Wondering if its down falls are potential toxic gas in the byproducts of decomposition. Seems like the material isn’t hydroscopic , maybe incompatibilities with other things (metals or secondaries)
Maybe it’s the low density, or Chrystal long needle’s sensitivity, or issues with packing in a det cap that may present a problem.
What pressures and or techniques are utilized to work with this primary . Maybe a visit with the IPA version will be a better fit for dets.

[Edited on 15-4-2024 by pjig]

Etanol - 14-4-2024 at 21:46

Quote: Originally posted by pjig  

It begs the question why it isn’t used more in an industry standard

I think it decomposes under the influence of moisture and CO2.

Microtek - 14-4-2024 at 22:34


Quote:

Chrystal long needle’s sensitivity


If you stir it continually during precipitation, it will form a powder rather than crystals.

Regarding decomposition when exposed to CO2 and moisture, I think you are right. But LA does this as well...


Laboratory of Liptakov - 15-4-2024 at 00:36


Add water ammonia by drop after mixing Ni(ClO4)2 and AGu*HClO4 to pH=7.5...8:
Ni(ClO4)2+2AGu*HClO4+2NH3=>Ni(AGu)2(ClO4)2 (solid)+2NH4ClO4 (solution)
Then cold it to 0...5 Celsium.
Very nice and fast reaction:)
Long heating is not required in this method.

I read that the crystals were tested for detonation properties. After a new method of preparation. Using ammonia water is a breakthrough in NAP preparation technology. It simplifies the whole process. Great job, Etanol.
Even ammonium perchlorate we obtain....:D...Absolut useful reaction.




[Edited on 15-4-2024 by Laboratory of Liptakov]

pjig - 15-4-2024 at 07:34

Damn! This is just getting better by the day! lol
I am going to give the ammonia process a run . I took the beaker off the hot plate after the 7.5 min and let it cool undisturbed , if left on hot plate it would have cooled much slower , maybe not a problem and left to stir during rechrystalization phase. Or pull off the hot plate and stir on a cold surface .
Yes I’ll do the ammonia process at this point , (at the boiling point or the point where the reaction starts to cool?) also what is your method of testing for ph….paper , pen , probe, tongue :P

pjig - 15-4-2024 at 07:43

Well I assumed that this newer process would offer a safer material for packing caps. What density would be suitable for the “old h2o method “ vs the new finer form of material?

Etanol - 16-4-2024 at 01:04

Quote: Originally posted by pjig  
at the boiling point or the point where the reaction starts to cool?) also what is your method of testing for ph….paper , pen , probe, tongue :P

neutralisation AGu*H2CO3 with HClO4
mixing of Ni(ClO4)2 and AGu*HClO4 solutions
heating to 80-90C (boiling is not necessary)
add NH3 with pH paper control
(evaporation of NH3 excess)
slow cooling with fast stirring
filtering
drying

Laboratory of Liptakov - 16-4-2024 at 02:21

And the NH3 (or NH4OH) is added to water at 80 C..?...I estimate some splashing liquid. Final solution should be pH neutral..?..Thanks...:cool:
(Edit: Etanol sure a lot years using as probe own tongue)

[Edited on 16-4-2024 by Laboratory of Liptakov]

B(a)P - 16-4-2024 at 11:43

Quote: Originally posted by Etanol  

neutralisation AGu*H2CO3 with HClO4
mixing of Ni(ClO4)2 and AGu*HClO4 solutions
heating to 80-90C (boiling is not necessary)
add NH3 with pH paper control
(evaporation of NH3 excess)
slow cooling with fast stirring
filtering
drying


What yield do you get with this method? Have you compared slow cooling to fast cooling?

Etanol - 16-4-2024 at 15:34

Quote: Originally posted by Laboratory of Liptakov  

Final solution should be pH neutral..?

Very weakly alkaline, I think.
It is difficult to immediately catch the pH drop by drop. But it is easy to evaporate the excess ammonia.

Quote: Originally posted by B(a)P  

What yield do you get with this method?

About 80-90%. I collected and evaporated the spent solution (NH4ClO4 + AGu*HClO4). A little red crystals formed and there was almost no green Ni(ClO4)2 or Ni(OH)2.

Quote: Originally posted by B(a)P  

Have you compared slow cooling to fast cooling?

Fast cooling forms dust and agglomerates.
Slow cooling forms visible crystals. Fast stirring and mechanical crushing break them into convenient powder with good bulk density.
NAP is well soluble in hot AGu*HClO4 solution, but poorly soluble in cold.

pjig - 20-4-2024 at 20:07

IPA method;
I have Found and confirmed that fast cooling does create a very fine particulate. Hopefully not a disadvantage. Usually finer material equals less sensitivity. After solution was heated for 7.5 minutes it was pulled and kept on stirring on a cool surface.. Stirring was continued for one hour then material was filtered with IPA. Not sure the solution needed to be stirred for that long while going to ambient temp.
Is the better method to do what I did , pulling off hot plate and continuing stirring, or turn off hot plate and let cool slowly while stirring , or discontinue stirring (with IPA) .
Is there a advantage to using ph control with NH3 at this point for improvement in Chrystal formation and yield?

[Edited on 21-4-2024 by pjig]

Etanol - 23-4-2024 at 10:14

Quote: Originally posted by pjig  
IPA method;
Is there a advantage to using ph control with NH3 at this point for improvement in Chrystal formation and yield?

Without NH3, method with HClO4 don't work. Yield is null.
In your method, from AGuCO3+Ni(ClO4)2 or AGuCO3+NiCO3+NH4ClO4, NH3 is not required.

[Edited on 23-4-2024 by Etanol]

pjig - 26-4-2024 at 06:50

I see. Thank you for clarifying. The IPA process is substantially a more desired product, in both particle size as well as returns , being a higher yield..
Is there any experimenting done with different percentages of alcohol, including absolute alcohol? Wondering if there is a need for a small percentage of water to take insoluble material into solution.

Hey Buddy - 27-4-2024 at 17:23

Quote: Originally posted by pjig  
I see. Thank you for clarifying. The IPA process is substantially a more desired product, in both particle size as well as returns , being a higher yield..
Is there any experimenting done with different percentages of alcohol, including absolute alcohol? Wondering if there is a need for a small percentage of water to take insoluble material into solution.


When first experimenting with this material, I attempted the patent procedure substituting denatured alcohol for water and was unable to achieve reaction within 5 minute boiling interval. I should also mention that I attempted the reaction with propylene glycol and it reacted to form a red oil product. I did not test its character.

I am continuing to experiment with variations of the material. Overall I have found that IPA product is less sensitive to impact but also somewhat less powerful when unconfined, likely due to native density of the morphology, being a powder. I havent had any problems with pressing the material. I have experienced failures to transfer heat to initiate DDT in some cap designs using secondary, then primary, then a high temp pyrogen between fuze and primary. I found more success with that initiation train plasticizing the pyrogen with nitrocellulose and dipping the end of the fuze. This seems to give longer duration of heat output on the side of the fuze rather than a short spit from the end axis of the fuze.

pjig - 29-4-2024 at 21:18

With e match There is a pretty energetic ignition. Any failures with this approach? Or need for boosting ignition beyond commercial ematch?

[Edited on 30-4-2024 by pjig]

Hey Buddy - 4-5-2024 at 18:03

Quote: Originally posted by pjig  
With e match There is a pretty energetic ignition. Any failures with this approach? Or need for boosting ignition beyond commercial ematch?

[Edited on 30-4-2024 by pjig]


I have been really working on this material. I have found another variation recently in the past week. Im still researching the particulars, because the procedure is a bit sensitive to variables, giving mixed results.

I begin with the standard process for H2O solvent. After 5 minutes of boiling, I decant the reaction fluid leaving behind unreacted solids. The reaction fluid is then placed in a larger cool water bath and sonicated at 42kHz for 10 minutes. The resulting product is a highly dense powder. Possibly nano. Not really sure. It appears smaller crystal than any comparative powder I have.

This powder is considerably more brisant than any other morphology tested. I would consider it a technologically different material. I would compare its brisance to AgNTz or PbNATz. It can achieve clean punctures on Al foil at masses less than 1 mg. This is not possible with even larger slow crystallized morphology NAP, although they do detonate as single crystals, They don't really puncture Al foil.

In terms of sensitivity, crystal NAP is by far the most mechanically sensitive. It is sensitive to impact and friction within range expected in primary explosives. It is pretty sensitive.

IPA NAP (iNAP) is friction insensitive and possibly two to four times less impact sensitive than crystal NAP. Perhaps less, I dont have an apparatus but i have tested this comparison by hand a few dozen times.

Ultrasonicated NAP (uNAP) is ever so slightly less impact sensitive than crystal form, practically the same. It is insensitive to friction compared to crystal NAP. I was unable to detonate uNAP with a 4 lb mallet with pressure and repeated rubbing on top of concrete. While it detonates with a slight tap.

So far in ematch firing of material, it appears that iNAP fires well on ETN with around 25 mg or more. Below that, I have had some failures but I have since updated ematch configuration and it appears to be firing very well in the new configuration into lead blocks, so I will be testing again at sub 25 mg masses. uNAP fires at very small masses. At 25 mg it leaves a considerable impression in lead block at a firing diameter 3.25 mm. Ematches work very well with NAP in any of its forms. E matches directly fire iNAP at lower masses. Still testing blasting cap fillers to determine minimum loads.

Untitled.png - 3.7MB Untitled2.png - 3.4MB

Untitled3.png - 1.6MB Untitled4.png - 1.5MB

Untitled5.png - 1.7MB





[Edited on 5-5-2024 by Hey Buddy]

pjig - 7-5-2024 at 20:26

That is very interesting, using frequency to reduce particle size. Very clever! As for ematch, it is usually a pretty energetic form of ignition . Almost enough to detonate plutonium… :P
Well not quite, but enough to start most primaries.
Are your ematch 25 mg primes very reliable for petn or etn ?
And you’re attempting to find reliable minimal amounts for initiation …….
I’m thrilled to see what new findings you come up with


[Edited on 8-5-2024 by pjig]

pjig - 26-5-2024 at 13:33

Any new findings for the threshold ddt amount for the NAP? 25mg seems a little high compared to other primaries like azides . Azides boast a .5~10 mg ddt ability on their initiation qualities. Pretty low compared to most primaries on the market

[Edited on 27-5-2024 by pjig]

B(a)P - 26-5-2024 at 13:55

Quote: Originally posted by pjig  
Any new findings for the threshold ddt amount for the NAP? 25mg seems a little high compared to other primaries like azides . Azides boast a .5~10 mg ddt ability on their initiation qualities. Pretty low compared to most primaries on the market

[Edited on 26-5-2024 by pjig]


When it is in the form of approximately 1 mm crystals it detonates in amounts starting from 5 to 10 mg in my experience.

Hey Buddy - 26-5-2024 at 20:37

Quote: Originally posted by pjig  
Any new findings for the threshold ddt amount for the NAP? 25mg seems a little high compared to other primaries like azides . Azides boast a .5~10 mg ddt ability on their initiation qualities. Pretty low compared to most primaries on the market

[Edited on 26-5-2024 by pjig]


For DDT, NAP detonates in single crystals, it certainly detonates in any range of higher masses. I think you mean standard minimum firings of secondaries?
There are quite a few issues with the minimum mass firing measurements in literature. The configuration of firing device, the density of the secondary, has a significant effect on detonation transfer when dealing with mg masses. These things typically aren't accounted for in literature, so comparisons without firing configurations and densities, aren't apples to apples or straight forward at all. It can be misleading if you assume it's all the same. For instance if detonating loose secondary, such as a loose pile of RDX, NAP can transfer detonation in minute quantities and there are differences in minimum quantities of NAP for other secondaries such as ETN.

Then there are detonator configurations which are the more realistic test medium. Detonator designs are all over the place. Most commercial IP is withheld so it just requires reproductions and comparisons. If a blasting cap has a compression cup, it reduces the minimum primary mass, sometimes by half. If a secondary is pressed to max density, it increases the minimum mass of primary needed to initiate.

I read your post as to insinuate that somehow NAP is not as powerful at initiation as common azide. It's quite a bit more powerful than Pb(N3)2. I dont know what to tell you, you should try both and see what your judgement is. Everyone I know that uses NAP, most of them are azide people, I'm an azide enjoyer. NAP is obviously more powerful to anyone that has used both.

If you are talking about iNAP, you should know that iNAP is a different complex than NAP, it's not simply an arbitrary alcohol solvent, the isopropyl is complexing in to form a new explosive. There are ways to drop out the isopropyl and the complex recomposes to NAP. It is also possible to make standard NAP and not iNAP in IPA depending on how the reaction is run. It's a different primary explosive material. It has different behaviors and requires larger masses for firing than NAP. uNAP is very similar in performance to Ag(NTz) and Pb(NATz)2, nearly indistinguishable. I have been able to get one and two millimeter perforations in foil with Pb(NATz)2 but for uNAP the smallest holes I can achieve are perhaps 4 or 5 mm. We are talking detonations of material masses the size of a grain or two of table salt.

In my testing of standard inefficient detonators, ie. a metal cap with a single high-density base charge (RDX or ETN) with an iNAP prime, I found < 25 mg gave erratic transfer of detonation, depending on the secondary density. NAP is different than iNAP and uNAP in performance. All of them can transfer detonation at a few mg in low density secondaries.

Hopefully that answers the question. It's really a matter that has to be worked out by each user. I cant give a straight forward answer because the issue is just too big.

pjig - 26-5-2024 at 22:20

That is a very good explanation. I guess I assumed its initiating ability to be less than azides. However it seems to have issues with density of secondary and ddt. Azides seems to not be affected by secondary density.( Inap) is very amazing , but may show weakness on high density secondary.( .2g of primary should have no prob getting det train going.
The I-nap was the material referring to in the question. It’s quantity and density as well as the densities of the secondary (2 densities to base, 1=max density ,and one 1/2 that density )with prime pressed less than that density. Ematch ignition.
What amounts of primary and pressure is needed for reliable ddt.? Not fun to find pellets of secondary after testing. .2 g primary in .5 base PE.

[Edited on 27-5-2024 by pjig]

Hey Buddy - 27-5-2024 at 11:33

Quote: Originally posted by pjig  
That is a very good explanation. I guess I assumed its initiating ability to be less than azides. However it seems to have issues with density of secondary and ddt. Azides seems to not be affected by secondary density.( Inap) is very amazing , but may show weakness on high density secondary.( .2g of primary should have no prob getting det train going.
The I-nap was the material referring to in the question. It’s quantity and density as well as the densities of the secondary (2 densities to base, 1=max density ,and one 1/2 that density )with prime pressed less than that density. Ematch ignition.
What amounts of primary and pressure is needed for reliable ddt.? Not fun to find pellets of secondary after testing. .2 g primary in .5 base PE.

[Edited on 27-5-2024 by pjig]


Ok I understand now. Just to be clear, .2 g is 200 mg. At 200 mg, all three materials are really powerful in detonation. There will be no problem initiating anything at that quantity. For iNAP, at 25 mg, it has trouble in loose configuration on a 3.5 mm fuze spit, against ETN and RDX pressed to near max densities. Ematch gives a much better firing than fuze, but I havent tested with .5 g base charge. I usually use around 800 mg for a base charge. I stopped testing it after I realized that it wasnt possible to compare my findings to compararable literature because of the unknown densities and configurations used. I have read about detonator designs using different densities for a base charge, but I didnt comprehend just how insensitive the secondaries were at max densities. I can test the configuration you are asking about and let you know the result.

pjig - 27-5-2024 at 20:35

Excellent. Yes curious about density and design to maximize efficiency of a I-nap det sys

pjig - 28-5-2024 at 21:03

It seems that there may be something to the pressing pressures / densities….. it seems that PE can Be pressed to density that I-nap needs more weight to ddt that secondary. As you said .2 gm should be way overkill to ddt lower density PE . 50% success with secondary pellet recovered isnt good. Hand packed pressures get complete ddt. There is obviously something being overlooked or missed. Could moisture in secondary being not 100% perfectly dry contribute to a sleepy base? Aluminum tube not enough confinement…?Azides never struggled to ddt standard densities for commercial requirements .



[Edited on 29-5-2024 by pjig]

[Edited on 29-5-2024 by pjig]

Hey Buddy - 29-5-2024 at 12:44

Quote: Originally posted by pjig  
It seems that there may be something to the pressing pressures / densities….. it seems that PE can Be pressed to density that I-nap needs more weight to ddt that secondary. As you said .2 gm should be way overkill to ddt lower density PE . 50% success with secondary pellet recovered isnt good. Hand packed pressures get complete ddt. There is obviously something being overlooked or missed. Could moisture in secondary being not 100% perfectly dry contribute to a sleepy base? Aluminum tube not enough confinement…?Azides never struggled to ddt standard densities for commercial requirements .

[Edited on 29-5-2024 by pjig]


Which document are you referencing with these minimum firing claims? Technology of the Inorganic Azide has a reference section for minimum quantities of DLA on standard secondaries. The minimum DLA is 30 mg. The firing configuration or density of secondary isn't listed. The minimum firing mass is AgN3 on PETN at 5 mg. For RDX the lowest masses are PVA LA and AgN3 at 25 mg. So 25 mg for iNAP isn't bad, it's inline with silver azide in an unknown condition test. My testing conditions are really basic, I'm not using a retainer cup at all or pressing primary explosive. It's just loose.

Untitled.png - 32kB

Etanol - 2-6-2024 at 07:45

Is it possible to prepare NAP from KClO4 in this way?:

NiSO4*6H2O+6NH3=>[Ni(NH3)6]SO4 (good soluble)
[Ni(NH3)6]SO4+2KClO4=>Ni(NH3)6(ClO4)2(bad soluble)+K2SO4
Ni(NH3)6(ClO4)2+2AGu*HClO4=>Ni(AGu)2(ClO4)2+2NH4ClO4+4NH3

[Edited on 2-6-2024 by Etanol]

B(a)P - 2-6-2024 at 13:57

Quote: Originally posted by Etanol  
Is it possible to prepare NAP from KClO4 in this way?:

NiSO4*6H2O+6NH3=>[Ni(NH3)6]SO4 (good soluble)
[Ni(NH3)6]SO4+2KClO4=>Ni(NH3)6(ClO4)2(bad soluble)+K2SO4
Ni(NH3)6(ClO4)2+2AGu*HClO4=>Ni(AGu)2(ClO4)2+2NH4ClO4+4NH3

[Edited on 2-6-2024 by Etanol]


For the last reaction, it would need to be done under conditions that remove the ammonia and favour the formation of the NAP complex without destroying the NAP complex. I can't think what that would be.

Microtek - 3-6-2024 at 00:04

During the usual synthesis of NAP, the solution is boiled for about 5 minnutes. This would drive off ammonia and push the equilibrium towards the product side of things.

I added the nickel ions as the hexaammine nickel perchlorate complex when I first made NAP, though I didn't use KClO4 to make it.

Etanol - 9-6-2024 at 00:04

Quote: Originally posted by Etanol  

[Ni(NH3)6]SO4+2KClO4=>Ni(NH3)6(ClO4)2(bad soluble)+K2SO4

It does not work :(
[Ni(NH3)6]SO4 and KClO4 mix settles.

[Ni(NH3)6]SO4+2NH4ClO4 - yes

[Edited on 9-6-2024 by Etanol]

iNAP Notes

Brightthermite - 7-10-2024 at 06:52

Shout out Dug for getting me interested. Wanted to share some finding.

1g of aminoguanidine bicarb
.43g Nickel Carb
.85g ammonium perchlorate
40 ish mL of IPA (99%, 70%, 91%)

Using 70% IPA produced a pretty awful yield. Lots of nickel left in the reaction vessel similar to using water (probably because its 30% water). The NAP that formed was very sensitive and powerful, it formed small needle like crystals. The yield was almost non existent. I assume I would need to let it crystalize out of solution for much longer just as if I was using water. Although I would say 70% was more or less a failure, might as well just use water.

Using 99% produced no energetic material at all. It turned a hazy oily red. Nothing seemed to fully dissolve or disassociate. It also lacked the initial release of gas that you see at the beginning of the other reactions. This leads me to believe some amount of water is needed. Again maybe it should have ran for longer then 5 min but I didn't investigate further.

91% produced a product just as expected. There was what appeared to be some undissolved aminoguanidine in the final product though. May need to use more solvent next time.

I was easily able to fire .75g of TACP pressed in .25g steps with around 6mg of iNAP using a 3D printed reinforcing cap. I need to run more test to see if this amount and outcome is consistent but I believe it will be. This material easily detonates with just a bit of confinement.

pjig - 11-10-2024 at 18:16

Brightthermite:
That is an interesting find. Just shifting the %of alcohol in the solution changes the outcome dramatically. It does seem for some reason that the 70% ipa is low yielding . While high concentrations lack enough water to kick the reaction. The standard process w/o ipa yields nice red long needles.
Strangely you have found the sweet spot of the reaction, using 90% . This is very interesting. Did you give the reacted materials a longer cool down process? How was your procedures done?

ManyInterests - 13-10-2024 at 15:34

Quote: Originally posted by Brightthermite  
Shout out Dug for getting me interested. Wanted to share some finding.

1g of aminoguanidine bicarb
.43g Nickel Carb
.85g ammonium perchlorate
40 ish mL of IPA (99%, 70%, 91%)

Using 70% IPA produced a pretty awful yield. Lots of nickel left in the reaction vessel similar to using water (probably because its 30% water). The NAP that formed was very sensitive and powerful, it formed small needle like crystals. The yield was almost non existent. I assume I would need to let it crystalize out of solution for much longer just as if I was using water. Although I would say 70% was more or less a failure, might as well just use water.

Using 99% produced no energetic material at all. It turned a hazy oily red. Nothing seemed to fully dissolve or disassociate. It also lacked the initial release of gas that you see at the beginning of the other reactions. This leads me to believe some amount of water is needed. Again maybe it should have ran for longer then 5 min but I didn't investigate further.

91% produced a product just as expected. There was what appeared to be some undissolved aminoguanidine in the final product though. May need to use more solvent next time.

I was easily able to fire .75g of TACP pressed in .25g steps with around 6mg of iNAP using a 3D printed reinforcing cap. I need to run more test to see if this amount and outcome is consistent but I believe it will be. This material easily detonates with just a bit of confinement.


Thank you for mentioning the lack of effectiveness of the 99% IPA. I don't know if 91% is available in my area, but 99% and 70% are everywhere.

Since 91% won't be super easy to find, I can just add a little water to the 99% to bring it down to 91% ish.

Also I will be very interested in looking at uNAP.


I am looking at uNAP and iNAP right now due to some difficulties that I am having with NHN going full detonation in non-steel containers. My questions are concerning its long-term stability and safety in hand loading.

The way I make my detonators, and I made a lot of them thus far, is to load the secondary first with as much pressure as I can do by hand (I don't have an arbor press or any mechanical means of loading my caps), followed by topping it with the primary and only very gently tamping it without any hard pressing (I sometimes tap on the sides of the cap to help the material get more compacted before gently tamping everything down.

I assume this is a safe process for doing it with uNAP or iNAP?

pjig - 15-10-2024 at 06:51

As per loading caps , it may be wise to not tamp , or even tap container to consolidate your primary. (Secondary maybe) …one could build his own wedge style press out of a hinge and some 2x4 lumber and with plywood.
Loading should be done methodically and consistent in speed , pressures etc . Fast or aggressive loading may result in a pop. Proper ppe and a blast shield are wanted

ManyInterests - 15-10-2024 at 11:02

I have loaded many, many caps by hand. For my last test run I loaded around 20. When loading the primary (nhn) I used to press mildly, but now I don't, instead just tamping very gently. There is no danger of detonation with such light force placed.

I know that iNAP and uNAP are more sensitive to impact than NHN, but they aren't lead azide or HMTD levels sensitive. I am just looking for a comparison if one is available.

BTW I assume you got your inspiration for a loading press from the improvised munitions handbook?




pjig - 15-10-2024 at 19:47

That’s where I saw a wood version of the press. But an arbor press with the shield will be a better option. Neat idea for Improvised set up .
How is the performance of NHN compared to the NAP? It appears a little moody if confinement is minimal from your description. Mixing a intermediate prime secondary isn’t helping step the det train either?
Is your ignition electrical or fuse? Sometimes a crimping or heavy glues needed to achieve confinement of the top side . If not steel tubes , aluminum? Is it alloyed, or soft al and your base plug ?(may be an issue). Just a couple things that can cause confinement issues.

[Edited on 16-10-2024 by pjig]

ManyInterests - 16-10-2024 at 05:55

Quote:
Quote:
[Quote]That’s where I saw a wood version of the press. But an arbor press with the shield will be a better option. Neat idea for Improvised set up .


Yeah the arbor press is good and strong, but the Improvised Munitions Handbook was all about making things out of commonly available stuff. I still load by hand since I find the end result still good... and I don't have an arbor press...


[Quote]How is the performance of NHN compared to the NAP?


That's my question. I have no experience with NAP. With NHN the thing I noticed is that it needs more confinement than I thought to detonate, and when it comes to detonating ETN or PETN you need stronger confinement than an aluminum or plastic case.

NAP, however, is different than NHN since NHN simply deflagerates at incredible speed when unconfirmed, but it does not detonate unconfined.

NAP appears to be one of those energetics that detonate unconfined from flame alone. This is why I am thinking of transitioning to it since I think it is the superior initiating agent. My main concern is the safety when loading.

Quote:
It appears a little moody if confinement is minimal from your description. Mixing a intermediate prime secondary isn’t helping step the det train either?
Is your ignition electrical or fuse? Sometimes a crimping or heavy glues needed to achieve confinement of the top side . If not steel tubes , aluminum? Is it alloyed, or soft al and your base plug ?(may be an issue). Just a couple things that can cause confinement issues.


I did do a 1:1 mix of melt-cast ETN with the NHN, and while it still worked well with the detonation, I am not sure if it had an overall improved effect, but it is still effective. Maybe I will continue using it. I think I should do a comparison of straight NHN to the 1:1 mix. Also the mixture failed to fully detonate either the brass casings or the aluminum casings. The aluminum was an alloy (Aliexpress said 6063 alloy). I am not sure if it is the same thing as the aluminum used in most commercial or military detonators, however. The steel caps where 304 stainless steel with 8x7x50mm.

The base plug was 0.5mm or thereabouts, as I was advised, but the ones that were entirely bottomless and simply had some electrical tape at the bottom (to waterproof and prevent anything from falling out) actually performed much better, so I will do that going forward. No bottoms. Just one layer of tape followed by a wrap around it to secure that tape.

The confinement at the top is sufficient. I know this because when I used plastic bodies the epoxy at the top almost always survives unscathed while the rest of the body is obliterated.

Perhaps... perhaps I need to make a detonator out of hardened epoxy? That might be crazy enough to work.

I've used both fuses and e-matches. Both work fine and have the same overall result.


[Edited on 16-10-2024 by ManyInterests]

[Edited on 16-10-2024 by ManyInterests]

pjig - 17-10-2024 at 07:00

I like LL’s pressed foil base idea in the det base . Aircraft Al is good.
Nap seems to be very good and safe to load if it is the unap or Inap version of the nap family. Due to the crystal morphology.
I’m assuming you’re pressing 3 layers to your caps: base, 1-1mix, and a topping of nhn primary on top. That should work. Maybe try the foil base in cap body or was that what your describing in the .5mm vs tape only?

Maybe try a harbor freight (cheap arbor press), if $ is tight.
Obviously the whole goal to the trade is keeping costs low, and performance repeatable .so finding cheap tools and materials / methods to make final product is desirable.

[Edited on 17-10-2024 by pjig]

Microtek - 17-10-2024 at 09:27

NAP (the unaltered form) can be had as a powder simply by stirring the mix as it precipitates. This disrupts the formation of the beautiful large crystals and gives a less lustrous powder. In this form it is less sensitive than ETN to both impact and friction, and far more reliable primary than NHN.

Hey Buddy - 17-10-2024 at 12:05

To more clearly explain the differences in the NAP forms-

NAP, large crystal, or small crystal:
Sensitive to impact
Sensitive to friction
Minimal detonation perforations in foil >~10mm

iNAP
this is a different material. It is a different complex than NAP, it has at least one or two isopropyl groups within the complex. It is possible to make standard NAP in IPA solvent, depending on process. It is also possible to decompose iNAP complex with solvents and then reform large red crystal standard NAP from the iNAP complex.
This material is a pink powder form, similar in consistency to flour.
Less sensitive to impact than NAP (~3 or 4x less)
Insensitive to friction
minimum perforations in foil >~10mm

uNAP
This is a crystal modification technique. It gives a different performance product than NAP similar to AgNTz.
Equal impact sensitivity to standard crystal NAP
Less friction sensitive than standard NAP
minimum perforations in foil <10mm, as low as 5mm

I have found that stirring standard crystal NAP does make a small crystal but it is the same practical sensitivity and performance as large crystal. The standard crystal forms of NAP detonate as single crystals, but are probably more of a deflagration because they wont puncture foil as single crystals. iNAP and NAP require confinement when used in small quantities (~5mg). uNAP detonates and perforates unconfined in microgram quantities.

iNAP and uNAP can be further desensitized by screen mixing them with 5-10% PTFE powder.

IMO all three are more sensitive to impact than ETN, iNAP is less friction sensitive than any primary I've used. NAP in any form (IMO) is superior to other primaries when all factors are considered. It is simpler to produce than peroxides. NAP is certainly detonating over 8 km/s. iNAP and uNAP detonate secondaries directly. uNAP caps with only around a gram can detonate ANNM directly, similarly to other high strength caps with PETN or RDX.

There also appear to be factors that affect uNAP depending on beaker diameter, size of batch and power of sonication. Small powder uNAP can be made in scaled up quantities but the transmission of sonication seems to limit the creation of actual uNAP. The way to tell if uNAP has been made correctly is to heat it to detonation on foil in microgram quantities, like the size of a large grain of table salt. If it perforates the foil, it is correct, if it poofs without perforating the foil, it is not achieving the small size of proper uNAP. I have most success with 1-4 g batches but have had lower performance batches when I increase batch size, likely due to the limitations of the ultrasonicator used.

The darker red material is uNAP 1500x
lighter material is iNAP 1500x
UORC3044.JPG - 385kB UJQL7770.JPG - 361kB

[Edited on 17-10-2024 by Hey Buddy]

Microtek - 18-10-2024 at 02:19

I have a couple of questions:

What do you mean when you state "Minimal detonation perforations in foil >~10mm"?

Also, on what do you base the assertion that iNAP contains isopropanol as a ligand?

Regardless, I have tested the fine grained NAP on my oblique impact apparatus using 180 grit sandpaper between steel hammer on steel anvil. In this test it is less sensitive than PETN, and since PETN is, AFAIK, not as sensitive as ETN, I must conclude that NAP prepared in this way is not as sensitive as ETN.

Hairsplitting aside, I agree that NAP is a superior primary. The only downsides that I can find are the instability in liquid water (not water vapour, so not a big deal) and the possible health hazards of the detonation products (potential Ni(CO)4 formation). The health concerns may be a non-issue but since I can't test it, I will err on the side of caution for indoor experiments.

Etanol - 18-10-2024 at 09:21

Quote: Originally posted by Hey Buddy  

The darker red material is uNAP 1500x
lighter material is iNAP 1500x

The first photo is NAP. The second photo is not NAP, but a mixture with a small NAP content.
Maybe white is NH4ClO4, grey-green is NiCO3.

Hey Buddy - 18-10-2024 at 17:57

Quote: Originally posted by Microtek  
I have a couple of questions:

What do you mean when you state "Minimal detonation perforations in foil >~10mm"?

Also, on what do you base the assertion that iNAP contains isopropanol as a ligand?

Regardless, I have tested the fine grained NAP on my oblique impact apparatus using 180 grit sandpaper between steel hammer on steel anvil. In this test it is less sensitive than PETN, and since PETN is, AFAIK, not as sensitive as ETN, I must conclude that NAP prepared in this way is not as sensitive as ETN.

Hairsplitting aside, I agree that NAP is a superior primary. The only downsides that I can find are the instability in liquid water (not water vapour, so not a big deal) and the possible health hazards of the detonation products (potential Ni(CO)4 formation). The health concerns may be a non-issue but since I can't test it, I will err on the side of caution for indoor experiments.


For the sonicated crystal, it is much smaller than other crystal morphologies, it punctures foil in 4 or 5 mm diameters. This is typically from microgram quantities. Standard forms of NAP in order to detonate unconfined, require masses that result in somewhere around 10 to 15mm diameter perforations. This higher power and the change in sensitivity is why it is differentiated as uNAP. In efforts to scale up, some people have made giant runs of uNAP, or attempted to do so, but the result is a mixed product. There appears to be limitation of the sonic transmission in bench sonicators.

My claim on the sensitivity of the various NAP is based on hammer testing with a 4 lb hammer, which isn't very precise, but I've tested such a huge volume of explosives this way that I can attain a relative repeatable comparison between samples. NAP and the analogues, I have impact and friction detonated quite a lot. In my testing, NAP, uNAP and NAP crystallized under 250 rpm stirring, all detonate with less force than what is required to detonate ETN, in my testing with the samples I've used, it this is observable unambiguously. iNAP seems fairly approximate to ETN in impact, and I haven't been able to detonate iNAP from friction at all.

I believe iNAP is complexing in isopropanol groups because of the different physical characteristics, the fact that it is possible to use IPA to produce standard NAP alone, and that it is possible to "drop out" whatever iNAP is, and revert it to NAP. For instance, in some solvents, iNAP will dissolve then reform as large red NAP crystals. Of course it could be some sort of co-crystal, or something else, I dont know. I would assume it is a complex including isopropyl groups, or at least one. NAP is very sensitive to reactant equilibrium and goes through radically different forms that seem likely to be different complexes with different materials like glycols, MEA etc.

Hey Buddy - 18-10-2024 at 18:17

Quote: Originally posted by Etanol  
Quote: Originally posted by Hey Buddy  

The darker red material is uNAP 1500x
lighter material is iNAP 1500x

The first photo is NAP. The second photo is not NAP, but a mixture with a small NAP content.
Maybe white is NH4ClO4, grey-green is NiCO3.


This is iNAP made with NH4ClO4 and NiCO3, there is probably some unreacted AGuHCO3 also. There are always unreacted solids in this method. I think you should probably just investigate iNAP yourself if you want to get to the bottom of what is going on. The differentiations are necessary because they are so different in behavior. uNAP, NAP and iNAP are all different from one another in performance and sensitivity. Some of the differences are radical, like sensitivity or minimum firing masses. uNAP for instance can detonate low density PETN unconfined in quantities less than a mg. It is my personal opinion, or theory regarding the complexation of the isopropyl group. It may or may not be the case, I have simply assumed this is the case because of the possibility of producing both NAP and iNAP in IPA solvent. I suppose the photo is a bit low res, IMO the crystals of iNAP appear distinct from NAP. Anyone is welcome to correct me on this, but until then, this is my best guess.

[Edited on 19-10-2024 by Hey Buddy]

Hey Buddy - 18-10-2024 at 18:27

Thinking about it now, if one didn't accept an ionic interaction of the IPA, it would require explanation of why iNAP is a product under certain IPA ratio and heating conditions, but NAP is a product at other ratios. There is such a distinct difference between iNAP and NAP that I cant imagine IPA isn't adding to the complex.

Hey Buddy - 18-10-2024 at 20:32

These are some pictures of a few hundred μg of uNAP detonating low density PETN. This isn't possible with standard NAP.

Untitled.jpg - 309kBUntitled2.jpg - 369kBUntitled3.jpg - 350kB

Microtek - 19-10-2024 at 00:20

Judging from the first picture of the uNAP, I would guess that your scales are playing tricks on you (some electronic scales have difficulty measuring amounts very close to zero, and will just round off digitally). That certainly looks more like ca. 5 mg than just a few hundred ug. By the way, the substance you term uNAP in these pictures look exactly like what I get with my version of the stirred precipitation method.

Many materials show markedly different properties based on the morphology and particle size. Some so much so that they appear to be completely different materials. The NAP that I make is also perfectly able to initiate PETN in amounts like these.

Hey Buddy - 19-10-2024 at 10:31

In the photo, it may look like a lot of material because that particular test had sprinkled material over a wide surface area. If the amount of material were consolidated, it appears very small. It broke apart when transferring with tweezers and powderized on the foil. I calibrate and level this scale. To the best of my knowledge, it accurately discerns 1 mg weights. Of course in sub milligram masses, it is difficult to accurately work, so I reference the perforation diameters in Al foil for comparison measurements. I've found it is difficult to achieve small diameter perforations in foil with other forms. There are limitations in the minimal diameters that can be achieved with NAP versus uNAP. I have also made batches of NAP with stirring as you suggested and in my judgement, these are different performance materials. I have stirred at 250 rpm during precipitation but the crystal size is still much larger and different in performance than ultrasonicated precipitation.

I will attempt to take some more images to hopefully better demonstrate scale. It would really be best to simply replicate it on your end to witness any difference observed first hand.

I think all three of these materials, NAP, iNAP and uNAP are distinct enough in performance and character to justify differentiation. Similarly to service lead azide, dextrinated and PVC azide. I think these NAP materials differentiate in quality even more than azide modification techniques, however.

It is my opinion that iNAP likely has complex interaction with isopropyl groups, beyond simply modifying the crystal in precipitation. That's my honest judgement to my own limitations of measurement and creative testing. I'm not married to that conclusion. It's just my best hypothesis. Anyone is welcomed to examine these materials and disprove these opinions or demonstrate any other conclusion.

There have been quite a few reproductions of these materials even outside of science madness, and they are consistently differentiated in performance across different users, using different processes, in different locations across the world. When the ideas are challenged without any measurements or proofs, it makes it difficult to take the criticism seriously. If you were experimenting with these materials, I believe it would likely influence your conclusion. It did mine.

[Edited on 19-10-2024 by Hey Buddy]

uNAP Common Minimum Foil Perforation Diameter Example 1

Hey Buddy - 19-10-2024 at 11:11



20241019_134850.jpg - 2MB 20241019_135031.jpg - 2.6MB 20241019_135142.jpg - 1.4MB

uNAP Common Minimum Foil Perforation Diameter Example 2

Hey Buddy - 19-10-2024 at 11:16

20241019_135322.jpg - 1.7MB 20241019_135408.jpg - 2.2MB 20241019_135722.jpg - 2.6MB

Hey Buddy - 19-10-2024 at 11:48

These masses are certainly less than 1 mg. If someone can detonate PETN with less than a mg of NAP or perforate a 5mm hole in Al foil, then I will reconsider my opinion on the significance of uNAP designation. iNAP will have to be analyzed by more capable chemists to determine what is going on exactly. Regardless, all three materials are different in performance and sensitivity necessitating separate designations.

20241019_143434.jpg - 1.9MB 20241019_143458.jpg - 2MB 20241019_143530.jpg - 2.6MB

Microtek - 19-10-2024 at 13:48


Quote:

When the ideas are challenged without any measurements or proofs, it makes it difficult to take the criticism seriously.


I am not trying to attack you or your work, I'm simply asking questions and putting forward my counterhypothesis to explain the results. I haven't been following this thread closely for the past year, but if you would reiterate your method for producing uNAP I would be happy to see if I can reproduce your results. I have tried using the search function, but the earliest mention of uNAP the engine turned up did not contain much more information than just the use of ultrasonication.

When using stirring to modify crystal size, the RPM obviously makes a large difference (the faster you go, the smaller the crystals will be). I was using somewhat more than 250 RPM (400-500 IIRC), so that may be the reason.

Hey Buddy - 19-10-2024 at 14:59

Quote: Originally posted by Microtek  

Quote:

When the ideas are challenged without any measurements or proofs, it makes it difficult to take the criticism seriously.


I am not trying to attack you or your work, I'm simply asking questions and putting forward my counterhypothesis to explain the results. I haven't been following this thread closely for the past year, but if you would reiterate your method for producing uNAP I would be happy to see if I can reproduce your results. I have tried using the search function, but the earliest mention of uNAP the engine turned up did not contain much more information than just the use of ultrasonication.

When using stirring to modify crystal size, the RPM obviously makes a large difference (the faster you go, the smaller the crystals will be). I was using somewhat more than 250 RPM (400-500 IIRC), so that may be the reason.


I did not mean to suggest this as an attack. I respect any opinion you put forward (even if it were an attack). I meant that the situation becomes hearsay if there is no demonstrated measurement or comparison or something to observe. I am using this method for both iNAP and uNAP https://www.youtube.com/watch?v=VR_9GZlIRRo&t
[Edited on 19-10-2024 by Hey Buddy]

[Edited on 19-10-2024 by Hey Buddy]

MineMan - 19-10-2024 at 17:11

Quote: Originally posted by Hey Buddy  
In the photo, it may look like a lot of material because that particular test had sprinkled material over a wide surface area. If the amount of material were consolidated, it appears very small. It broke apart when transferring with tweezers and powderized on the foil. I calibrate and level this scale. To the best of my knowledge, it accurately discerns 1 mg weights. Of course in sub milligram masses, it is difficult to accurately work, so I reference the perforation diameters in Al foil for comparison measurements. I've found it is difficult to achieve small diameter perforations in foil with other forms. There are limitations in the minimal diameters that can be achieved with NAP versus uNAP. I have also made batches of NAP with stirring as you suggested and in my judgement, these are different performance materials. I have stirred at 250 rpm during precipitation but the crystal size is still much larger and different in performance than ultrasonicated precipitation.

I will attempt to take some more images to hopefully better demonstrate scale. It would really be best to simply replicate it on your end to witness any difference observed first hand.

I think all three of these materials, NAP, iNAP and uNAP are distinct enough in performance and character to justify differentiation. Similarly to service lead azide, dextrinated and PVC azide. I think these NAP materials differentiate in quality even more than azide modification techniques, however.

It is my opinion that iNAP likely has complex interaction with isopropyl groups, beyond simply modifying the crystal in precipitation. That's my honest judgement to my own limitations of measurement and creative testing. I'm not married to that conclusion. It's just my best hypothesis. Anyone is welcomed to examine these materials and disprove these opinions or demonstrate any other conclusion.

There have been quite a few reproductions of these materials even outside of science madness, and they are consistently differentiated in performance across different users, using different processes, in different locations across the world. When the ideas are challenged without any measurements or proofs, it makes it difficult to take the criticism seriously. If you were experimenting with these materials, I believe it would likely influence your conclusion. It did mine.

[Edited on 19-10-2024 by Hey Buddy]



Ahh, there was a YouTube channel discussing all of this.

MineMan - 19-10-2024 at 17:14

Quote: Originally posted by Hey Buddy  
In the photo, it may look like a lot of material because that particular test had sprinkled material over a wide surface area. If the amount of material were consolidated, it appears very small. It broke apart when transferring with tweezers and powderized on the foil. I calibrate and level this scale. To the best of my knowledge, it accurately discerns 1 mg weights. Of course in sub milligram masses, it is difficult to accurately work, so I reference the perforation diameters in Al foil for comparison measurements. I've found it is difficult to achieve small diameter perforations in foil with other forms. There are limitations in the minimal diameters that can be achieved with NAP versus uNAP. I have also made batches of NAP with stirring as you suggested and in my judgement, these are different performance materials. I have stirred at 250 rpm during precipitation but the crystal size is still much larger and different in performance than ultrasonicated precipitation.

I will attempt to take some more images to hopefully better demonstrate scale. It would really be best to simply replicate it on your end to witness any difference observed first hand.

I think all three of these materials, NAP, iNAP and uNAP are distinct enough in performance and character to justify differentiation. Similarly to service lead azide, dextrinated and PVC azide. I think these NAP materials differentiate in quality even more than azide modification techniques, however.

It is my opinion that iNAP likely has complex interaction with isopropyl groups, beyond simply modifying the crystal in precipitation. That's my honest judgement to my own limitations of measurement and creative testing. I'm not married to that conclusion. It's just my best hypothesis. Anyone is welcomed to examine these materials and disprove these opinions or demonstrate any other conclusion.

There have been quite a few reproductions of these materials even outside of science madness, and they are consistently differentiated in performance across different users, using different processes, in different locations across the world. When the ideas are challenged without any measurements or proofs, it makes it difficult to take the criticism seriously. If you were experimenting with these materials, I believe it would likely influence your conclusion. It did mine.

[Edited on 19-10-2024 by Hey Buddy]



Ahh, there was a YouTube channel discussing all of this.

Etanol - 19-10-2024 at 19:04

The real accuracy of Chinese electronic scales is 5...10 divisions. That is, for scales with a division of 1 mg, the real accuracy is 5...10 mg.
To get a submilligram mass, you should weigh about 10mg on the scales, then divide it 2 times, 4 times and so on.

I have never heard the alcohols form a complex or clatrate compound. But I know that the solubility of perchlorates decreases in the row water>methanol>ethanol>isopropanol. This leads to incomplete reactions in anhydrous isopropyl alcohol.

Hey Buddy - 19-10-2024 at 20:19

I'm not going to argue with someone on the internet about a supposed inaccuracy of a cheap scale. I have more than one scale, and more than one calibration weight to cross reference scales. I already wrote, to the best of my knowledge the scale is accurate to the mg. If you don't accept that, it's your problem. The scale of minimum detonation mass is verified to be microgram by other people that have prepared the material, with much more expensive scales than I possess, so whatever point you're attempting to make is irrelevant.

What are you even claiming? --"Chinese scales are inferior, thus your scale is inaccurate, thus your measurements of masses are inaccurate, thus the material is not performing as claimed" Is that what you're suggesting?

These are tiny, tiny masses. Anyone familiar with NTz and NAP will recognize the significance from the images alone. They fit on the end of a pen head. I have tetrazole reference materials for comparison. It is in the tetrazole territory in both det velocity 8km/s + and minimal detonation masses. If you don't agree with these findings then you can probe with your own research. Speculation is worthless. The whole internet is ripe with speculation, it's like a rectum, everyone has it. Pull some data or comparisons. That is the only thing useful, not elongating these threads with needless disagreement. You disagree, fine, prove it.

As for iNAP, I suppose anything is possible with the structure. I was suggesting that IPA is complexing. Perhaps it isnt. Perhaps you can also investigate that while you're researching uNAP, then after you have examined it, make your own valuable determination. That would be a post worth reading.

The behavior of IPA is very unusual in this reaction. There isn't an analogous phenomenon that takes place with other alcohols, it is unique to IPA. It could be a clathrate, co-crystal, or simply dirty NAP as you have claimed. In my opinion, it seems likely to be complexing, the crystal is clearly different, I posted a 1500x digital microscope image to show the crystal differences. Apparently, those images are ambiguous, to you (not me). My scale measurements to demonstrate uNAP are ambiguous, to you (not me). The images of detonation demonstrations are ambiguous, to you (not me). Now it's time for you to do some testing and produce something other than rhetoric to support your own arguments which you've put forward.
It is your responsibility to demonstrate what is going on with this unknown IPA mechanism, or at least verify that it is simply NAP diluted with contamination as you claimed. It is also on you to demonstrate that uNAP does not detonate at the microgram scale.




[Edited on 20-10-2024 by Hey Buddy]

Laboratory of Liptakov - 19-10-2024 at 22:29

To lighten the thread, I say: ...In my opinion, the Nickel Aminoguanidine perchlorate does not work at all.....:D

Etanol - 20-10-2024 at 00:53

Perhaps my comment looks too sharply because of the language barrier.
I just indicated how to get a higher accuracy of measurements based on my experience with many scales so that you can quickly find the truth.
My laboratory capabilities are limited, so my own check will take a long time and you probably get ahead of me.

It is great that you have made microphotography of your substance. And these microphotography clearly show the multi-components of the IPA-NAP.
The most simple explanation of the uniqueness of IPA is its poor dissolving ability relative to water or ethyl alcohol.

In addition, I would advise you to change your “detonation” criterion, since a very thin foil can be torn not only under the influence of the brisant action of detonation, but also from the fougasse effect of explosive combustion.
To talk about detonation, you should select the thickness of the metal foil in accordance with the mass of the sample in the range of approximately 1/5 ... 1/10 from the size of the portion of the substance.
For 1 mg (1 mm3), this should be at least 100 microns. Household aluminum foil has a thickness of 10 ... 15 microns, so it can be torn from the non-detonation explosive of 1 mg of substance.

Hey Buddy - 20-10-2024 at 08:22

Quote: Originally posted by Etanol  
Perhaps my comment looks too sharply because of the language barrier.
I just indicated how to get a higher accuracy of measurements based on my experience with many scales so that you can quickly find the truth.
My laboratory capabilities are limited, so my own check will take a long time and you probably get ahead of me.

It is great that you have made microphotography of your substance. And these microphotography clearly show the multi-components of the IPA-NAP.
The most simple explanation of the uniqueness of IPA is its poor dissolving ability relative to water or ethyl alcohol.

In addition, I would advise you to change your “detonation” criterion, since a very thin foil can be torn not only under the influence of the brisant action of detonation, but also from the fougasse effect of explosive combustion.
To talk about detonation, you should select the thickness of the metal foil in accordance with the mass of the sample in the range of approximately 1/5 ... 1/10 from the size of the portion of the substance.
For 1 mg (1 mm3), this should be at least 100 microns. Household aluminum foil has a thickness of 10 ... 15 microns, so it can be torn from the non-detonation explosive of 1 mg of substance.


These statements just don't possess significant substance to me. I'm not offended by any sharpness of any statement you would make. You can be as direct as you want in your communication. I'm not offended at all. I'm annoyed that you are so lazy and unwilling to put in the effort to demonstrate your claims, but readily willing to offer definitive or insinuative claims with no data, imagery or demonstration. These threads stay up for a long time, people search this sort of information out and will continue in the future. When SM is gone, people will continue to archive the information and instead of viewing responses that help understand the material in examination, people will have to wade through the posts that dont have much substance. The speculation without demonstration is counter productive to the development of the material. It is good that you have a counter hypothesis in response. It should be accompanied by demonstration, not theoretical rhetoric.

Hey Buddy - 20-10-2024 at 08:26

Quote: Originally posted by Laboratory of Liptakov  
To lighten the thread, I say: ...In my opinion, the Nickel Aminoguanidine perchlorate does not work at all.....:D


I suppose it depends on the definition of "work". For detonating secondary explosives, it works alright.

Hey Buddy - 20-10-2024 at 09:03

Quote: Originally posted by Etanol  

In addition, I would advise you to change your “detonation” criterion, since a very thin foil can be torn not only under the influence of the brisant action of detonation, but also from the fougasse effect of explosive combustion.
To talk about detonation, you should select the thickness of the metal foil in accordance with the mass of the sample in the range of approximately 1/5 ... 1/10 from the size of the portion of the substance.
For 1 mg (1 mm3), this should be at least 100 microns. Household aluminum foil has a thickness of 10 ... 15 microns, so it can be torn from the non-detonation explosive of 1 mg of substance.


I don't know what your definition of detonation is, uNAP detonates secondary explosives in sub mg quantities. Insensitive secondaries that don't explode unless struck or detonated by another explosive, they detonate unconfined on top of sub mg quantities of uNAP. That is about the minimum limitation, somewhere in the sub mg mass, beyond that the uNAP just starts launching secondary explosive in the air like confetti. When it does detonate a secondary, There is some detonation fade out, due to the secondary being unconfined and low density, this is related to the sympathetic sensitivity of the secondary, but it detonates for sure. Equivalent quantities of standard NAP are incapable of this, as best as could be determined from my testing.

The reason foil is used, is to demonstrate comparison between materials: There is simply a limitation of minimum detonation perforation diameter of primary explosives. Something like PbNATz for example, can exceed the minimal diameter of uNAP, where as NAP, whether a powder or a large slow crystal, is incapable of perforating the same scale of small diameter hole. That is according to my testing. It might be the case that you can achieve 5mm holes in foil with standard NAP. I have not been able to do this. I've been testing this material for a year now, continuously. It doesn't matter the mils of the foil thickness, because it is arbitrary. The foil is only used as a constant medium to comparably measure the affect of the detonations. The only thing that matters is maintaining the same roll of foil between the various materials so that accurate comparison can be made.

The greater minimum detonation capability of uNAP agrees with findings of other phenomenon such as detonator efficiency studies. I attached a PDF of a study on detonator efficiencies. On p. 664 it discusses the phenomenon of increased efficiency of detonation correlating to the diameter of a detonator body. The smaller diameter, the greater relative efficiency. Because ultrasonication results in disruption of the boundary layer of crystallization, it forms smaller diameter crystals, smaller than the diameter of mechanically disrupted material. Thus the crystals are cylindrical in shape, and follow the same principal as found in detonator studies, the smaller diameter of cylinder crystal demonstrates greater efficiency per mass, in detonation. This is likely the result of the geometry of a cylinder and its surface area per volume.

Attachment: det_grant_Factors_affecting_Initiating_efficiency_of_detonators.pdf (759kB)
This file has been downloaded 47 times

[Edited on 20-10-2024 by Hey Buddy]

ManyInterests - 20-10-2024 at 17:14

Quote:
NAP (the unaltered form) can be had as a powder simply by stirring the mix as it precipitates. This disrupts the formation of the beautiful large crystals and gives a less lustrous powder. In this form it is less sensitive than ETN to both impact and friction, and far more reliable primary than NHN.


Quote:
When using stirring to modify crystal size, the RPM obviously makes a large difference (the faster you go, the smaller the crystals will be). I was using somewhat more than 250 RPM (400-500 IIRC), so that may be the reason.


Is it possible that strong stirring and the ultrasonic vibration are ultimately doing the same thing? I am just throwing that thought out there.

But that being said, I am really getting excited to try to make some uNAP soon and contributing to this discussion. Are you serious about the impact sensitivity being less than ETN? This is fantastic, because I always hand load and press everything and the reason why I went for NHN was due to it's insensitivity to friction and impact, but its high sensitivity to flame (even a simple hot wire is sufficient without the need for any additions to it, as long as it is making direct contact with the material).

I have one question about uNAP/iNAP. Are they just as flame sensitive? Or is something more needed? In all my past detonators I used an e-match that had nichrome wire loop over a match head that would burn once power is applied to it. But in many detonators I tested, especially with the plastic bodies, I noticed that in many cases the match head didn't burn and actually survived the initial explosion. It would still burn later when I was disposing of them. This leads me to believe that only the wire is necessary and the actual match is unnecessary.

Would this also work with uNAP/iNAP/NAP as well? Also in terms of how much it can detonate insensitive secondaries, I am thinking of switching from melt-cast ETN to RDX as RDX is the superior secondary, but I am wondering if (say) 50 or 100mg of lightly pressed uNAP/iNAP/NAP is sufficient to set it off? Or is more pressing/quantity needed for it to work?

Hey Buddy - 20-10-2024 at 18:26

Quote: Originally posted by ManyInterests  

Is it possible that strong stirring and the ultrasonic vibration are ultimately doing the same thing? I am just throwing that thought out there.


Yes, if it is possible to magnetic stir precipitate a material which can perforate 5mm holes in foil, or detonate PETN in masses less than a mg, then NAP and uNAP are identical in performance and there is no reason for a uNAP designation, they are then the same material. If not, then no, they are not doing the same thing, and are different in performance.

Quote: Originally posted by ManyInterests  

Are you serious about the impact sensitivity being less than ETN?


Microtek has claimed this, so I would assume it to be accurate. I have not found a form of NAP that is less impact sensitive than ETN. Once in a while, a sample will withstand quite an impact, but I judge on average, it is a more sensitive material than ETN. iNAP is close, but slightly more impact sensitive than ETN in my judgement. ETN is a fairly insensitive secondary explosive. Melt state ETN is more impact sensitive than NAP. iNAP is insensitive to friction within the capabilities of my testing.

Quote: Originally posted by ManyInterests  

I have one question about uNAP/iNAP. Are they just as flame sensitive? Or is something more needed?


uNAP and NAP detonate at approximately 270 C. iNAP, perhaps a little higher temp.

Quote: Originally posted by ManyInterests  

Would this also work with uNAP/iNAP/NAP as well? Also in terms of how much it can detonate insensitive secondaries, I am thinking of switching from melt-cast ETN to RDX as RDX is the superior secondary, but I am wondering if (say) 50 or 100mg of lightly pressed uNAP/iNAP/NAP is sufficient to set it off? Or is more pressing/quantity needed for it to work?


No two detonator designs are the same, they have wide ranges. The density of the RDX alters the minimum priming masses. The interface from primary to secondary influences the transfer of the detonation. 50 or 100 mg is more than enough to detonate RDX. RDX can be detonated with 5 mg of uNAP confidently. I was attempting to demonstrate in this thread that uNAP detonates PETN at less than 1 mg masses. It's like I'm just writing these posts to myself.:P


[Edited on 21-10-2024 by Hey Buddy]

Brightthermite - 21-10-2024 at 09:10

Quote: Originally posted by pjig  
Brightthermite:
Did you give the reacted materials a longer cool down process? How was your procedures done?


Procedure - Heat each liquid to a boil, dump all materials in at once, reflux for 5 min. If material formed during this like iNAP it was immediately dumped out. If not I gave the liquids 10 mins to precipitate. I did not wait longer because if it takes longer to form then 10 mins I might as well just use water which we know to work and produce a good product.

What did form at 70% looked pretty much identical to what would form with water. Next time I revisit this I'll make some both with water (looking to test out uNAP and NAP anyway) and compare to the 70%.

Brightthermite - 21-10-2024 at 09:22

Quote: Originally posted by ManyInterests  


I am looking at uNAP and iNAP right now due to some difficulties that I am having with NHN going full detonation in non-steel containers. My questions are concerning its long-term stability and safety in hand loading.


I cant speak for stability yet but looking at this forum and youtube it seem to be pretty good. Handing was really good. I was able to be much rougher with it then I ever would be during loading and had no issues. I don't have experience with other primaries to give you a comparison though.

Quote: Originally posted by ManyInterests  

The way I make my detonators, and I made a lot of them thus far, is to load the secondary first with as much pressure as I can do by hand (I don't have an arbor press or any mechanical means of loading my caps), followed by topping it with the primary and only very gently tamping it without any hard pressing (I sometimes tap on the sides of the cap to help the material get more compacted before gently tamping everything down.

I assume this is a safe process for doing it with uNAP or iNAP?


I would say that's safe with iNAP, I cant speak for uNAP. As long as you have a set up where a cap can go off and not kill you, you should be fine. Looking at Buddy's research tho be aware that you may have to use some larger loads for iNAP to work well unless you use some kind of reinforcing cap like I mentioned. 

Brightthermite - 21-10-2024 at 09:36

Quote: Originally posted by Hey Buddy  
Quote: Originally posted by ManyInterests  

Is it possible that strong stirring and the ultrasonic vibration are ultimately doing the same thing? I am just throwing that thought out there.


Yes, if it is possible to magnetic stir precipitate a material which can perforate 5mm holes in foil, or detonate PETN in masses less than a mg, then NAP and uNAP are identical in performance and there is no reason for a uNAP designation, they are then the same material. If not, then no, they are not doing the same thing, and are different in performance.


I take it you have not investigated this much yet? Again when I am able to revisit this I'll check it out. Im very curious and it would save some people having to get an ultrasonic cleaner if they are similar enough materials.




Hey Buddy - 21-10-2024 at 10:45

Quote: Originally posted by Brightthermite  

I take it you have not investigated this much yet? Again when I am able to revisit this I'll check it out. Im very curious and it would save some people having to get an ultrasonic cleaner if they are similar enough materials.


Yes, I have investigated it. Ultrasonic crystallization was first tried because of the better performance of small crystals from large crystals.
I have multiple sizes and grades of NAP from small powders to large crystals. uNAP out performs everything Ive produced. Most likely, because it is a smaller crystal.

Microtek has claimed he is achieving the same performance as uNAP from stirred precipitation.

My attempts at stirred precipitation are at 250 rpm. Microtek stated he is using a higher RPM of 500 or so. I am working on some experiments at 500 rpm and up today to more accurately examine if this can be replicated. If the same criterion can be met, I see no reason for uNAP to be differentiated from NAP at all. Of course I don't suspect it is possible at all, because I have attempted it. Still, if Microtek says it, I trust his judgement.

I bought the ultrasonic cleaner used to develop uNAP for $25. The same principle of crystal disruption via sonication should apply to anything else so it is a worthwhile investment IMO.

20241021_134910.jpg - 3.1MB

[Edited on 21-10-2024 by Hey Buddy]

[Edited on 21-10-2024 by Hey Buddy]

Hey Buddy - 21-10-2024 at 13:18

I followed Microtek's recommendation to stir at higher rpm than 250. I stirred during precipitation at 1200 rpm, which was aggressive and precipitated quickly. This produced a pink powder that is able to detonate 5mm holes in foil, it seems just as capable from that point. I have not had success with transferring detonation to PETN in tiny quantities. Going to attempt some more high magnification images to compare.

[Edited on 21-10-2024 by Hey Buddy]

I've been trying to recreate the small mass detonations of PETN and have not been able to replicate. The difference is small but there appears to be a difference in high rpm and uNAP materials.

[Edited on 21-10-2024 by Hey Buddy]

iNAP

Hey Buddy - 21-10-2024 at 13:43





[Edited on 21-10-2024 by Hey Buddy]

BITN6993.jpg - 105kBTYOM9419.jpg - 114kBWIJE0054.jpg - 108kB

Low rpm NAP

Hey Buddy - 21-10-2024 at 14:03



CBEU8845.jpg - 196kBDQFP8442.jpg - 154kBRMPF3466.jpg - 189kBBMJV6250.jpg - 194kB

uNAP

Hey Buddy - 21-10-2024 at 14:04



EFGV9775.jpg - 201kBQZOS6428.jpg - 226kB

1200 rpm NAP

Hey Buddy - 21-10-2024 at 14:05



ELZQ2287.png - 1.1MBFEZJ5068.jpg - 160kBPWVB6838.jpg - 173kBUQNA0407.jpg - 156kB

ManyInterests - 21-10-2024 at 17:17

Quote:
Microtek has claimed this, so I would assume it to be accurate. I have not found a form of NAP that is less impact sensitive than ETN. Once in a while, a sample will withstand quite an impact, but I judge on average, it is a more sensitive material than ETN. iNAP is close, but slightly more impact sensitive than ETN in my judgement. ETN is a fairly insensitive secondary explosive. Melt state ETN is more impact sensitive than NAP. iNAP is insensitive to friction within the capabilities of my testing.


Yeah I don't need to lose any fingers (or whole hands) to misconceptions. So far with this hobby I have avoided any and all serious injuries and I don't plan on having any incidents. The worst I had is inhalation issues and given the toxicity of NAP byproducts I am having some serious worries about that.

By melt-state ETN I assume you mean ETN as it is molten? Once it cools back down and hardens it is safer to handle. Still more sensitive, but I have melt-cast ETN and ground it back up again many times without any incident.

Which is the more impact sensitive than NAP? Melt-cast and resoldified ETN or ETN as it is in liquid form?


Quote:
uNAP and NAP detonate at approximately 270 C. iNAP, perhaps a little higher temp.


I'll have to test that by putting a nichrome wire e-match next to some when testing to see if it does set it off then without a safety match on the wire.


Quote:
No two detonator designs are the same, they have wide ranges. The density of the RDX alters the minimum priming masses. The interface from primary to secondary influences the transfer of the detonation. 50 or 100 mg is more than enough to detonate RDX. RDX can be detonated with 5 mg of uNAP confidently. I was attempting to demonstrate in this thread that uNAP detonates PETN at less than 1 mg masses. It's like I'm just writing these posts to myself.:P


Yeah sorry about that, I didn't have time to fully read everyone's posts... and wow, that is a teeny tiny amount, so maybe just 25mg that is very lightly and gently pressed is all I need.

and I am very tired as I write this, so I probably missed out on what others have written. I also will need to review Dugan Boomfax's videos on it. He does show quite a lot of good stuff there.

There is one safety question I do have: Is there a safe way to neutralize and dispose of NAP (and all variants) without detonating them in some remote area?

Hey Buddy - 21-10-2024 at 17:58

Quote: Originally posted by ManyInterests  

Which is the more impact sensitive than NAP? Melt-cast and resoldified ETN or ETN as it is in liquid form?


NAP forms I've tested are all more impact sensitive than powder ETN. If it is melted ETN in question, it is much more impact sensitive than NAP. Large crystal slow precipitation NAP is quite sensitive, detonating with only a slight tap from a 4lb hammer. iNAP is more impact and friction insensitive than any other high powered primary I'm familiar with besides some of the unusual tetrazoles.

Quote: Originally posted by ManyInterests  

I'll have to test that by putting a nichrome wire e-match next to some when testing to see if it does set it off then without a safety match on the wire.


Glowing nichrome ranges from somewhere between 400 C to 1000 C so it is definitely going to surpass 270 C, which will detonate NAP immediately assuming there is heat transfer.

Quote: Originally posted by ManyInterests  

Yeah sorry about that, I didn't have time to fully read everyone's posts... and wow, that is a teeny tiny amount, so maybe just 25mg that is very lightly and gently pressed is all I need.


No worries, I'm happy if I can help. I am soft for SM members. SM has taught me so much.-- On primes, It will depend on your exact configuration but IMO 25 mg of any NAP in contact with RDX at medium to low density, will transfer detonation.

Quote: Originally posted by ManyInterests  

There is one safety question I do have: Is there a safe way to neutralize and dispose of NAP (and all variants) without detonating them in some remote area?


You can boil NAP to decompose it, it will turn black when destroyed. Water itself desensitizes it and it doesn't detonate when wet. It sort of crackles and pops. If you boil NAP black, it is likely nickel oxide in there along with some perchlorate which can contaminate water and interfere with thyroid glands in people and animals if they indirectly ingest it or absorb it at high enough concentration.

ManyInterests - 22-10-2024 at 15:04

Quote:
NAP forms I've tested are all more impact sensitive than powder ETN. If it is melted ETN in question, it is much more impact sensitive than NAP. Large crystal slow precipitation NAP is quite sensitive, detonating with only a slight tap from a 4lb hammer. iNAP is more impact and friction insensitive than any other high powered primary I'm familiar with besides some of the unusual tetrazoles.



Quote:
No worries, I'm happy if I can help. I am soft for SM members. SM has taught me so much.-- On primes, It will depend on your exact configuration but IMO 25 mg of any NAP in contact with RDX at medium to low density, will transfer detonation.



This information is what I need, and the uNAP variant is what I am looking at the most, since it does appear to be superior to iNAP. I plan on hard pressing RDX in my caps as much as I can (as it is much safer to press anyway... RDX is quite forgiving), but as you and others have noted: The harder the pressing of the secondary, the bigger punch you need to set it off, meaning I need I will want to add more than 25mg (like I said, 50mg or 100mg... make it 100mg) to absolutely guarantee detonation.

And loading that much might be dangerous. But given that it did take Dugan Boomfax did give some uNAP bits a few good smacks with his 4 lb steel hammer to get it to go off, I might be exaggerating, especially with how softly I press my primaries nowadays.

Another thing that could be done is to do what Dugan did with iNAP by loading the material in a plastic tube that is making contact with a fuse/e-match and then inserting that into the blasting cap. He said he does this mostly with iNAP and not often with uNAP, but he did imply he has done it that way. This does more friction work than impact, and uNAP is quite friction insensitive.

Quote:
Glowing nichrome ranges from somewhere between 400 C to 1000 C so it is definitely going to surpass 270 C, which will detonate NAP immediately assuming there is heat transfer.


I believe you! I will still test it to be sure once I have everything.

Quote:
You can boil NAP to decompose it, it will turn black when destroyed. Water itself desensitizes it and it doesn't detonate when wet. It sort of crackles and pops. If you boil NAP black, it is likely nickel oxide in there along with some perchlorate which can contaminate water and interfere with thyroid glands in people and animals if they indirectly ingest it or absorb it at high enough concentration.


and I assume after the NAP is destroyed, some elemental iron will be needed (some steel bits will work I assume?) in order to destroy the perchlorates as well.

Brightthermite - 26-10-2024 at 18:15

Quote: Originally posted by Hey Buddy  

I've been trying to recreate the small mass detonations of PETN and have not been able to replicate. The difference is small but there appears to be a difference in high rpm and uNAP materials.

[Edited on 21-10-2024 by Hey Buddy]


Interesting information. So would you say for all practical purposes they are equivalent?

Side note - where did you get those containers from in your above post? They look to be the perfect size to store primaries.

Hey Buddy - 26-10-2024 at 19:41

Quote: Originally posted by Brightthermite  
Quote: Originally posted by Hey Buddy  

I've been trying to recreate the small mass detonations of PETN and have not been able to replicate. The difference is small but there appears to be a difference in high rpm and uNAP materials.

[Edited on 21-10-2024 by Hey Buddy]


Interesting information. So would you say for all practical purposes they are equivalent?

Side note - where did you get those containers from in your above post? They look to be the perfect size to store primaries.


Yes, I think they are practically equivalent, there is a difference in sensitivity, and uNAP seems to have a slight edge in small masses. I tested this 1200 rpm for mechanical sensitivity and found it similar in friction sensitivity. iNAP is considerably more insensitive to impact and friction than uNAP or high RPM NAP.

I buy those special containers from a seller on ebay for small experimental samples, because they have colored caps that help me keep track of the samples. https://www.ebay.com/itm/264701055849

Microtek - 27-10-2024 at 09:26

Ok, I have synthesized uNAP from [Ni(NH3)6](ClO4)2 and AQ*HClO4, which is the method I prefer to use. After boiling 5 minutes, the clear black solution was transferred to an ultrasonicator which was set to 22 C, and sonicated for 10 minutes. The product was seen to precipitate very abruptly shortly after being put in the sonicator. After the 10 minutes, the mix was filtered, washed with a small amount of water and twice with ethanol and then dried at around 30 C in air.

My observations are:

The uNAP contains very fine particles (some hundreds of nanometers), but also larger crystals of up to about 5 um in diameter and somewhat longer than that.

When heated on Al foil over a flame, uNAP is very impressive, detonating with great brisance in sub-milligram quantities as Hey Buddy has reported. In this regard it surpasses NAP prepared with continuous stirring.

I haven't yet had time to test sensitivity.

I think ultrasonication offers at least one distinct advantage over other methods of NAP preparation, and that is the rapidity with which the product separates from the mother liquor. I hypothesize that the ultrasonics help with nucleation, and it obviously and unsurprisingly also prevents the formation of large crystals as precipitation occurs.

ManyInterests - 28-10-2024 at 13:51

Quote: Originally posted by Microtek  
Ok, I have synthesized uNAP from [Ni(NH3)6](ClO4)2 and AQ*HClO4, which is the method I prefer to use. After boiling 5 minutes, the clear black solution was transferred to an ultrasonicator which was set to 22 C, and sonicated for 10 minutes. The product was seen to precipitate very abruptly shortly after being put in the sonicator. After the 10 minutes, the mix was filtered, washed with a small amount of water and twice with ethanol and then dried at around 30 C in air.

My observations are:

The uNAP contains very fine particles (some hundreds of nanometers), but also larger crystals of up to about 5 um in diameter and somewhat longer than that.

When heated on Al foil over a flame, uNAP is very impressive, detonating with great brisance in sub-milligram quantities as Hey Buddy has reported. In this regard it surpasses NAP prepared with continuous stirring.

I haven't yet had time to test sensitivity.

I think ultrasonication offers at least one distinct advantage over other methods of NAP preparation, and that is the rapidity with which the product separates from the mother liquor. I hypothesize that the ultrasonics help with nucleation, and it obviously and unsurprisingly also prevents the formation of large crystals as precipitation occurs.


I will be looking with great interest in your tests. Especially the sensitivity tests for obvious reasons.

Microtek - 29-10-2024 at 01:21

I have performed a round of sensitivity tests on the uNAP. I recorded 5 out of 5 no go's a the max setting of my apparatus, same as the stirred NAP. For this reason, I can't conclude anything about the sensitivity of uNAP versus stirred NAP, but I can conlude that they are both less sensitive in this test than PETN.

I took this picture through my microscope. It is perhaps not clear in this image, but the little specks seen in the frame are small crystals of NAP. The much larger crystal just on the right edge of the central frame is about 10 micron in diameter (I have an etched slide with a scale to compare).

In my opinion there are real differences in the performance of uNAP and stirred NAP on the very small scale, however, I think it can be explained solely by particle size effects. Furthermore, I think the differences are negligible in most practical applications. The purpose of a primary is usually to initiate a base charge, and stirred NAP (or even larger crystals of NAP) will accomplish this very effectively in minute quantities; 10-20 mg or so. Even 100 mg pressed into a standard detonator body takes up space like the skin on an apple, so there is rarely a reason to use just 5 mg.



IMG_20241027_134102_446.jpg - 754kB

ManyInterests - 29-10-2024 at 17:07

Quote:
I have performed a round of sensitivity tests on the uNAP. I recorded 5 out of 5 no go's a the max setting of my apparatus, same as the stirred NAP. For this reason, I can't conclude anything about the sensitivity of uNAP versus stirred NAP, but I can conlude that they are both less sensitive in this test than PETN.


So they are less impact sensitive than PETN? That is a big big advantage, but I am also kinda still worried if there is something different about your uNAP vs how Dugan Boomfax did it. What was your test? when you say 5 out of 5 no go's you mean you tested it 5 times with impact tests and they all failed to detonate? Or was your test something else? I know that uNAP has greatly reduced friction sensitivity, enough that I don't need to worry about it when loading and pressing, but it is the impact that worries me the most.

Because like I said many times before, when I load by hand (wearing gloves of course) and am using NHN, if some NHN lands on my glove and not in the cap, I scrape it into the cap gently. So I know uNAP can handle that. After that I take my dowel and tap the side to get everything to be more compacted before I slowly and gently insert the wooden dowel and very lightly and slowly press a few times with less than 1kg of force (maybe even a less than 100 grams) to more simply compact the stuff than to press it. The NHN might even still fall out if I tip it to the side (albeit I never tried that) due ot how lightly pressed it is. I do do some scraping on the side to make sure everything is in an even layer.

After this it is either the e-match with some epoxy or a fuse with crimping the cap (I collar the fuse with electrical tape to make a snugger fit).

I could build a pressing apparatus using syringes and water (similar to this), but that might apply more pressure than what is needed.

I mentioned it many times, but this is my anxiety disorder speaking. I was like this when I was loading my first caps with ETN and NHN, and I know now those are very safe to work with. I just want to know if I can do the same with uNAP.

pjig - 29-10-2024 at 18:47

U-nap should be very well suited for this process , probably better than anything I’ve run across in years of research. Its is very healthy to be extremely cautious with HE materials. Never loose that , complacency is the mother of all disasters.

Hey Buddy - 30-10-2024 at 10:06

Quote: Originally posted by Microtek  
I have performed a round of sensitivity tests on the uNAP. I recorded 5 out of 5 no go's a the max setting of my apparatus, same as the stirred NAP. For this reason, I can't conclude anything about the sensitivity of uNAP versus stirred NAP, but I can conlude that they are both less sensitive in this test than PETN.

I took this picture through my microscope. It is perhaps not clear in this image, but the little specks seen in the frame are small crystals of NAP. The much larger crystal just on the right edge of the central frame is about 10 micron in diameter (I have an etched slide with a scale to compare).

In my opinion there are real differences in the performance of uNAP and stirred NAP on the very small scale, however, I think it can be explained solely by particle size effects. Furthermore, I think the differences are negligible in most practical applications. The purpose of a primary is usually to initiate a base charge, and stirred NAP (or even larger crystals of NAP) will accomplish this very effectively in minute quantities; 10-20 mg or so. Even 100 mg pressed into a standard detonator body takes up space like the skin on an apple, so there is rarely a reason to use just 5 mg.



I really enjoyed reading this. Thank you.

Microtek - 30-10-2024 at 11:26

Hey Buddy: It was my pleasure.

Many Interests: When I refer to 5 out of 5 no go's, it means that I have conducted the experiment five times (with fresh samples of uNAP on fresh sand paper each time) and all five times the uNAP did not react by being struck. In the same test, PETN usually reacts once or twice in five attempts.

Bear in mind that mechanical sensitivity is stochastic in nature, at least to an extent. That is to say, 5 out of 5 no-go's is not a guarantee that it will never react to this stimulus.
However, I am surprised that impact sensitivity is your main concern when loading caps. I think high force impacts should be exceedingly unlikely during this operation, but grinding the substance between surfaces such as detonator body and ram rod is probably a fairly common occurence.

ManyInterests - 30-10-2024 at 17:40

Quote:
However, I am surprised that impact sensitivity is your main concern when loading caps. I think high force impacts should be exceedingly unlikely during this operation, but grinding the substance between surfaces such as detonator body and ram rod is probably a fairly common occurence.


So I was wrong to assume that impact and pressure is the thing I should be worried about but more on the friction side? If that is the case, then given that uNAP is very friction resistant then I guess I scan safely assume I can load it and press it normally like I do NHN?

My main worry about that when I was pressing (with gradual increases in pressure obviously, no sudden smacks!) that would be the thing that would set off my cap prematurely. I always thought this would be more impact than friction (though the friction obviously would have a huge factor, too).

pjig - 30-10-2024 at 19:48

So the issues that arise are usually from large Chrystal formations that are very sensitive, some primary’s like lead azide are prone to det upon breaking the Chrystal structure. Same with nap, large crystals (not u-nap or inap) . But I believe that the sensitivity of this nap material is way less compared to LA. I still would caution being aware of this potential danger. Microscopic investigations are a good way to confirm your size and shape of finished primary .
Blast sheild all safety gear are recommended for pressing process. It’s always un-nerving feeling pressing primary portions .
Several folks suggest a lot of pressure to get commercial standard pressures for caps … some say (amateurs) light pressure. I assume the caps purpose is more the dictating factor and what materials it has to initiate.

Microtek - 31-10-2024 at 08:59

I would recommend building a setup that can handle an accidental detonation during the pressing process. A vice with a shield that can resist the small fragments from a cap is not hard to improvise. It will be worth it in terms of peace of mind, even if NAP (stirred or ultrasonicated) or other very safe primary is used.

In regards to pressure, I would suggest pressing the base charge quite firmly (maybe a few thousand psi), then optionally a layer pressed at just a few hundred psi, and finally the primary also at a few hundred psi. I set off my NAP with an arc discharge through a pinch of fluffy gun cotton held in a 3 mm ID plastic cup that is inserted into the cap. The flash is enough to get it going every time, so I don't think you have to worry that pressing the primary will make it too difficult to ignite.

ManyInterests - 1-11-2024 at 07:34

Well I have always used an e-match with the nichrome wire around a safety match to provide flame and the only time it failed it when the epoxy plug seeped down and blocked the circuit. For my next attempts I am actually retiring the safety match and going to rely on the hot nichrome wire alone, in addition to a tighter fitting electrical tape collar and more crimping than epoxy (which I will still use as a waterproofing measure).

As for making a loading fixture, I have decided to build one. I looked online for various ideas but I settled on making something similar to the fixture found in the improvised munitions handbook. Except I will make it half as long and I will add more blast shielding. I will still need to give the primary a very, very light tamp to get rid of any air pockets. Before pressing but I should be safe. I will play loud music also when doing it as a just in case...

Edit: the reason why I am getting rid of the safety match in my igniter is because I noticed in some instances where I used things like pen bodies and even aluminum bodies that the match actually survives the blast! Meaning it was the heat of the nichrome that got to the primary before it had a chance to burn the safety match.

Once I get my nickel carbonate (the only ingredient I am missing) I will test out my e-matches to see if the nichrome alone is reliable. I will also see if it is possible to coat the wire with uNAP to turn the match also into the primary container.

[Edited on 1-11-2024 by ManyInterests]

pjig - 2-11-2024 at 09:18

Just curious why you don’t dope your nichrome wire and make a E match? There are many compositions at work great for a dip. One that comes to mine is the co-precipitate of potassium ferricyanide and potassium perchlorate

ManyInterests - 2-11-2024 at 12:35

Well I have very little potassium perchlorates (I keep forgetting to coat my old MMO electrode with PbO2 to get it to become a perchlorate anode), but I got no ferricyanide. I did read about some compositions and tested at least one out, but it didn't work. So I ditched those ideas and just stuck with a safety match.

Do you have any suggestions? Maybe putting a little gun cotton at the absolute end like Microtek did?

Microtek - 2-11-2024 at 14:34

You can crush up match heads and mix the powder with an acetone solution of NC to make a thick porridge. Then dip your nichrome wire in that. It works very well, and I use it when I do VOD measurements with ionisation probes and an oscilloscope. The fluffy NC ones are less labour intensive since all I need to do is to snip off a piece of wire with two leads and put one end into the 3d printed plastic cup I mentioned earlier. Then stuff in a small piece of gun cotton and insert the cup into the cap. It is then fired by a couple of batteries through a one dollar boost converter. This makes an arc from one lead to the other across the cut end of the wire.
These don't work for VOD measurements however, since the arc triggers the scope before the the CJ-zone even arrives at the first probe.

Axt - 2-11-2024 at 17:23

Quote: Originally posted by Microtek  
I use it when I do VOD measurements with ionisation probes and an oscilloscope. The fluffy NC

This makes an arc from one lead to the other across the cut end of the wire.
These don't work for VOD measurements however, since the arc triggers the scope before the the CJ-zone even arrives at the first probe.


Curious, at what voltage you are using across the probe and over what gap? I had made boards up which are still sitting around pic attached, with the intent to fire a charge across the PCB tracks. 2 types, some to break the 0.2mm track and other to act as ionisation probes with a gap; some 2mm and some 0.5mm. These were never tested as I never had a battery powered scope at the time.

Originally, I had planned to use about 1kV over the 2mm gap but then toned it back to low voltage over 0.5mm. Your comment seems to confirm that thought, that the higher voltage discharge would interfere with the other gaps (acting as antennas) so a lower voltage should be used.

vod boards.jpeg - 2.9MB

Brightthermite - 2-11-2024 at 17:58

Quote: Originally posted by Microtek  
You can crush up match heads and mix the powder with an acetone solution of NC to make a thick porridge. Then dip your nichrome wire in that. It works very well, and I use it when I do VOD measurements with ionisation probes and an oscilloscope. The fluffy NC ones are less labour intensive since all I need to do is to snip off a piece of wire with two leads and put one end into the 3d printed plastic cup I mentioned earlier. Then stuff in a small piece of gun cotton and insert the cup into the cap. It is then fired by a couple of batteries through a one dollar boost converter. This makes an arc from one lead to the other across the cut end of the wire.
These don't work for VOD measurements however, since the arc triggers the scope before the the CJ-zone even arrives at the first probe.


Can you explain the VOD measurement process a bit?

Also what does your primary cup look like? Pic of mine attached, there is a very small hole on the underside. These works so well to fill with then insert into your cap. Its about 10mm long.

PrimaryCupv1.png - 14kB

 Pages:  1  2