Sciencemadness Discussion Board

Exotic Primaries - Complex Salts

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chemoleo - 30-3-2004 at 17:44

A while ago I had a conversation with Ph Z. on nickel complex salts. With his permission, I post the preparation of the extremely potent
Nickel Hydrazine Nitrate primary, which is known to have high VODs (betw 6-7 km/sec).
This primary has the advantage of being relatively insensitve to friction and shock, yet sensitive to heat (flame).

The preparation is very simple, once you have hydrazin or hydrazin sulphate. For the preparation of hydrazin and hydrazin sulphate, see
http://www.sciencemadness.org/talk/viewthread.php?tid=1128
http://www.sciencemadness.org/talk/viewthread.php?tid=376
http://www.sciencemadness.org/talk/viewthread.php?tid=757
for details.


PREPARATION:

1. Take Nickel nitrate (green emerald salt) saturate hot water with it...then add for 1 volume of this 1 volume of ethanol (80-99%) is fine.You have now a green ethanolic solution of Ni(NO3)2.

2. Perform the same mix but with concentrated hydrazine...use i.e. 80% NH2-NH2 what equals NH2-NH2.H2O the monohydrate....take one volume of this and add one volume ethanol. Alternatively, react hydrazine sulphate with Ca/Ba hydroxide, and filter Ca/BaSO4 off to be left with a solution of hydrazine.

3. Take the whole hydrazine batch and add dropwise under stirring the green alcoholic Ni(NO3)2 solution. A deep blue (saphire) precipitate appears which upon agitation turns lila pinkish. Continue adding the nickel nitrate solution until no more precipitate occurs. It is not a bad idea to filtrate the precipitate from time to time to ascertain whether a green coloration persists (if it does, then stop adding the nitrate solution). While mixing and precipitating, heat the mix a bit so as to adjust the addition speed in a way you can hold the mix (<50°C) (with this phrase i am not sure what he meant - surely the precipitation is works better at lower temperatures?)
The complex salt filtrate is insoluble in ethanol/water which helps fast and smooth precipitation.You get plenty of precipitate and yield is close to 100%.
Make sure the nickel nitrate solution is added in excess so as to completely use up the hydrazine.

4. Once filtered (and possibly washed with 50% EtOH/H2O0, dry on a radiator (60°C max), and after a few hours/days one gets a solid clay like cake. This can be broken ground into small pieces/dust (no risks of explosion as long as you don't hit it with a strong hammer blow...grinding with a spoon is riskless). After grinding allow to dry one more day. After this the complex salt has turned into a pale white dust that burn fiercely and bright white when lit (like nitrocellulose). When wrapped in Al foil, and thrown into a fire, one gets a powerful detonation (whereby the Al foil acts as a weak confinement)


Side Notes:
Make sure the hydrazine is free of ammonia, best way to assure this is to simply use the hydrazin sulphate, which doesnt dissolve well, while ammonium sulphate does.
NH3 makes a blue complex with Ni(NO3)2 that is unsoluble in pure ethanol but soluble in water. So if you have only a blue precipitate and no pink, this means that you have a majority of NH3 in your NH2-NH2.
The pink hydrazine complex is weakly soluble in cold water while the blue ammonia complex is very soluble!
Upon shock the nickel hydrazine nitrate comple has the sensitivity of TNT (which is very safe) but still don't hit a hammer on it and grind it mildly.

This primary can be used in combination with Ag2C2.HNO3x (1/2-1/3), which increases the sensitivity a bit, while reducing the VOD/Power only very little...

To confirm you have the right stuff, the NHN complex salt should dissolve in excess ammonia, i.e. 6NH3 + Ni(NH2-NH2)3(NO3)2 <---> NH2-NH2 + Ni(NH3)6(NO3)2



Other hydrazine nitrate complexes:
Of course there are many to be tried.
Cu(NH2-NH2)3or2(NO3)2 decomposes immediately... so the corresponding Co, Ag, etc complexes are definitely worth trying.
In fact, I just realised, he actually tried the Co complex too, it is pale orange-brown and when dry it displays identical properties to Ni salt (same burning rate) .



Some more notes on energetic complex salts:

Copper tetraamine nitrates can be seemingly prepared the same way. Partially alchoholic solutions of each, and precipitation of the complex salt upon mixing (which by itself suggests a new compound formed). To achieve better precipitation, one can add ether, which precipitates ionic compounds.
Copper tetraamine perchlorates/chlorates exist too, they have a higher VOD than the nitrates (4-6 km/s, as opposed to 3-4 km/s for the nitrates). The perchlorates go to up to 95% of that of TNT, however they are more sensitve than the nitrates.

On the note of nitrate/chlorate/perchlorate complexs, consider this: Ni(NH2-NH2)3(ClO4)2 is explosive in solution while its nitrate is stable (! see above preparation); Cu(NH2-NH2)2(ClO4)2 doesn't exist but its nitrate is on the edge of existance.
Tendency-wise, such Co and Ni complexes are more likely to exist than their Cu brother.


At last

What I'd like to see in this thread is the general discussion of more or less energetic complex salts, as long as they haven't been discussed before (such as acetylides, TACC etc).
I am thinking of, i.e. ethylenediamine perchlorate complexes, hydroxylamine nitrate/perchlorate complexes, and so on!
Plus, all the different types of ammonia-nitrate/perchlorate complexes, whatever you can think of!
Get your imagination going!

[Edited on 31-3-2004 by chemoleo]

The_Davster - 30-3-2004 at 18:24

I have done some work with tetraaminecopper(II) nitrate, and I hope to try tetraaminecopper(II) acetylide soon. I had started a thread on these types of copper compounds already, do you think I should repost my experiments here in this thread for completeness?

chemoleo - 30-3-2004 at 18:41

Yes, I realise now it's a bit tricky.

In that thread ( http://www.sciencemadness.org/talk/viewthread.php?tid=1732 ), copper complex ions are discussed in general, while here, I'd hope to focus on the energetic ones, with any metal ions.
Might make sense to separate the two.
The reason why I posted this as a general topic (i.e. complex salt primaries) was because it doesn't just mention the nickel hydrazine complexes, but a few more, plus the tendencies between different cations.

I don't know how well it will work out in reality, but it may make sense to keep these things separate...plus it will keep such ideas combined in a single thread, which is easier to follow.

Nick F - 31-3-2004 at 04:44

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...

energetic complexes

Alchemist - 1-4-2004 at 07:13

How about trying some of these! I have many more I’ll try finding this weekend. The Alchemist.

hexamminenickel perchlorate (HANP)
tetramminecopper perchlorate (TeACP)
tetramminecopper nitrate (TeACN)
tetramminecopper perchlorate-nitrate (TeACPN)
tetramminezinc perchlorate (TeAZP)
tetramminezinc permanganate (TeAZM)
tetramminecopper permanganate (TeACM)
hexamethylenetetramine sulfate-perchlorate (HSP)
tetramminezinc chlorate (TeAZC)
hexamethylenetetraminemagnesium chlorate (HMC)

kryss - 15-4-2004 at 15:27

Found this in a patent :US 6,241,281

Example 7

The nitrate salt of copper tetraammine was prepared by dissolving 116.3 g of copper(II) nitrate hemipentahydrate in 230 mL of concentrated ammonium hydroxide and 50 mL of water. Once the resulting warm mixture had cooled to 40.degree. C., one liter of ethanol was added with stirring to precipitate the tetraammine nitrate product. The dark purple-blue solid was collected by filtration, washed with ethanol, and air dried. The product was confirmed to be Cu(NH.sub.3).sub.4 (No.sub.3).sub.2 by elemental analysis. The burning rate of this material as determined from pressed 1/2-inch diameter pellets was 0.18 inches per second at 1,000 psig.

Interesting!

chemoleo - 15-4-2004 at 16:43

This surely confirms that non - aqueous conditions are not needed, ultimately. Essentially, precipitation by EtOH/aceton should be sufficient. I wonder whether that holds for copper tetraamine chlorate, too - and still I don't see why not, despite, the fact that the synth. is recommened to be done by bubbling NH3 gas through the solution.

Anyway... keep checking, there are a number of interesting complexes to test - i.e. ethylenediamine nitrates, hyrdroxylamine nitrates, and hydrazine nitrates (and possibly chlorates, perchlorates, with various metals).
It's quite a task I know.. but an interesting one!

[Edited on 16-4-2004 by chemoleo]

Other Alcohols?

hodges - 16-4-2004 at 16:22

I wonder if it has to be ethanol? Would isopropyl alcohol work. I take it the only purpose of the alcohol is to produce a solution that the desired product has a lower soluability in than the original aqueus solution?

Guanidine complexes?!?

chemoleo - 25-4-2004 at 17:01

Recently I did a few trials with guanidinium chloride.
I prepared the guanidine base by mixing GdnHCl with NaOH, specifically by dissolving GdnHCl in hot ethanol, and adding a 1.2 fold stoichiometric excess of NaOH. The NaCl precipitates (mostly), and I am left with a reasonably clean alcoholic guanidine-base extract.
This was diluted 50% with H2O.

I mixed this with 50% alcoholic CuCl2, NiCl2, and CoCl2 (as I dont really know the stoichiometry, I added an excess of guanidine base).
Interestingly, for the first two no colour change was observed, and no precipitation occurred. However, the cobalt solution changed to a very dark beautiful blue ink-like solution... clearly indicating that complexation occurred!
Unfortunately, adding more alcohol did not lead to precipitation. However, this will be tested with ether, and various other solvents.
Anyway... these experiments where done to see whether guanidine forms complex salts, and it was found indeed they do!
I shall, when I get the chance again, try the same story with cobalt nitrate, or possibly perchlorate. Hoping I can purify this!

Let's see where this adventure shall lead!!!


PS hodges, isopropylalchohol should work, too, if not better. Its hydrophobic character is more pronounced. In fact, I think I should try my future experiments with isopropylalcohol, maybe I could have precipitated the cobalt-guanidine complex with that!

[Edited on 26-4-2004 by chemoleo]

Trinitrotriamine cobalt (III) Co[(NO2)3(NH3)3]

chemoleo - 27-6-2004 at 17:03

Here's a prep I recently found. I suspect it has some interesting properties :)

Procedure
Dissolve 6.2 g (0.025 mole) of Co(II) acetate tetrahydrate in 50 ml of hot water, then cool in an ice bath and add a cooled solution of 5.2 g NaNO2 in 25 ml 0.88 molar (?? it's not clear on that) ammonia.
Cool to 10 deg C.
Add 7 ml of 20 volume (2 M ) H2O2 slowly, with sitrring, and then add 1 g of activated charcoal. Keep the mix cool for 10 minutes. Then bring to the boil, and keep boiling for 30 minutes.
Filter the solution while it is still hot, then cool and filtrate in an ice bath/refrigerator. Filter off the crystals which form, wash with ethanol and leave to dry.
A further crop of crystals can be obtained by adding to the filtrate about 0.5 g of charcoal and evaporating to half the volume, filtering and cooling as before.
The mustard-yellow crystals are slightly soluble in H2O.

The H2O2 is used to oxidise the Co from II+ to III+ .
I wonder whether one can do the same with the NO3- ion?!? or how about the ClO4- ion?

Like nitrogen?

Nick F - 29-6-2004 at 11:16

Diaminotetrazole silver nitrotetrazole, [Ag(CHN4NH2)2]CN4NO2 :D

Now that is one that would scare me... I'll have to try making it!! I have aminotetrazole, silver nitrate and sodium nitrotetrazole all in stock...

confused by Co[(NO2)3(NH3)3]

KABOOOM(pyrojustforfun) - 2-7-2004 at 12:57

is it a complex ion or a neutral coordination compound without coupling ions? if the former how the nitro ligands could form without being oxidized? if the later then why is it named Trinitrotriamine cobalt <b>(III)</b> ?
are you sure the ammonia solution is 0.88 M? maybe it's been 8.8 M ?&nbsp;&nbsp;25 ml 0.88 M means 0.025*0.88=0.022 mol NH<sub>3</sub> which means less than 1 mol NH<sub>3</sub> per 1 mol Co!:o.
anyway nitro and nitoso complexes are indeed cool especially that most energetic complexes we have discussed had a "fuel" cation and an "oxidizer" anion. but these cations can play the roll of an "oxidizer" or both oxidizer and fuel together (aka an energetic cation!) which makes use of energetic anions with moderate to perfect OB like azide, picrate, styphnate ... (as their coupling ion I mean)

Nick F - 2-7-2004 at 15:09

"0.88 ammonia" is an aqueous ammonia solution that has a density of 0.88g/mL, not 0.88 M.
I'm not sure what it's concentration is, but I assume it is saturated, because otherwise it would be a rather strange concentration to have as the standard. So just look up ammonia's solubility...

chemoleo - 5-7-2004 at 18:48

Yes, the info where I got it from says '0.880' ammonia, without a specification as to whether it's M or % or whatever. I guess Nick F is correct on this.
Kaboom, as to your question, I have no clear answer. I guess it is a complex ion of the Co[(NH3)3]3+ type. So the same thing shold work with KNO3 instead of KNO2, too. But this is guesswork :(
The information I posted is all I have, with no omissions.

PHILOU Zrealone - 6-7-2004 at 13:35

True that there is an ambivalence with nitro nitrito complexes; sometimes with cobalt you have nitro complexes but nitrito too...this would mean there is a solid Co-N bond in the first and a Co-O bond in the second.

I just wonder why they feel like using Co II and H2O2 instead of Co III imediately?
Also activated charcoal?

Many nitro complexes and nitroso are obtained by bubbling NO, NO2 or N2O4 though solutions of complexating metal salts.

PHILOU Zrealone - 6-7-2004 at 14:00

In principle the field of investigation is infinite....
oxoAnions:
ONO2(-)
ONO(-)
-NO2
-NO
OCl(-)
OClO(-)
OClO2(-)
OClO3(-)
(idem with bromine and iodine core)
-MnO4

reducing coordinators or ligands:
-C=O
-CN
CN(-)
-NC
N3(-)
CS3(2-)
Sx(2-)
S(2-)
P(3-)
-N=S
-S-CN
SCN (-)
-N=C=S
-O-N=C
-S-N=C
NH3
NH2OH
NH2NH2
NH2-CH2-CH2-NH2
orthoC6H4(NH2)2 (eventually nitro or polynitro)
NH2-CO-NH2
NH2-CO-CO-NH2
NH2-CO-NH-CO-NH2
O=CH-CH=O
O=CH2
NH2-CH2-CO2H and AA
NH2-CH=NH
NH2-CH=O
(NH2)2C=NH
(NH2)2C=S
NH2-CN
NH2-C(=NH)-NH-CN
NxSx
NC-CN
....

on metal core catalyst
with various valence/oxydation states:

Zn II
Fe II Fe III
Ni II Ni III
Co II Co III
Mn II Mn III Mn IV Mn V
Cu I Cu II
....
Unusual metals...
Ru III
Pt II
Au III
...

Also many complexes have ... chirality and isomers...thus different cristallinity, sensitivities, stabilities, colours, optical activity...and then explosive properties.

PH Z

PHILOU Zrealone - 6-7-2004 at 14:13

Here is a synthesis I have but I don't know form where since it is a long time ago and it is not obvious for the second one if it was Ni(NH3)6(NO3)3 or Co(NH3)3(NO3)3 because the writter mixed up Co and Ni; maybe is it acceptable for the two and here too HNO3 or H2O2 is used as an oxydiser of the Co II or Ni II into Co III or Ni III...

***********************
1. Synthesys of {Ni(NH3)6}(NO3)2.
Ni(NO3)2 + 6NH3 = {Ni(NH3)6}(NO3)2.
Calculated quantities of Ni(NO3)2 are mixed with the calculated quantity of 25% NH3. The mixture is stirred until the Ni(NO3)2 dissolves and then cooled 20-30 minutes with ice-water mix. The suspension of {Ni(NH3)6}(NO3)2 is then filtered, washed with alcohol and dried at 40-50 C.
(pretty much the same procedure I used thus but I didn't knew I had this)

2. Synthesys of {Ni(NH3)6}(NO3)3.
The synthesys is done by the reaction:
4Co(NO3)2 + 4NH4NO3 + 20 NH3 + O2 = 4{Ni(NH3)6}(NO3)3 + 2H2O
7g Co(NO3)2 is dissolved in 10 cm3 water.This is mixed with 8g NH4NO3 and 18g 25% NH3 and 1 g active charcoal. After this for 2,3 hours air is bubbled through the solution. Then the solution is tranfered into 250 cm beaker glass and 150 cm water with 2,3 ml conc HNO3 is added to it. This solution is heated on water bath for 30 minutes.Filter this to discard the carbon, and add 20 cm3 conc HNO3. Left it some days until orange chrystals({Ni(NH3)6}(NO3)3 ) form, filter and dry in 100 degrres C.
The oxidizing from air can be substituted with adding 3%H2O2. 1mol H2O2 to 2 mols Co(NO3)2 . H2O2 is added to the solution after the
NH4NO3.
**********************************
I guess we have to try both to be sure ;)

PHILOU Zrealone - 6-7-2004 at 14:19

***********************************
2-(5-cyanotetrazolato)pentaaminecobalt (III) perchlorate
 
The compound 2-(5-cyanotetrazolato)pentaaminecobalt(III) perchlorate (CP) is a Primary explosive compound, and has been utilized in
low-voltage detonators because it reliably undergoes
deflagration-to-detonation transition (DDT). One of the precursers in its preperation is cyanogen.
 
Another compound similar is:
 
cis-bis (5-nitrotetrazolato) tetraaminecobalt (III) perchlorate (or "BNCP";)
*************************************

Complex Persulphates

Axt - 23-9-2004 at 20:05

I found a reference to "Amminated cupric Persulphates", reference in full:

G. Morgan & F. Burstall, Cupric salts stabalised by ethylenediamine, Journal of the Chemical Society, (1926) Pg. 2026, London

It mentions that the ethylenediamine complex has explosive properties, but only mentions that the tetramine has been prepared and gives a reference, in full:

Cupric persulphate has not been isolated, but its tetramino- and tetrapyridine derivatives, [Cu,4 base]S2O8, have been prepared (Barbieri and Calzolari, Z. anorg. Chem., 1911, 71, 347).

One would think the tetraamine woud have better explosive qualities then the ethylenediamine, so I tried it.

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.

When dry the crystals of tetraminocopper (II) persulphate responded very energetically, a pinch of it explodes in a thump when exposed to a flame. Even though very sensitive to flame, in the drop test it wont fire at a height that will reliably fire PETN.

Ive added a movie of its ignition here - http://geocities.com/roguemovies7/

Looks promising, good yield, not very soluble, not hygroscopic, not impact sensitive and quite energetic. Hopefully it doesnt decompose.

EDIT: Igniting 0.2g resulted in a crack. Dont think you will have to much higher to get a true detonation.

[Edited on 24-9-2004 by Axt]

Axt - 24-9-2004 at 19:31

Disregard what I said about impact sensitivity before, as it was based on a one off test, today it's firing at a drop of 20-25cm (PETN was 40-45cm) leaving a green molten plastic-like residue.

<center><img src="http://www.sciencemadness.org/scipics/axt/greenresidue.jpg"></center>
<br><br>

[Edited on 9-12-2005 by Axt]

chemoleo - 27-9-2004 at 17:05

Wow, who'd have thought that! Complex persulphates.... I'd have assumed that the low OB would make them pretty useless!
It might be interesting to test this on additional metal ions (Ni in particular).

Did you try to see whether it is friction sensitive? How about larger amounts, do they leave a dent on a surface at all (trying to find out whether it's a true det.)

Edit: Merged this with existing thread to related complex salts.

Axt - 27-9-2004 at 17:56

I have tried with nickel ammonium sulphate (only nickel salt I have), which yielded a very small amount of precipitate looking just like the copper salt, but it decomposed on drying to inert black gunk. The next day the purple solution itself had gone black and left a black film stuck fast to the glass. H2SO4 removed it.

The copper salt also looks to be decomposing, turning light blue, and lighting some up today resulted in a smoldering green blob :( It has been sitting in the hot sun this whole time, so that cant help, but its probably too unstable to have any uses.

The ethylenediamine salt is said to decompose explosively, selected quotes from the reference I gave above "Extremely unstable ..... decomposed, leaving a blue residue ..... exploded when contained in cooled specimen tube ..... detonated on percussion" So that aint real useful either :(

Since Im now in this thread, I've found Ag(NH3)2MnO4 to be pretty crap. Will burn simular to "good" KNO3/sugar, and ignites within a few minutes exposure to sunlight. Maybe its only possible practical use is as a sun sensitive ignitor.

[Edited on 30-9-2004 by Axt]

chemoleo - 29-9-2004 at 07:46

Regarding the copper amine persulphate, how does it behave if it is stored in absolute ethanol? I am sure you could increase stability that way, and use it when desired.
Interesting, about the ethylenediamine. As I have some, might be interesting to test as the nitrate complex!

Marvin - 29-9-2004 at 13:29

Umm, run that theory by us once again chemleo, you want to store a peroxydisulphate in a liquid reducing agent to make it more stable?

chemoleo - 30-9-2004 at 02:19

Yes, I would.
Just like I'd store HMTD in absolute ethanol.
As long as not acid/base traces are present, I wouldn't see much of a problem. Admittedly one never knows, so I'd test it with a small amount first... You could also try acetone, if worried about oxidation.

PS who is 'chemleo'? :P

Marvin - 30-9-2004 at 23:46

My apologies for forgetting the 'o'.

From the sodium persulphate MSDS....

"Unstable. Strong oxidizer. Contact with combustible material may cause fire. Incompatible with combustible material, strong reducing agents, strong bases, alcohols, aluminium, magnesium. Protect from moisture. "

I'm not convinced I'd try to keep organic peroxides very long, but this strikes me as fractionally less insane if the alcohol is dry.

Axt - 1-10-2004 at 18:04

<a href="http://ww1.altlist.com/~58717/pulse.altlist.com/images/complexpersulphates.jpg">Heres</a> the reference from the journal on ethylenediamine "stabalised" persulphate, theres not much that hasn't already been said but its always better to see the original. Ive tried to form a complex using urea with no luck.

Below is tetramminocopper permanganate, the silver salt burns simularly, with dull flame and gouts of fluffy residue.

<center><img src="http://www.sciencemadness.org/scipics/axt/tetramminocopper-permanganate.jpg">
<a href="http://www.geocities.com/roguemovies7/index.html">Movie</a></center>
<br>

[Edited on 9-12-2005 by Axt]

Complex Cu - persulfates (with ammonia, hydroxylamine, ethylenediamine)

chemoleo - 10-10-2004 at 09:15

I had a go at various persulphates, and I have to say I am quite impressed with them (compared to the i.e. copper tetramine nitrate)

A copper sulphate solution was prepared (no stoichiometric quantities given as this was a testrun), and to this, a saturated ammoniumpersulphate solution was added. No significant colour change, except that the colour became lighter due to dilution. Note that ammonium, rather than Na persulphate was used.
The same thing was done vice versa, i.e. to copper sulpahte solution, either Hydroxylamine (base, H2NOH), ammonia NH3 or ethylendiamine NH2-C2H4-NH2 was added.

In either case, with an excess of the respective base, in case of
1) the hydroxylamine, the solution turned a deep turbid green (when it contained just CuSO4), with visible signs of fine precipitation. I am not sure at all what this is, the green stuff. As soon as the ammoniumpersulphate was added, lots of bubbled formed, and the greenness disappeared, leaving me with a blue solution again. I believe that the action of the persulphate is to oxidise the hydroxylamine, destroying both in its course and leaving me with CuSO4 solution once again. I don't think the hydroxylamine/persulphate system is a workable one.
2) the ammonia, , the solution turned an even deeper blue (slightly purple hint), and crystallisation ensued once it was put into an ice batch. I found it is actually quite soluble, so if you do the experiment work with minimum amounts of water. As axt said, it forms fine needle-like crystals.
3) the ethylenediamine, the solution turned a deep violet, and IMMEDIATELY forms masses of violet needle-crystals once again. The colour is distinctly purple, easily told apart from the ammonia complex from above. Also, the ethylenediamine persulphate complex is a lot less soluble - nearly all is crystallised, and the solution above is only slightly purple. Great stuff to work with, really easily isolated!
Edit: I just read the original article on the ethylenediammine complex, and I can't really confirm this. It seemed no more sensitive than the amine salt. The description of it being purple and sparsely soluble fits though. Yet again they state it decomposes to leave a blue residue, while mine leaves a brown snake (see below). Hmm. Are they colourblind? Also (see below) I didn't observe these explosive properties. Maybe I ought to try with their quantities, but I don't see why this would make a difference. Comments?

Below is a picture of the two on the filter paper, it was first washed with cold water, and then washed with ethanol (96%). No adverse reaction with the ethanol, as I said above I'd have been surprised if there had been (plus the article from Axt confirms this). The top pic is the ethylenediame complex, the bottom the ammonia one.
<center>

</center>

Stability: In solution/crystals in the original reaction mix (which still contains excess complexant), both solutions are fine (after two days storage), no visible colour change, bubbles etc. I think I can keep it there for a while, in the fridge. The dry powder, in case of the ethylenediamine complex turns green overnight, so definitely not stable. Also it doesn't burn anymore. The ammonia complex seemed fine.

Flammability, Friction etc: ABSOLUTELY WICKED STUFF! The ammonia complex burns very fast, instantaneous, with a small whoosh/pop, with a BEAUTIFUL GREEN FLAME, leaving a small green residue. The ethylenediamine complex burns nearly equally well (but definitely less rapidly), and leaves a snake of a brown substance that is sticky and soft. Quite funny to watch, the stuff burns and produces an extremely fast moving brown snake... anyway, Axt, it seems you were right in your prediction that the ethylenediamine complex is not as powerful. Both need yet to be tested under confinement, though.
Anyway, both burn well, and both don't seem particularly friction sensitive. In case of the ammonia complex, after deflag. it smells of ammonia (surprise).


To sum it all up:

DEFINITELY A MUST to anyone who is interested in these salts. So far this was the fastest/best of the copper variety I have played with, and incredibly easy to make. In greater amounts, I could definitely see this as a weak primary. THe only downside I can see is durability, so store in aqueous solution before use, then filter and wash with ethanol. Use right after its dry. Have fun :)



PS I wonder what other bases (aside from hydrazine) I could test. Ideas anyone?

[Edited on 10-10-2004 by chemoleo]

Axt - 11-10-2004 at 06:28

Nice :cool:

As I said before, I tried with urea, but no colour change nor precip, though I was using K persulphate so I had to use a lot more water then you would be using. (NH4)2S2O8 should be better and easier to find anyway (circuit board etchant), actually I just bought some today.

Try putting it in a tube and lauching a "snake" into the air :D, I never noticed a green flame from the ammonia complex, have to make it again just to see it. At least they have novelty value.

Maybe its zinc salt (if possible) should be next on the list to try. There is sweet few primaries that can be made easily from OTC chems, the persulphates may be one of them.

Axt - 18-10-2004 at 08:12

Talking of complex persulphates, what of the other peroxy complexes! its a whole branch that hasnt been touched on. check P185 vol 8 of PATR;

(NH3)5Co-O-O-Co(NH3)5(NO3)5

Co2H30N15O17 --> 2CoO + 15H2O + 12.5N2, nice balance! Though it lists no refs/synth nor properties but one can imagine its quite energetic!

It doesnt list the copper salts but it does list the tetramminozinc persulphate so yep, it can be done, "explodes on heating or impact".

Very interestingly, Ca persulphate itself is listed as "sensitive to shock, explodes violently", I assume syth is as easy as Ca nitrate + ammonium persulphate.

I've tried triamminochromium tetroxide before (starting with CrO3) but couldn't get a precip, should be easier to start with ammonium dichromate. PATR gives it good properties.

So, theres lots of interesting ones!

Axt - 18-10-2004 at 09:12

Quote:
Originally posted by Axt
12.5N2


7.5N2 :(

Mellor 9 (1939), 795 for K2O6V ... anyone? looks deadly.

mark - 30-10-2004 at 18:56

AXT

If you wouldn’t mind would you please tell me where you got your potassium persulphate? I have reagent grade catalogue however this stuff would be extremely expensive to buy at $130.00 Au for 500g. Thank you.

Ium - 30-10-2004 at 19:22

You will want Ammonium Persulfate not the Potassium salt. Solubility of Ammonium salt is many times higher according to references.

This should be enough to help you to find a source;).

Google Search

The_Davster - 30-10-2004 at 20:11

Well, I am in a good mood now so I might as well help him out a bit more...:P;)

Froogle

[Edited on 31-10-2004 by rogue chemist]

mark - 31-10-2004 at 18:54

I live Australia so froogle is basically useless. I have done numerous searches on google and found nothing about sources or common materials that contain this chemical. I always search before posting but a lot of times my not very extensive knowledge holds me back. I really wish to try the salt because I don’t want to play with the usual Organic peroxides, I like to experiment with unusual substances to help get a large knowledge of the world around me.

chemoleo - 31-10-2004 at 19:26

Well, come on, 4 posts on ammoniumpersulphate availability, where the Na-derivative is available by any electronics supply shop. It's not like it's massively tricky to obtain. Or are you going to discuss availability of ammonia in the next four posts? A single U2U would suffice instead.

If you want to discuss making persulphate, check other threads on persulphates, or create one.

If this kind of thread dilution was to happen in other threads as well, we would be discussing peripherals most of the time. So please try to avoid this.

KemiRockarFett - 2-11-2004 at 14:21

Thought about the persulfates that they may be explosive due to the bonding situation, so way should not ammoniumperoxidisulphate and ammoniumpersulphate have explosive properties ?

Reading in Federof:
Ammonium Peroxodisulfate Explodes violently on addition of Ag salts.

About the peroxidisulphate of Ca it says:
Calcium Peroxodisulfate, Sensitive to shock; explodes violently.

Peroxides are often fast primarys so I wonder where to read about initiating properties about these peroxi sulphates and other inorganic peroxi compounds.
Have somebody tried to detonate ammoniumperoxodisulphate ?

Axt - 30-11-2004 at 15:11

OK, just got some ethylenediamine, since chemoleo has reported that the persulphate precipitates easily from solution (relative to the amine) my thoughts were that the more energetic complexes may be easily isolated from an aqueous solution as well.

TACB is very sensitive, 2.5x more sensitive to impact then MF, but it can't be made in aqueous solutions. It wont precipitate nor can it be evaporated out without losing its NH3. So I set out to attempt Bis(ethylenediamine)copper (II) bromate. But alas, it doesnt precipitate, maybe I was being a bit optimistic especially with the S2O4 in solution. So I tried evaporating it out. Its been 40°C outside the last few days, so no problem getting it dry.

The extract explodes with a bang in nearly any amount. 1/4 matchhead worth will sound like a cap gun when ignited in the open, even though its half composed of the sulphates.

Na2SO4 seems to be the first thing to precipitate in ethanol, so this looks like the way to get the relatively pure bromate complex.

The bromate/sulphate extract explodes at a drop of 0-5cm (comparable with the peroxides), but doesnt seem sensitive to friction. Its been sitting in the sun for 3 days now with no decomposition.

There is a <a href="http://www.geocities.com/roguemovies7/index.html">movie</a>, but its only 0.2g ignited in open.

bisenbromate.jpg - 13kB

chemoleo - 30-11-2004 at 15:18

That's interesting, becuase I tested tetraamine /ethylenediamine periodate / copper complexes. As far as I remember, complexing worked well, but after a while I seemed to get fluffy precipates which looked more like hydroxides than anything else, as soon as I added ethanol(or acetone) to facilitate precipitation (the complex remained soluble). This fluffy precipitate has to be tested though, yet.
I guess I will try this with perchlorate at some point.

mark - 30-11-2004 at 22:50

Feeling a bad about my stupid question I am trying rectify the situation. To day recently tried to prepare calcium persulphate. 5 grams of calcium nitrate was added to a solution of 5 grams of ammonium persulphate in 40ml of hot water (70 degrees). The solution was then chilled in an ice bath until a fluffy suspension was noticed in the liquids this was filtered out. The filtrate is still drying. I’ll edit this with a movie link in a couple of hours to see if anything happens when I put a propane torch to it.

The stuff didn't deflagrate unless you just want a movie of a bottle cap burning. So no movie sorry.

[Edited on 1-12-2004 by mark]

PICT0004.JPG - 10kB

mark - 3-12-2004 at 03:27

I had success using the ammonium persulphate used the same method as Axt except using 30 ml of ammonia solution made by bubbling ammonia gas through water. The good thing a bout ammonium persulphate is I only needed 75ml of hot water to dissolve the ammonium persulphate other than the 200ml for the potassium persulphate. I got what looked like an excellent yield although I took some out of the filter and dried it on paper (most of the yield) and before it was fully dry most of decomposed into the same gunk as when you light a pile. However, the bit left on the filter was watched with mentholated sprits and showed no sign of decomposition. Also, lighting relatively large amounts amount of this explosive seemed very un-energetic, merely just burning instantaneously. I also confined a smallish amount in a old antenna tube (1 gram) and it busted the top open with a very light report.

Over rated I think.

Back to calcium persulphate. I had done the same procedure as last time except using 10 grams of each in 40 ml of hot water. Same precipitate except much denser and cloudier it still didn’t burn. So maybe another calcium source?

Edit by chemoleo: You do realise that Ca/NH4 persulphate aren't exactly complex salts? Besides this they are very unlikely to fall into the category 'primary'.

[Edited on 3-12-2004 by chemoleo]

t3sla_trooper - 23-12-2004 at 04:21

Excuse me for excavating this old thread, but has anyone actually tried using the tetramine copper persulphate as primary ?

mark - 23-12-2004 at 17:08

I have. I have pressed into several tubes (antenna, straws, etc) used as filler in a Polumna (Sp?) None of which gave a detonation or even a half decent report. I have also ignited whole batches (10g to 10g ratio) and got a small noise but defiantly no detonation. It’s a nice novelty but if your to close it splatters you with this little green residue that stings a lot. Have fun by the way wash your yield with ethanal other wise it has a habit of decomposing if it contains water.

t3sla_trooper - 25-12-2004 at 11:52

can you please make one more test with unpressed tetramine copper persulfate?

mark - 25-12-2004 at 17:55

Test complete. No detonation, or primary chracterisitcs noted upon ignition.

The_Rsert - 3-1-2005 at 15:02

Quote:
Originally posted by Axt
OK, just got some ethylenediamine, since chemoleo has reported that the persulphate precipitates easily from solution (relative to the amine) my thoughts were that the more energetic complexes may be easily isolated from an aqueous solution as well.

TACB is very sensitive, 2.5x more sensitive to impact then MF, but it can't be made in aqueous solutions. It wont precipitate nor can it be evaporated out without losing its NH3. So I set out to attempt Bis(ethylenediamine)copper (II) bromate. But alas, it doesnt precipitate, maybe I was being a bit optimistic especially with the S2O4 in solution. So I tried evaporating it out. Its been 40°C outside the last few days, so no problem getting it dry.

The extract explodes with a bang in nearly any amount. 1/4 matchhead worth will sound like a cap gun when ignited in the open, even though its half composed of the sulphates.

Na2SO4 seems to be the first thing to precipitate in ethanol, so this looks like the way to get the relatively pure bromate complex.

The bromate/sulphate extract explodes at a drop of 0-5cm (comparable with the peroxides), but doesnt seem sensitive to friction. Its been sitting in the sun for 3 days now with no decomposition.

There is a <a href="http://www.geocities.com/roguemovies7/index.html">movie</a>, but its only 0.2g ignited in open.


Axt, how have you prepared this stuff exactly?
Because it looks very powerful and interesting. I'm pleased to get an answer.

Axt - 3-1-2005 at 15:37

I dont have the amounts used anymore, I think I simply mixed the stoichiometric quantities to see if anything would precipitate, but nope.

So,

2M sodium bromate
2M ethylenediamine
1M copper sulphate pentahydrate

The_Rsert - 5-1-2005 at 17:39

Quote:
Originally posted by Axt
I dont have the amounts used anymore, I think I simply mixed the stoichiometric quantities to see if anything would precipitate, but nope.

So,

2M sodium bromate
2M ethylenediamine
1M copper sulphate pentahydrate


So, you have mixes satturated solutions of 2M SB with 2M EDA and 1M CS in water.
And than, you've evaporated the water and extracted the bromate complex from the sulphate complex with ethanol. Right?
Or?

Axt - 5-1-2005 at 20:07

Yes, but the ethanol should extract the bromate complex leaving the <i>sodium</i> sulphate, but this isn't confirmed. The movie you see is the raw mix of crap after evaporation.

K9 - 16-2-2005 at 22:36

What was the process for tetramminocopper permanganate? Would it just involve the addition of a potassium permanaganate solution or is there more? Thanx.

Axt - 17-2-2005 at 01:36

I had this written down so I think its what I did:

36g 25% ammonia solution was added to A warm solution of 16g CuSO4.5H2O in 150ml water. To this was added a solution of 20g KMnO4 in 270ml water. The mixture was then chilled to 10°C and the fine sludgy precipitate filtered out and dried.

I dont know about the purity of the product, but the silver salt is nearly insoluble, thus easily extracted and its properites are no better, so I dont think much more can be expected.

Trihydrazine Nickel (II) Nitrate

man_from_mystery_babylon - 17-7-2005 at 23:20

Hello,

I'm wondering, does anyone have experience with this compound?

There is a Wikipedia article about it here:

http://de.wikipedia.org/wiki/Nickelhydrazinnitrat

(It's in German, but you can easily translate it using the following).

http://babel.altavista.com/babelfish/

It seems to have many good properties, but I would like to know about long term stability in storage and compatability with metals, which the article doesn't say.

12AX7 - 18-7-2005 at 06:57

For convienience: http://babel.altavista.com/babelfish/trurl_pagecontent?lp=de...

Interesting...

[Edited on 7-18-2005 by 12AX7]

Rosco Bodine - 18-7-2005 at 07:43

See

GB821586

chemoleo - 18-7-2005 at 14:57

Merged with this thread.
Please note that nickel hydrazine nitrate has been discussed already in the first post of this thread.

There is a paper from the Journal Propellants, Explosives, Pyrotechnics that deals with it (Title: Evaluation of a New Primary Explosive: Nickel Hydrazine Nitrate (NHN) complex ), if someone's got access to this journal please upload the article here!

man_from_mystery_babylon - 18-7-2005 at 18:10

Thanks for the references.

I wonder about zinc vis-a-vis nickel. Has anyone any theoretical or experimental info? Seems to me it would be a little less toxic if nothing else.

Anyway, I've given up on TACC and TACN...I'm now looking for new bones to knaw on.

I got nowhere with TACN. I made one batch of successful TACC that detonated some picric acid, but it was not repeatable. Moreover, the TACC rapidly lost ammonia and became inert after sitting around for a few days.

Kinepak - 19-7-2005 at 10:39

Can anyone tell me something about tetramminecopper perchlorate? Because ive HClO4 i could try it. How sensitive is it and how strong? It would be great if you could tell me something. The tetraminecopper persulfate is also very interesting.

[Edited on 19-7-2005 by Kinepak]

TACP

man_from_mystery_babylon - 20-7-2005 at 20:27

You can find some information by following the link below (about 3/4 of the way down the page).

http://roguesci.org/theforum/showthread.php?t=161&page=5...

I would like to know if anyone has experimented with hexammine nickel perchlorate.

artem - 21-7-2005 at 13:17

Quote:
Originally posted by chemoleo
There is a paper from the Journal Propellants, Explosives, Pyrotechnics that deals with it (Title: Evaluation of a New Primary Explosive: Nickel Hydrazine Nitrate (NHN) complex ), if someone's got access to this journal please upload the article here!

Here:

Attachment: PEP97_06_317.djvu (36kB)
This file has been downloaded 2051 times


PEP articals required

Lambda - 21-7-2005 at 13:47

Artem, I think it will be very much appreciated, if you would be so kind as to uploade any PEP articals you may have to MadHatter's FTP. I don't want to burden you with any obligations, but maybe oneday when you have any spare time and some extra bandwidth available.....please !.

Detonation of Nickel Hydrazine Nitrate???

jlithen - 6-12-2005 at 01:47

I have made som Nickel hydrazine nitrate both by using Hydrazine sulphate and hydrazine solution. It is a nice substance that burns extremely fast. I also like the fact that it is easy to prepare if you just avoid breathing the hydrazine fumes and getting poisoned.

I have made many detonators containing about 0.8-1g of NHN but they don't detonate. I have made the detonators by rolling Al-foil around a pen.
I once stuffed a detonator into a wood log that I had drilled a hole into and it made a loud bang that shot the log into 5-6pieces. But I have still not managed to detonate any other explosive by means of NHN, I'd say it CAN NOT substitute Lead azide.

Anyone had any success?

I have been thinkin of using some sturdier tubing for the detos. but I don't like havin explosives in metallcontainers and then there is always the need for a hole for the fuse (if not using electrical ingnition)

Tetramine copper perchlorate

jlithen - 6-12-2005 at 02:02

Quote:
Originally posted by Kinepak
Can anyone tell me something about tetramminecopper perchlorate? Because ive HClO4 i could try it. How sensitive is it and how strong? It would be great if you could tell me something. The tetraminecopper persulfate is also very interesting.

[Edited on 19-7-2005 by Kinepak]


TACP is an easy to prepare compound. I have made it by dissolving coppersubcarbonate into perchloric acid untill no gas develops anymore. The solution can be very concentrated but it is hard to dry. It may be a good idea to dilute it slightly before the next stepp and deffinitely let it cool before adding ammonia.
To the Cu(ClO4)2 solution carefully add (in some excess) ammonia solution. And some of the TACP will precipitate. To precipitate the rest add about 5 times the volume of ethanol (92%EtOH/8%acetone has worked fine) Filter (maybe wash with EtOH) and dry!

The explosive formed is first a blue fine crystalline powder but turns violet when dried. It is very sensitive compared to most other complexes and I think it is poweful too.
Hitting it with the pestle in a mortar will make it go bang very easily, I have luckily not had any accidents though. Neither have I managed to make any working detos. woth it. A tube with 1g resulted in a mini-rocket:)

(I don't remember exactly but I think i have used something around 3ml HClO4 (70-72%), maybe about 5g Cusubcarb. and 10ml 25% NH3 and the added about 1/2 dl of ethanol. The yield is then around 5grams.)

artem - 6-12-2005 at 08:24

Quote:
Originally posted by jlithen
I once stuffed a detonator into a wood log that I had drilled a hole into and it made a loud bang that shot the log into 5-6pieces. But I have still not managed to detonate any other explosive by means of NHN, I'd say it CAN NOT substitute Lead azide.


I think, there is no "ideal" primer. More safety - hard to initiate. Many complexes are of high safety, but very often, without appropriate confinement and initial impulse they tend to deflagration or low-velocity detonation (for NHN, see, for example, PATR H199). Probably, particle size also play role.

jpsmith123 - 9-12-2005 at 16:58

Hello jilithen,

Can I ask, how did you prepare NHN from hydrazine sulfate?

BTW, with regard to its use in detonators, here is some relevant information from PATR 2700, p H200:

"The possibility of using Ni nitrohydrazinate
in commercial detonators was investigated
by loading Cu caps of 5mm diam with 2.5g of
Ni complex and trying to detonate them by
means of a fuse, or an electric igniter. No ‘
detonations were produced unless the substance
was primed by ca 1.5g of Black Powder.
In attempts to increase the detonability of
Ni hydrazinate, it was mixed with equal parts
of an easily ignitable initiating substance, such
as Pb- styphnate or Pb- picrate, and then ignited.
The best that could be obtained was a deflagration
but no detonation. Mixtures of the Ni
complex with RDX deflagrated and only in
one case detonated (Ref 3)."

Regards,
Joe

Quote:
Originally posted by jlithen
I have made som Nickel hydrazine nitrate both by using Hydrazine sulphate and hydrazine solution. It is a nice substance that burns extremely fast. I also like the fact that it is easy to prepare if you just avoid breathing the hydrazine fumes and getting poisoned.

I have made many detonators containing about 0.8-1g of NHN but they don't detonate. I have made the detonators by rolling Al-foil around a pen.
I once stuffed a detonator into a wood log that I had drilled a hole into and it made a loud bang that shot the log into 5-6pieces. But I have still not managed to detonate any other explosive by means of NHN, I'd say it CAN NOT substitute Lead azide.

Anyone had any success?

I have been thinkin of using some sturdier tubing for the detos. but I don't like havin explosives in metallcontainers and then there is always the need for a hole for the fuse (if not using electrical ingnition)

Rosco Bodine - 9-12-2005 at 21:35

There may be critical diameter >7mm and
a critical mass > 1.5 grams with strong confinement
for the DDT to high order detonation to occur
with samples of the complex which are not mixed
with other primaries having better self-accelleration .
A similar problem exists for lead styphnate ,
by itself it can take several grams to reach the
velocity needed for a detonator , unless a third
of the styphnate is replaced with something much
more rapid in small quantities , like lead azide .

The attached patent also mentions that copper and
perhaps other metal salts of other oxidizing acids besides nitric , can form explosive complexes not only with hydrazine ,
but also with semicarbazide , and " oxiamines " ?

There are some other possibilities for experiments with
complexes . It would be my guess that cobalt and zinc
would also possibly form such complexes .

Attachment: GB821586 Nickel Hydrazine Nitrate Complex Detonators.pdf (253kB)
This file has been downloaded 1971 times


jlithen - 11-12-2005 at 11:35

Hi joe!

I made NHN by dissolving about 50 grams of Hydrazinesulfate and 1xx grams of Ba(OH)2*8H2O in water (stochiometric ratio, can't remember exact ammounts) and then vacum filtering it for about 2h...to get the water sol. which contained about 4% H4N2... to this I adder ethanol and then the solution of Ni(NO3)2...

PHILOU Zrealone - 12-12-2005 at 11:05

As mentionned in the first post...Ni(NH2-NH2)3(NO3)2 might be mixed with Ag2C2.xHNO3

The original idea came to my mind because I had the info...that THNiN complex was better than mercury fulminate on many points but that it suffers from a lack of detonation propagation reliability. So I had the idea to mix 1/3 to 1/2 of the silver acetylide nitric acid complex to it and it was a succes...With 5g of the 2/1 mix I did detonate 70 g of hydrazine nitrate in a pipe bomb (5mm wall thickness) detonator was made of copper 4 cm long and 5 mm diameter (wall thickness was 1.5 mm)...

The THNiN was made by the use of 80% NH2-NH2 (100% NH2-NH3OH) dissolved in 97% ethanol and with green solid nickel (II) nitrate saturated in ethanol 97%.
The complexation produces a lot of heat beause of the concomitant precipitation...matter contraction always heats up!

Attempt with Cobalt delivered the same way a compound of comparable properties...Beautiful orange-brown precipitate.

After a few attempts I isolated a copper salt but it is unstable and most batches had turned into a black lump with N2 evolution...I stil had the chance to get a mittiged reaction wich was a mix of two compounds a black one (certainly colloidal copper) and a trukoise blue precipitate...upon drying on the filter (hopefully in tiny quantity)...filter had burst into flame...but a part of the truquoise precipitate was dry and stil intact...I had the ability to test it and it made a beautiful blue flash upon contact with a flame...why it remained intact after the filter had burned is a mystery...hereby I confirm that the copper is quite hazardous and an unpredictible compound (or a mix of compounds)...

Based on a experienced incident I suspect hydrazine nitrate to be able to react with copper to deliver the unstable truquoise compound...
NH2-NH3NO3 + Cu --> NOx + N2H4 + CuO + Cu(OH)2 + Cu(NO3)2... --> Cu(NH2-NH2)4(NO3)2

Warning about NH4NO3 with Cu powder must thus be taken seriously in the case of Hydrazine nitrate.
And even more with perchlorate...Ni(NH2-NH2)4(ClO4)2 is indeed said to be shocksensitive even if dissolved in water...

NH2-NH3ClO4 is rather fun stuf and isn't too sensitive to heat...catches the moisture from the air...much more than NH...
And because of its properties better keep it away from complexing metals...

[Edited on 12-12-2005 by chemoleo] - removed quote/unedited original.

[Edited on 12-12-2005 by chemoleo]

silver salts

Axt - 14-12-2005 at 23:13

I've tried to form some silver salts, the only success was ethylenediaminesilver (I) bromate. Which detonates in very small quantities when ignited. It also seems uneffected by sunlight.

It was made by precipitating silver bromate (very insoluble ~0.2g/100ml) by combining solutions of AgNO3/NaBrO3. Filtering, washing and drying. 5ml distilled water was added to 3g AgBrO3 then 0.8g ethylenediamine which took the AgBrO3 into solution. This was then poured into a tray and left overnight where it formed chunky crystals of Ag(C2H8N2)BrO3.

If 2mol ammonia was used instead of 1mol ethylenediamine it also went into solution and formed feathery crystals on evaporation, but they had very feeble explosive properties, melting and sometimes going "puff", perhaps it loses NH3 on drying.

I also tried AgClO2 instead of AgBrO3, but it also forms a very soluble complex with NH3, on evaporation it started looking suspiciously like fulminating silver so it was disposed of it. Never tried ethylenediamine/AgClO2.

<center><img src="http://www.sciencemadness.org/scipics/axt/silver-bromate-complexes.jpg">
Ag(C2H8N2)BrO3 on left, Ag(NH3)2BrO3 on right.</center>

Regarding permanganate complexes (Ag(NH3)2MnO4 ignited in sunlight) The Cu(NH3)4(MnO4)2 complex that I posted before is improved on in the attached reference, it mentions that it must be combined and precipitated at low temperatures to avoid decomposition to NH4MnO4 & MnO2.

Attachment: tetraaminecopper (II) permanganate.pdf (129kB)
This file has been downloaded 5645 times


pihop - 15-12-2005 at 06:33

Quote:
Originally posted by Ium
You will want Ammonium Persulfate not the Potassium salt. Solubility of Ammonium salt is many times higher according to references.


But would it work with potassium or sodium Persulphate?

I'm woundering because it's kind of hard finding a reasonable price on ammoniumpersulphate here in Sweden.
Ammonium is 50USD per kilo (shipping included) while Sodium is 9USD per kilo and is widely available.

PHILOU Zrealone - 16-12-2005 at 16:53

Out of the tread about picrates

I have made a mix of Ni(NH2-NH2)3(NO3)2 (usually pale lilas-pink) coprecipitate with NH2-NH3O-C6H2(NO2)3 (hydrazine picrate-pale yellow).....the original pink complex had turned that way pale brown.
In the mix probably Ni picrate, Hydrazine picrate and nickel trihydrazine dinitrate complex...properties not very wel studied owing to the lack of made material (a few mg)...burns fiercely but difference with the original nickel nitrate hydrazinate not noticeable at that quantity...
I'll certainly come back on that study since I have plenty of Ni(NO3)2 at home, about 300g TNP, and about a kilogram of hydrazine sulfate...
And then I'll try to set a testing up to compare:
1)Ni(NH2-NH2)3(NO3)2 (pink)
2)Ni(OC6H2(NO2)3)2 (?colour?)
3)(Ni(NH2-NH2)3(NO2)3)x.(NH2-NH2-O-C6H2(NO2)3)y.(Ni(OC6H2(NO2)3)2)z (pale brown)

The idea of the mix came to the fact I discovered hydrazine picrate to precipitate upon the mixing of saturated ethanolic solutions of hydrazine monohydrate and saturated ethanolic solution of picric acid...I decided to make an hybrid of the usual proces of the pink complex by mixxing three saturated solutions from which I had to get 2 or 3 coprecipitates...

Hydrazine picrate has proven to be very strange stuf...said to be less sensitive than the ammonium salt in litterature...while making a confinement test in aluminium foil in a flame...it puffed and smoked yellow :o without burning...looks like it sublimates...

[Edited on 17-12-2005 by PHILOU Zrealone]

PHILOU Zrealone - 16-12-2005 at 17:42

Axt,
I think you used not enough amine...silver is a tetracoordinating metal core...Thus Ag(NH3)4BrO3 and Ag(EDA)2BrO3
Because of its single oxoanion Ag is a poor choice vs other metals

**********************************
I have an idea...what if we all gather here all the interesting complexating and precipitation ability we can find about metals...
The aim would be to have idea of potent combination of precipitate that would allow coprecipitation, cocristallisation or cocomplexation of mixed energy fuels (CN, SCN, C2O4,NH3, N2H4, ....) and oxydisers (BrO3, IO3,....) of potentially interesting metals....meaning thus the mixing on a molecular level of oxydisers and fuel on catalytic core or vicinity :):):):)

As the field of investigation is nearly infinite...it would provide a good starting material for testings...:cool::cool::cool:


My complexation tables lists:
Co(NH3)6(2+) Kco= 1.3*10-5
Ag(CN)2(-) Kco1= 4*10-6 Kco2= 1*10-20
Cd(NH3)6(2+) Kco= 1.9*10-7
Ag(NH3)4(+) Kco= 5.9*10-8
Ni(NH3)6(2+) Kco= 2*10-9
Zn(NH3)4(2+) Kco= 2.6*10-10
Cu(NH3)4(2+) Kco= 7.1*10-14
Cd(CN)4(2-) Kco= 7.8*10-18
Fe(CN)6(4-) Kco= 1*10-24
Cu(CN)3(2-) Kco= 5*10-28
Fe(CN)6(3-) Kco= 1*10-31
Co(NH3)6(3+) Kco= 1*10-33
Hg(CN)4(2-) Kco= 4*10-42

My precipitations tables lists:
Co(IO3)2 Ks= 1.21*10-2
Pb(SCN)2 Ks= 2.11*10-5
Ca(IO3)2 Ks= 6.47*10-6
Zn(IO3)2 Ks= 4.29*10-6
Mn(IO3)2 Ks= 4.37*10-7
AgIO3 Ks= 3.17*10-8
Ba(IO3)2 Ks= 4.01*10-9
CaC2O4 Ks= 2.34*10-9
PbC2O4 Ks= 8.51*10-10
CuC2O4 Ks= 4.43*10-10
AgSCN Ks= 1.03*10-12
Pb(IO3)2 Ks= 3.68*10-13
CuSCN Ks= 1.77*10-13

5-HYDRAZINOTETRAZOLE-MERCURY (II) PERCHLORATE [Hg(CH4N6)](ClO4)2

jpsmith123 - 17-12-2005 at 16:36

Just in case anyone is interested, I came across a Russian patent regarding the preparation of this compound, apparently for use as a primary. The abstract is in English, but unfortunately the rest of it is in Russian.

Abstract of RU2225840

FIELD: inorganic chemistry, chemical technology. SUBSTANCE: invention relates, in particular, to methods for preparing mercury (II) compounds used as initiating explosive substance, in film charges for devices generating flat impact waves and others. Invention provides preparing 5-hydrazinotetrazole-mercury (II) perchlorate with the yield of the end product 50%, not less. Method for preparing involves mixing mercury (II) compounds as mercury (II) salt or mercury (II) oxide with 5-hydrazonotetrazole or its salt in 5-70% perchloric acid solution at temperature 10-70 C in the mole ratio 5-hydrazinotetrazole or its salt : mercury (II) compound = (0.8-2.0):1. Precipitate of 5-hydrazinotetrazole- mercury (II) perchlorate is filtered off, washed with water and alcohol and dried. Mercury (II) perchlorate is used as a mercury (II) salt. EFFECT: improved preparing method. 2 cl, 3 ex

Axt - 19-12-2005 at 04:42

Quote:
Originally posted by Rosco Bodine
and " oxiamines " ?


Oxiamines would be the somewhat energetic compounds R-O-NH2, I guess you could include hydroxylamine in that group.

Quote:
Originally posted by PHILOU Zrealone
Axt,
I think you used not enough amine...silver is a tetracoordinating metal core...Thus Ag(NH3)4BrO3 and Ag(EDA)2BrO3 Because of its single oxoanion Ag is a poor choice vs other metals.


Google argues against "tetraamminesilver" in favour of "diamminesilver" by a 1:149 vote :cool:

And this, regarding the nitrate:

<i>Diamminesilver nitrate and (diammine-d6)silver nitrate were formed by dissolving silver nitrate in concentrated ammonium hydroxide (or ND4OD) at room temperature. The white crystalline products were separated by direct drying in a desiccator containing molecular sieves. Anal. Calcd for Ag(NH3)2NO3: Ag, 52.9; NH3, 16.7. Found: Ag, 53.0; NH3, 17.0. Calcd for Ag(ND3)2NO3: Ag, 51.4; ND3, 19.0. Found: Ag, 51.0; ND3, 18.7. These compounds are quite stable if stored in subdued light in a dry atmosphere. They lose ammonia rapidly if heated to about 70".</i> Inorg. Chem.; 1969; 8(4); 802-807.

Heres a <a href="http://ww1.webtop100.net/~62552/xmovies.webtop100.net/banners/ethylenediaminesilver-bromate.mpg">movie</a> of a crystal of Ag(C2H8N2)BrO3 being ignited.

On paper Ag(N2H4)ClO2 would be hard to beat, AgClO2 being explosive in itself, a high energy fuel and perfect OB. Though in practice .... dunno.

PHILOU Zrealone - 19-12-2005 at 06:03

AgNO2 + NH2-NH2 --> AgN3(s) + 3 H2O
Interesting :)

AgNO3 + NH2-NH2 --> Ag(s) + N2 + H2O
Sadly this is unstable :(

Axt,
In place Ag(N2H4)ClO2...which is interesting to test of course...I would suggest Ag(N2H4)2ClO4...also perfect OB ...

About diamino silver nitrate...
:o:o:o
I find really stange that no mirror Ag or Ag3N,Ag2NH and AgNH2 did form...do you see any explanation to this phenomenon?
AgONO2 + NH4OH --> NH4NO3 + AgOH/Ag2O -NH4OH-> AgxNyHz + Ag(s).
NH4OH conc is 33% by weight NH3 in water or so...
I could understand the reaction to succeed with dry liquid NH3 flowing on dry AgNO3 ... but with NH4OH???...They seem to mean that water is a problem for the stability...
Is there something said about this silver mirror problem or risk of explosion?

Axt - 20-12-2005 at 02:19

You'll need a reducing agent to get silvering, I silvered a beaker trying to precipitate the chlorite with ethanol. The fulminating silvers would need heating or extended periods to form. There no mention of explosive properties for Ag(NH3)2NO3 in the article, though no doubt it is energetic.

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

[Edited on 1-11-2007 by Axt]

PHILOU Zrealone - 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

pihop - 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.

Microtek - 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.

PHILOU Zrealone - 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...

Axt - 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.

pihop - 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]

Rosco Bodine - 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

pyrochem - 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]

Mephisto - 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.

&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;

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

New "green" nitrotetrazole-based primaries

pdb - 2-4-2006 at 06:37

This the abstract:

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

Would anyone have access to the full article ?

The_Davster - 2-4-2006 at 09:23

Was definatly an interesting read!

Attachment: green primarys Environmentall friendlyenergetic complexes.pdf (473kB)
This file has been downloaded 2176 times


Chris The Great - 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]

Nice detos.

jlithen - 3-5-2006 at 08:57

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!

Iron-anion based new primary

pdb - 24-10-2006 at 13:44

See the following link:

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

Any idea of what this stuff could be ?

Axt - 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.

pdb - 25-10-2006 at 06:12

You are obviously right, my dear Sherlock ! ;)

I just have forgotten my previous request... Alzheimer, so soon ?!

Rosco Bodine - 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)
This file has been downloaded 1142 times


pdb - 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.

quicksilver - 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. . .

Rosco Bodine - 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]

Boomer - 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!

Rosco Bodine - 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

The_Davster - 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)
This file has been downloaded 2474 times


Rosco Bodine - 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 .

The_Davster - 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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