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Zelot
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| Quote: | Originally posted by Taoiseach
*snip*
Make the perchlorate complex - it keeps well for years and isn't moisture sensitive. Or go for the nickel chlorate, it keeps perfectly well too and
due to its very low solubilty it precipates even from dilute solution.
Btw. the corresponding zinc ammine is useless as well (hygroscopic and decomposes within weeks). |
If I had some perchlorate, I probably would make TACP. What do you mean by "the corresponding zinc ammine"?
So... what did you do over the weekend?
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woelen
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A zinc ammine is a zinc ammonia complex. IIRC [Zn(NH3)2](2+), but I am not really sure about the number of ammonia molecules in the complex.
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Zelot
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I think I'll try TANC, or maybe TANN. Nickel is less expensive than copper. Does anyone know something about Tetra Amine Nickel Nitrate? It seems easy
to synthesize, just add metallic nickel to an ammonium nitrate solution...
So... what did you do over the weekend?
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Taoiseach
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I think there are 4 molecules of NH3 in the zinc ammine. The persulfate, chlorate and perchlorate are explosive but none of them is stable AFAIK. The
persulfates are especially dangerous.
Hexamminenickel(II)nitrate is indeed easy to prepare. Unlike the corresponding copper complex it is stable in air. Bubble NH3 trough a hot saturated
solution of nickel nitrate, then cool down in the fridge. Or put nickel wire into a hot AN solution, bubble air through it until all dissolves. Then
add ammonia and cool down below 0°C. Reactions going on should be:
2Ni + O2 --> 2NiO
NiO + H2O --> Ni(OH)2
Ni(OH)2 + 2NH4NO3 --> Ni(NO3)2 + 2NH3 + 2H2O
(I dont know if nickel is able to reduce NO3(-) under these conditions but I doubt it. I think air will be needed to oxidize Ni to Ni(2+))
So per mole of Ni you get only 2 moles of NH3. You need to add ammonia to provide the 4 missing ligands to form [Ni(NH3)6](2+). Use in large excess
because quite some NH3 will escape when you heat the solution.
The complex forms nice & dry non-hygroscopic blue crystals. It is very insensitive, comparable to TACN. I doubt it can be detonated without lead
azide or a comparable primary.
Its possible to grow BEAUTIFUL crystals of it tough so its definetely worth making!! 
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Zelot
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I have done some thinking, and want to make some nickel chlorate. The only problem is, where to get nickel and how to get it into solution. Are US
nickels made of nickel, or are they an alloy?
So... what did you do over the weekend?
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not_important
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There is at least one thread on this. US 5 cent coins are 3/4 copper, 1/4 nickel. That alloy can be used as a source of nickel, as can be nichrome
and other heatring/resistive wire.
Often pottery supply houses sell nickel compounds; carbonate, oxide, and sulfate are the common ones.
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Formatik
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| Quote: | Originally posted by Zelot
I have done some thinking, and want to make some nickel chlorate. |
Hexamminenickel (II) chlorate makes a poor initiator according to Ephraim and Jahnsen (didn't ignite tetryl). Under a flame it decomposes weakly, and
in a test tube ignited with a fuse it burns slowly. In a capsule pressed to 80 kg/cm it would not ignite. It detonated partially when a non-initiating
ignitor was added to it in order to make it ignite, but it did not cause a significant indentation on a lead plate.
The [Ni(NH3)6](ClO3)2 is a blue solid (d=1.52), averg. expl. temp: 210 deg., shock sensitivity: 25 cm with 2 kg weight (47 cm with 1 kg weight).
Trauzl: 68% of TNT. The azide and bromate variants are noted to lose NH3 at
room temperature.
Tetramminezinc (II) chlorate precipitates from the preparation solution only if it is saturated entierly with ammonia and the solution kept cool. They
are colorless crystals that resolubilize if let stand in the mother liquor. In its behavior it is said to be similar to the copper and nickel salts.
Tetramminezinc (II) chlorate is 79%, and the perchlorate is 70% of TNT in the trauzl test. There is also the hexammine coordination compounds of zinc,
Zn(ClO3)2.6NH3 will form from the tetrammine although the tetrammine does not absorb any more NH3 at room temperature, in the cold it does. The
tetrammine chlorate coordination compound is sensitive (2kg at 15 cm).
In general E & J note about ammonia ammine halogenates:
1)Decomposition temperature of the bromates is not much lower than the chlorates, but the shock sensitivity is much greater (e.g. 2 cm with 2kg for
Cu- or Zn(BrO3)2.4NH3 compared to 15 cm for both the respective chlorates of those metals)
2) Ammine iodates: (of Cu, Ni, Zn, Cd) do not explode when heated in air or impacted, but from 20 cm height (2kg) there is seen some decomposition
(localized)
3) Their prospects as initiators are gloomy. Especially since the moisture in the air replaces a NH3 molecule with a H2O. For the speed of this you
have to see more of their work on this.
Not only with ammonia, but with many other nitrogenous bases are complexes formed e.g. monoamines (allylamine, ethanolamine, methylamine, etc),
ethylenediamine, hydrazine, etc. All can be expected to show differing stabilities and sensitivity, like the copper chlorate hydrazine compound
Cu(ClO3)2.2N2H4, which is a colorless salt that detonates upon drying in air after about 4 minutes, and at 35°C it takes a few seconds.
Sources: PATR A275-86. And Ephraim and Jahnsen, Ber., 48. pgs. 41-56. Gmelin "Cu" p. 335.
| Quote: | | The only problem is, where to get nickel and how to get it into solution. Are US nickels made of nickel, or are they an alloy?
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If you have any, older Canadian nickel coins are pure nickel.
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Phantom
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First of all it is not a primary explosive. It is very easy to make. You'll need only NH3, NH4NO3 and CuO. It has about 3600m/s
[Edited on 21-8-2011 by Phantom]
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plante1999
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Does someone have succefully made tacc? I have tried to make some by boiling 25ml methanol/ 2.5g CuSO4/ 1.5g KClO3 and than filter, I get neon green
sol. of copper chlorate and than I passed ammonia gass trougth the sol. When it started to smell stronghly ammonia I stopped to pass ammonia and I
filtered, I think I got copper hydroxide since the salt did not disolve in water/methanol. I dried the salt and heated it with a torch, It seam to
release ammonia when heated but it is not energetic at all. (my objestive is not to to explode something , simply to explore the proprety of
coordination complex.
Thanks!
I never asked for this.
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Formatik
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TACC is easily destroyed by water and the air atmosphere. Everything in its preparation is at best anhydrous, and then it protected form the air. The
nitrate salt is easier to make and doesn't degrade as easily.
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quicksilver
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I had experimented with chlorate salts. Tetra-amine-copper-chlorate....The amine often can be resolved using strong ammonia solution (simple source),
yet all the warnings of copper and chlorate should be thoroughly understood. It provides an explosive when confined. Yet is deliquescent and must be
stored in a sealed container. Recipe for disaster.... (see Formatik 's comment) Results are undefined (broken platelet shape) brittle crystal
material that requires continuous desiccant.
Does it provide a strong initiation as used in a primary explosive? Generally [and in practical terms], no. The requirements for maintaining an
anhydrous form would be a challenge at best and the weight to initiate a sensitive secondary such as PETN are generally unstudied. I believe that the
Journal P.E.P. may have some wider-range metal chlorate salt studies, perhaps lumped together with chlorate initiation (I am not sure: a Search would
be in order). However it would take some weight (must likely more than a gram) and would not propagate in a compressed manner; so there is a volume
issue.
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