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Author: Subject: Exotic Primaries - Complex Salts
PHILOU Zrealone
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[*] posted on 20-12-2005 at 10:37


Quote:
Originally posted by Axt
Ag(N2H4)ClO2 didnt work, vigourous clear odourless bubbling on addition of AgClO2 to N2H5OH, dark grey precipitate, solution neutral. Precipitate not explosive :(


What was the exact procedure you used?
Cold Ethanol/ether saturated solutions of the reactants?
I found no reference of NH2-NH3ClO2!
But wel on NH2-NH3ClO3, NH2-NH3ClO4 and N2H4.2HClO4!
This might suggest the compound doesnt stand long if in solution or must be very unstable at room temperature... regarding the sensitivity of chlorites and of silver and hydrazine complexes maybe it is a wild dream ;) but scientist are enless daydreamers :P




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[*] posted on 20-12-2005 at 11:41


Quote:
Originally posted by Axt
Synthesis I Tried

10g copper sulphate pentahydrate was dissolved into 50ml warm water, to this was added 22g 25% ammonia, solution turned dark bluey purple on formation of the complex sulphate. Another solution was made of 10g potassium persulphate in 200ml warm water. The solutions were poured together, put into the freezer and brought down to 0°C.

On pouring off the cooled solution, a good yeild of purple "shaved-hair-like" crystals were left, they were scooped out and placed on absorbent paper in the sun to dry.



[Edited on 24-9-2004 by Axt]


I did this exact procedure exept for one variation, i used sodium persulfate. The result was a turquise goo.

I also tried adding the ammonia to a boiling solution of CuSO4 and after adding the sodium persulfate solution i let the mixture cool down. Now i got a black slush, when dry it looked and behaved exactly like CuO when mixed and ignited with Al.

What am i doing wrong? Could it be the sodium persulfate? The jar says sodiumperoxydisulfate.
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Microtek
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[*] posted on 21-12-2005 at 04:38


About the silver and hydrazine complex above, I think it fails due to oxidation of the hydrazine by the silver ions. At least, I get the same result if I mix AgNO3 and hydrazine hydrate ( and also CuSO4 and hydrazine ). I believe that the precipitate is the colloidal metal which then flocculates.
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PHILOU Zrealone
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wink.gif posted on 21-12-2005 at 05:04


Yes but it seems that under certain solvents conditions one can stil get Cu(NH2-NH2)2(NO3)2...(read above posts)...I suppose the same might happen with Ag complexes of hydrazine...



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Axt
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[*] posted on 21-12-2005 at 05:35


Quote:
Originally posted by PHILOU Zrealone
What was the exact procedure you used?

Aqueous hydrazine was added to AgClO2 under water, under ethanol it does the same (its not soluble in ethanol, only slightly in water). Hydroxylamine acts on AgClO2 the same as hydrazine.

pihop, the persulphate is quite unstable, and practically useless, decomposing within a couple days. Try milder conditions, dont heat it, the higher solubility of sodium persulphate should allow you to keep it cool.
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[*] posted on 22-12-2005 at 08:39


Quote:
pihop, the persulphate is quite unstable, and practically useless, decomposing within a couple days. Try milder conditions, dont heat it, the higher solubility of sodium persulphate should allow you to keep it cool.


I don't really mind that it's unstable, I want to do it just for the heck of it and for the feeling of success even though the synth is really easy.

I tried many different variations of the method, boiling solutions, cold solutions. I tried to dissolve the CuSO4 and sodiumpersulfate in the same solution and then adding the ammonia.

I will buy more ammonia and get ammoniumpersulfate and then try again.

It crossed my mind that the chemicals i use isn't really lab grade. Since such pure chemicals are hard to come by in sweden and are very expensive (i'm a poor student) i use chemicals from the hardware store and such. I guess the sodium persulfate is fairly pure but the CuSO4 and and the ammonia is from the local hardware store.

How sensitive is the reaktion to contamination of any sort?

[Edited on 24-12-2005 by pihop]
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Rosco Bodine
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[*] posted on 23-12-2005 at 20:08


Quote:
Originally posted by Nick F
I've made nitroguanidine and aminotetrazole complexes of silver nitrate, I can't remember if I tried copper... it was a while ago so my memory is a bit hazy, but I can make some more and post a bit of info.
They seemed quite good from what I can remember, but they're probably less effective, and no more OTC, than azides...



Two different compounds which are lead double salts involving tetrazole variants
and styphnic acid , may be superior initiators to lead azide .

See PATR vol. 9 page T-121
Lead Diazoaminotetrazolate Styphnate is an
interesting compound .

US2064817 supplies useful information for the precursor to this and related cpds.

US2090745 describes the simple Lead Diazoaminotetrazolate salt

US3310569 Crystalline Double Salt Pb Styphnate and Pb Nitroaminotetrazole
GB1069440 British patent same subject
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[*] posted on 7-2-2006 at 18:45


Pihop: I have sucessfully used sodium persulfate (from electronics store) to make tetraamminecopper persulfate. Try adding the ammonia to the copper sulfate first. I add the ammonia directly to crystals of CuSO4 until it dissolves to form a deep blue solution of tetraamminecopper sulfate. Then, add a solution of the sodium persulfate to this. Add alcohol (I used 70% isopropanol) until the crystals precipitate and a layer of clear alcohol can be seen on top of the suspended crystals. Filter these out and let dry for about 2 days.

Also, heating will decompose the ammonia complex and possibly the persulfate. Keep the reaction cold.

The finished product consists of light purple needle-like crystals.

[Edited on 8-2-2006 by pyrochem]
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[*] posted on 28-2-2006 at 12:37


I have seen, that hexaamminenickel diperchlorate was mentioned in this thread before. Therefore I thought it may be interesting for some people to see how hexaamminenickel diperchlorate looks like. Here's a picture. It can be enlarged by clicking on it.

              

I've prepared this compound by adding ammonia and ammonium perchlorate solution to a nickel sulfate solution. I prepared it, because I was curious the see how it looks like and beside I read in an old book, that hexaamminenickel diperchlorate is such insoluble, that it can be used for quantitative precipitations of nickel-ions. However this was not true under my conditions. Only 70% of the nickel-ions precipitated. I worked at room temperature with diluted solutions. Cold ethanolic solutions would cause for sure the precipitation of more nickel.

I know, that this compound isn't only interesting for analytical purposes, but for pyrotechnics too. I am not very interested in pyrotechnics, so the only thing I tested was if the compound burns or not. I light it with a lighter and it burned slowly with a white to bright blue flame.

Perhaps German speaking members want to take a look at the preparation on LambdaSyn: www.LambdaSyn.com/synfiles/hexamminnickelperchlorat.htm.

~Mephisto




Visit the German synthesis collection LambdaSyn and our new LambdaForum!
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[*] posted on 2-4-2006 at 06:37
New "green" nitrotetrazole-based primaries


This the abstract:

http://www.pnas.org/cgi/content/abstract/0600827103v1

Would anyone have access to the full article ?
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[*] posted on 2-4-2006 at 09:23


Was definatly an interesting read!

Attachment: green primarys Environmentall friendlyenergetic complexes.pdf (473kB)
This file has been downloaded 2192 times





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Chris The Great
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[*] posted on 4-4-2006 at 00:36


Agreed! As good as lead azide, easily ignited, high brisance/power, insensitive, non-toxic, stores easily....

The only drawback is that the synthesis is a little long but completely doable by someone who is determined and has a little time. I have set it as my new priority, I have all the chems needed I just need to combine them in the right order and sequence under the right conditions...

Thank you for posting this roguechemist and pdb.

[Edited on 4-4-2006 by Chris The Great]
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[*] posted on 3-5-2006 at 08:57
Nice detos.


Hi everybody!

During the weekend and the 1:st of May I experimented with homemade detos.
In short they concisted of 1g copper tetramine perchlorate with 0.5g of LNP (lead nitrato phosphite) on top...then just a fuse.
They were incredibly powerful! You can check som sort of instructions for making CTAPC above (in an earlier post from me) LNP is also very simple, and safe to make...i usually make a batch of say 100g and keep it wet as it is very sparksensitive but not sensitive to impact. Check the synthesis from Megas site.
I must say that LNP is one of my favourites, simple, detonates from flame, insensitive, but unfortunately weaker than e.g. lead azide.

One concern with these detos is that will the two components react?
I will test the sensitivity of CTAPC mixed with LNP when I have time. Does Lead Xamine perchlorate exist? I know that copper nitrato phosphite does not, because I have tried to make it when I was younger...

If these detos prove to be stable I will definitely start using them...I have tried 4 of them so far and they performed great! A 10-15cm crater on the lawn. I have 2 now in storage to see if they blow up or preserve, I have to be very carful with them till I know more. Actually I should have done more experimenting with the substances before I made detos.

One more thing that I wanted to say is that AgNTZ is absolutely great. Less shocksensitive than many others and more powerful. I made some 1:st of may bangers with 100mg in each...they were loud and nice!
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[*] posted on 24-10-2006 at 13:44
Iron-anion based new primary


See the following link:

http://www.townhall.com/News/NewsArticle.aspx?ContentGuid=73...

Any idea of what this stuff could be ?
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Axt
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[*] posted on 24-10-2006 at 15:25


Quote:
Originally posted by pdb
Any idea of what this stuff could be ?


Isn't it likely, just the NH4FeNT or NaFeNT as mentioned in the green primary article you requested a few posts up? both mention Los Alamos National Labs as the culprit, same scientist too.
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[*] posted on 25-10-2006 at 06:12


You are obviously right, my dear Sherlock ! ;)

I just have forgotten my previous request... Alzheimer, so soon ?!
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[*] posted on 26-10-2006 at 15:23


This is an unusual mixture which I have posted before
in another thread , but probably deserves mention here
also . It is one of the few primaries capable of use as an
initiator of base charges , which is relatively insensitive to
shock , but is sensitive to detonation by heat or flame .

Possibly the barium styphnate would behave similarly
in admixture with silver azide , or with silver acetylide / silver nitrate double salt . Another possibility which
could be useful is silver fulminate in combination with
the barium styphnate .

Silver fulminate has always been intriguing to me even though I have never made it . It has exceptional power
as an initiator and is easily made and is storage stable , yet it is reportedly too dangerously sensitive to have practical value in its common form . So I have wondered
if there was possible some special treatment for silver fulminate which might change its properties to a safer form , which could have practical use . Recrystallizing the silver fulminate in a microcrystalline , very fine almost
colloidal particle size form should desensitize it considerably . And another thought is that depositing
upon the silver fulminate crystals a very thin layer of
silver chromate , similarly as is done for chromated lead azide , could have value in taming the sensitivity of the
silver fulminate .

It is also possible that simply in combination with barium styphnate as an intimate mixture that a desirable desensitization might be achieved particularly if some sort
of finely divided coprecipitation or combined crystal scheme
could be achieved .

And there is also the possibility that silver fulminate could be made an included molecular component of a clathrate or other multiple salt .

I have seen absolutely nothing referenced in the literature
about these possibilities .

Attachment: US3284255 Barium Styphnate - Lead Azide mixtures.pdf (135kB)
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[*] posted on 27-10-2006 at 01:21


I have made SF a few dozain times before I could access to sodium azide and switch to LA. Among all the primaries I met, it is clearly, and by far, the one that caused the greatest number of unexpected explosions. I once had such an accident when, the filter being still dripping on the funnel, I gently brought together the SF spread on the inner walls with another piece of paper. Fortunately, it was so soaked that it deflagrated more than it detonated (and I got my face covered with black Ag2O, like in -bad- movies). Just to say that at this degree of sensitivity, I doubt there is an easy way to desensibilize it while preserving most of its initiating power (most of the time, I personnaly used it mixed with some vinylic glue diluted with water, such blend being then spread on a PETN pill and dried).

However, I am fully ignorant of the chromatization method mentionned by Rosco.

To come to the clathrates, whose Rosco is undoubtly the expert on this forum, it may be a way worth exploring, but I fear that the violence of the SF preparation reaction (MF preparation is more regular and quiter) be somewhat incompatible with the required slow growing of well balanced SF-SPicrate double salts. Unless there is an alternative way using already prepared SF ?

Last, regarding patent US3284255, it unfortunately doesn't say a single word about crystal size of the components... Also, the fact the mixture succeeds to initiate PETN doesn't teach much about its initiation strength, given PETN's high sensitivity.
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[*] posted on 27-10-2006 at 06:57


Quote:
Originally posted by Rosco Bodine

Silver fulminate has always been intriguing to me even though I have never made it . It has exceptional power
as an initiator and is easily made and is storage stable , yet it is reportedly too dangerously sensitive to have practical value in its common form . So I have wondered
if there was possible some special treatment for silver fulminate which might change its properties to a safer form , which could have practical use . Recrystallizing the silver fulminate in a microcrystalline , very fine almost
colloidal particle size form should desensitize it considerably . And another thought is that depositing
upon the silver fulminate crystals a very thin layer of
silver chromate , similarly as is done for chromated lead azide , could have value in taming the sensitivity of the
silver fulminate .


IICR there was a method of "dextrination" wherein the silver fulminate was adulterated with a hot water infused solution of dextrin and the resultant fulminate could be handeled with a margin of safety (not by much mind you). Another item from a very old pyrotechnic book included the mixing of a cuperic salt to the silver nitrate / acid solution which resulted in a fine white powder, it's crystaline element being very tiny (read azide fine) and this diminished the sensitivity while maintaining the initiation power of SF.
I have seen SF under a microscope and it does not share the consistent physical properties of MF. While mercury fulminate is relitivly consistent in shape and crystal appearence, SF is a brohen "hodge-podge" of shapes, sizes, and appearent densities. This may be a contributing factor in it's sensitivity. It's not something I would want to ever keep on the shelf however nor even work with in glass vessels. . .




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Rosco Bodine
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[*] posted on 27-10-2006 at 10:58


There has been some experimentation with silver fulminate synthesis by alternative methods done
by a Russian group . Reportedly a much lowered
sensitivity form of silver fulminate was produced .

http://mihailru.freeservers.com/

This should probably fit the " needed translations "
category nicely :D

Here is what an online translator does for the linked page above .....if you can follow any of the muddy translation

http://www.online-translator.com/url/tran_url.asp?lang=en&am...

Also there is a PEP article if anyone has access to the full pdf , please share .

http://www3.interscience.wiley.com/cgi-bin/abstract/10961752...

[Edited on 28-10-2006 by Rosco Bodine]
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[*] posted on 29-10-2006 at 09:30


There's also an American patent about forming an ammonia complex with SF, which is reportedly *much* safer than even the best dextrinated product. Later it looses NH3 and becomes sensitive again. IIRC the patent is by Gerald L. Hurst (yes the astrolite/kinepack guy). Quote:

"I have also taken a ride in an EMS
vehicle carrying one of my lab techs to the hospital with a face
and chest full of funnel splinters and eyes burned by hot gases.

His mistake? He let one single drop of water fall on a few grams
of silver fulminate resting on a filter paper.

The injured man had a lot more experience with explosives than
most of you have, and more experience with fulminates than any
of you will EVER have unless you are crazy or suicidal.

...

The best method of making the stuff is described in a 1970's US patent
which you can find by perusing the Patent Gazette in any major library.
Basically, the process creates the material as a stable chemical
adduct which subsequently slowly changes into pure explosive silver
fulminate in situ after the assembly of the final product, i.e.,
silver snaps or the like.

Personally, I wouldn't trust the author of that patent any farther than
I could throw him -- and he is a big guy (and ugly, too).

Jerry (Ico)"

Note he is describing himself!
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Rosco Bodine
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[*] posted on 29-10-2006 at 10:27


Yeah , IIRC what Jerry Hurst did is to patent something
which was already known and used by others in
the art for a long long time :D

US4270435

Speaking of taking a ride :D ........

http://music.musictnt.com/media_player/2180-10-hi.html
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[*] posted on 29-10-2006 at 10:38


Rosco, the PEP article link does not go anywhere, if it is after issue 23, I can obtain it.
I can't explain it, but I have an attraction to SF, I have made it around a half dozen times, and attempted to do some experiments with it many times. I have only suffered a couple minor accidents with it, the worst involving a small glass cut on my stomach.


While I was on PEP website...


[Edited on 30-10-2006 by The_Davster]

Attachment: silver fulminate.pdf (348kB)
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Rosco Bodine
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[*] posted on 29-10-2006 at 10:57


Sorry about the bum link , it has some sort of session cookie view authenticator which prevents off-site linking the page .

That PEP reference was Volume 3 , Issue 6 ,
( December 1978 )
p. 159-162 , Collins and Holloway ,

" A reappraisal of Silver Fulminate as a detonant "

Liebig worked with quantities of a hundred grams
in some analysis work , and while there were many
explosions .....obviously Liebig must have known
what he was doing to survive to report his findings .
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[*] posted on 29-10-2006 at 17:27


Dang, older than what I have access to.

Making clatrate type complexes with silver fulminate, would be very difficult with its standard method of preparation from acidic nitrate and EtOH, but there is sodium fulminate from the action of sodium amalgam on Hg-fulminate, which may work for the slow precipitation(which seems to be necessary) for clathrates. Or even the NaAg(ONC)2 soluble salt could potentially be used here, and it is much easier to prepare. No idea on how whether or not you determine whether or not clathrate complexes form, but could there be an interesting result from creating some sort of silver fulminate/silver nitrotetrazolate co-precipitate? Although from what I have read on SNT, it is already very good by itself.




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