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[*] posted on 18-6-2004 at 13:17
TeACN


Several days ago I tried to detonate about 5g TeACN - [Cu(NH3)4](NO3)2 but it didn't explode. At first I trried to light it but this was almost impossible. Then I began to hit it with a hammer but it didn't explode again! I don't know what was wrong. I made the TeACN by mixing 20g CuO with 50g NH4NO3 and then added 100ml 10% NH3 solution. I left the mixture for 4 or 5 days (I was busy). The product was blue.
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[*] posted on 18-6-2004 at 15:03


Did you obtain the product by filtering out the precipitate formed? If you did you most likely filtered out Cu(OH)2, the TACN is more soluble in water than copper hydroxide.
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[*] posted on 19-6-2004 at 12:40


yes. I filtered the solution. How to obtain the TeACN from итс ватер солутион ?
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[*] posted on 19-6-2004 at 12:42


..and for those of us here who don't know the cyrillic alphabet nor russian...?



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[*] posted on 19-6-2004 at 12:51


To err is human. :)
yes. I filtered the solution. How to obtain the TeACN from its water solution?
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[*] posted on 19-6-2004 at 12:53


According to dictionary.com итс ватер солутион means in english "its the ring spinning frame of solution" So how to obtain the TACN from its the ring spinning frame of solution?...must be a bad translator:(. Im going to intrepret this as how to obtain the TACN from the solution. First filter your mixture after doing what you said in your first post. What stays in the filter is NOT your TACN. What is in the filter is copper hydroxide. Your TACN is in the liquid that passed through the filter. To isolate it just evaporate.
Also, call it TACN not TeACN, you get better search results this way.

Edit. YAY, I intrepreted it right

[Edited on 19-6-2004 by rogue chemist]
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[*] posted on 21-6-2004 at 14:25


i think the best thing to do would be to reduce it by evporation, cool it to 0C and add some very cold EtOH, and filter that.

thats what i would do, anyways




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mad.gif posted on 23-6-2004 at 03:04


This subject has been extensively developped in the beginning of this forum.
Also mentionned Ni and Co nitrato amino complexes.

The isolation from the watery saturated solution might be done after partial evaporation and addition of excess NH3.

Usually my procedure calls for dry Ethanol or better methanol saturated with Cu(NO3)2, Ni(NO3)2 or Co(NO3)2 then introduce excess concentrated NH3...It will cristallise out..if it doesn't add a little ether.
The proof it is a new compound is that it precipitates in ethanol/methanol what doesn't precipitate the original nitrate..you can dissolve quite a lot in surprisingly.

Also it isn't the best thing to do since those are relatively unsensitive nor effective.
Better play with perchlorates!
Maybe a mix of perchlorate/nitrate would be worth a try.

As soon as I have my appartement and lab operational again...i'll persue my experiments on this.




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[*] posted on 23-6-2004 at 22:13


For some reason I seem very attached to TACN. I have only ever experimented with small amounts but I seem drawn to it. I know, as Philou stated, that they are not too usefull, but still I have an inherrant belief that they are cool. I have tried many different routes with varying success' but I am still determined to get it "right".
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[*] posted on 13-8-2004 at 10:28


Quote:
Originally posted by rogue chemist
Did you obtain the product by filtering out the precipitate formed? If you did you most likely filtered out Cu(OH)2, the TACN is more soluble in water than copper hydroxide.


What colour should the Cu(OH)2 be? I have also attempted to make TACN, and after mixing the Cu(NO3)2 solution with NH3OH I got a dark blue precipitate, which I filtered off.

Now I have saved both the precipitate and the filtered solution, because I have heard more than one story about which is the good stuff.
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[*] posted on 13-8-2004 at 10:37


Cu(OH)2 is a light blue ppt. An excess of ammonia soln. will make sure that all the copper hydroxide will turn to TeACN. I have carried out such a synthesis lately and obtained quite a large amount of TeACN, by cooling the solution to nearly 0 deg celcius before filtration.

The solution is simply a solution of the tetraamine copper (II) complex in water. For the ppt. to be highly explosive I suppose it mush be thoroughly dried previous to use. It does deflagrate to a certain extent even when quite wet.




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[*] posted on 14-8-2004 at 21:28


Quote:
Originally posted by Esplosivo
Cu(OH)2 is a light blue ppt. An excess of ammonia soln. will make sure that all the copper hydroxide will turn to TeACN. I have carried out such a synthesis lately and obtained quite a large amount of TeACN, by cooling the solution to nearly 0 deg celcius before filtration.

The solution is simply a solution of the tetraamine copper (II) complex in water. For the ppt. to be highly explosive I suppose it mush be thoroughly dried previous to use. It does deflagrate to a certain extent even when quite wet.


Do you mean that the dark blue crystals that remain after I've added the ammonia solution should also be filtered off and discarded, and what I want is what will be left after the filtered solution has evaporated?

I've saved both the solution and the dark blue crystals for now, since I've heard different points of view about which of them contains the TeACN...
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[*] posted on 15-8-2004 at 01:30


I think I might have explained myself wrongly. What I wanted to say is that the deep blue crystals you filtered off should be the TeACN. If the ppt was light blue instead it would have been Cu(OH)2 and more ammonia should have been added so to convert it into the TeACN. To increase the yield of TeACN I cooled the solution.

The solution itself does contain TeACN, but I don't know if it is worthit to boil the solution to get out more TACN.




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[*] posted on 15-8-2004 at 01:43


Quote:
Originally posted by Esplosivo
I think I might have explained myself wrongly. What I wanted to say is that the deep blue crystals you filtered off should be the TeACN. If the ppt was light blue instead it would have been Cu(OH)2 and more ammonia should have been added so to convert it into the TeACN. To increase the yield of TeACN I cooled the solution.

The solution itself does contain TeACN, but I don't know if it is worthit to boil the solution to get out more TACN.


Okay, then I got it right. Just need to let the deep blue crystals dry now then.

The crystals seem to burn, but very slow so I guess they need to be mixed with something in order go be used as an explosive.

[Edited on 15-8-2004 by Macgyver]
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[*] posted on 28-12-2004 at 07:18


Sorry for bouncing this thread again, but yesterday I made TeACN.
I used pure cupper and 70% HNO3 and made Cu(NO3)2.
Than I mixed this solution (blue) with NH4OH solution.
It made more crystals and turned deeper blue

[img]http://www.upload2.pyrozone.net/[Cu(NH3)4](NO3)2/filtering.JPG[/img]

now its drying.......

I know its not Cu(OH)2 because its blue and not green
But now whan it dried all night all the outside of this lump turned less blue and more green, so I think its deflagrate :-\

Is there any way I can check what I got?
It could be Cu(NO3)2 too I think.....
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[*] posted on 29-12-2004 at 18:11


Well you could sperate it by adding it to ethanol. CuNO3 is soluble in Ethanol and Tetra amine copper nitrate isn’t.

There is away to make it anhydrous I believe. We precipitate the CuNO3 and heat till anhydrous (white). Then dissolve in ethanol and bubble ammonia through it. Which should precipitate the anhydrous tetra amine Copper nitrate. I guess the yield could be washed with ethanol to make sure the copper nitrate does dissolve and then discarded.
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[*] posted on 30-12-2004 at 04:24


thx, but now I got another problam

I successfuly synthesis the TeACN
but its wet from water.....

whan i put in outside it dry and all the outside is turning Cu(NO3)2 green.......

its not hot in here so I dont know what it decomposed :-\
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[*] posted on 30-12-2004 at 05:34


Quote:
Originally posted by quest
whan i put in outside it dry and all the outside is turning Cu(NO3)2 green.......


Green is quite strange. IIRC the only Copper salt which is green in the solid state is the chloride. Copper nitrate is blue in colour, just like pure Copper sulfate.




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quest
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[*] posted on 30-12-2004 at 06:02


I found some picture in google with some metarial in the same color of the "green" I got:

click here

[Edited on 30-12-2004 by quest]
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[*] posted on 30-12-2004 at 18:34


Strange. Next batch wash it EtOH to get rid of the water and that should leave dry in a few hours at most. Usally 10 minutes for me to get a bone dry product.
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[*] posted on 12-5-2005 at 11:50
TACN


I made TACN thus: I liquified about 170g NH4NO3 in 320ml 25% ammonia, and then I dumped to it 250 g well puloverized CuSO4.5H2O. I waited about 5 hours and then I filtered it. I didnt poured to it any other liuids. I put it (it was like violet gel) on the "filtering" paper, in paper-lined paper box and placed it on radiator in bathroom:). (Before it I left it outside because it smelled terribly..ammonia...and after about two days I placed it tu our bathroom... and all the first day I hed our ventilator turned on....) After 5 days on radiator I had lumpy, but dry violet "powder". I grinded it in mortar to "real" powder...after it it was really fine violet powder. I hope that I helped you.

[Edited on 12-5-2005 by Unipetrol]

[Edited on 12-5-2005 by Unipetrol]




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[*] posted on 7-10-2005 at 10:26


Sorry that this thread is bumped again, but I think this is the best place for my little words...

I have questions about the previous synthesis. Although you indeed will get a tetrammine copper compound, how does it assure that the nitrate is obtained and not the sulfate? I think that a mix of both is obtained at best.

I have my own method:
Take CuO (from a ceramics supplier)
Dissolve this in as little as possible HNO3. Assure that a small amount of CuO remains undissolved. Heat a little to dissolve as much as possible of the CuO. This assures that no (or only a very small amount of) free HNO3 remains in the solution of copper nitrate.
Decant the blue liquid from the solid CuO.
Pour cold NH3 (25%) in the blue liquid. This causes formation of a light blue precipitate, but if more NH3 is added, the precipitate becomes deep blue/purple. The solution also becomes deep blue.
Now, a dark paste is obtained, with a deep blue liquid above it. There must be a strong smell of ammonia.
Let the dark blue precipitate get soaked with ammonia. This can be done by allowing the mix to stand for one or two days and occasionally stirring the paste and liquid.
Decant the liquid from the paste and spread the paste on a large glass surface. Do not use filter paper. It tends to dissolve the paper!
Let stuff dry for several days in a warm and dry room.
Do the final drying by blowing hot air over the powder (using a fohn, assuring that not all powder is blown away ;) ).

In this way I prepared approximately 2.5 grams of TACN. Here is a picture of approximately 1.5 grams I saved.

Now I have a few questions:
Is this how it should look like?
I can light it with difficulty. If I put a flame of a torch on it, then it first melts and then I get kind of 'poof' with a small cloud of black smoke. It does not really explode, it is more like nitrated cotton-wool, but with a less visible flame. Is this normal for TACN, or should it really explode?

Edit(woelen): Made link working again

[Edited on 10-3-19 by woelen]




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[*] posted on 7-10-2005 at 11:16


I'll say thats practically the same as my experiance with it. I've never found a definate answer, but the problem (from an energetic aspect) is going to be hydration. For more amusement try looking for complexes not prone to hydration, theres a more established thread here: http://www.sciencemadness.org/talk/viewthread.php?tid=1778

Right now I'm thinking Diaminesilver (I) bromate, Ag(NH<sub>3</sub>;)<sub>2</sub>BrO<sub>3</sub>, should be anhydrous, and quite insoluble, so should precipitate from AgNO3/NH4OH + NaBrO3. Though likely light sensitive sensitive :cool:

Oh, and if your nitrated cotton burns like that, it has serious issues :(

[Edited on 7-10-2005 by Axt]
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[*] posted on 7-10-2005 at 12:06


Quote:

I'll say thats practically the same as my experiance with it. I've never found a definate answer, but the problem (from an energetic aspect) is going to be hydration.

WIth 'hydration' you mean water, attached to the copper ion, instead of ammonia, or do you mean hygroscopic nature, in the sense that the compound is not really dry?

My stuff is perfectly dry. If I shake that container with the powder, then it does not stick at the glass walls and the powder is free flowing. So, I think it is really dry. Of course, water of crystallization or water, coordinated to the metal ion, still can be in the compound. In that case I expect something like

[Cu(NH3)4-x(H2O)x](NO3)2

where x > 0. This indeed would be less energetic, because the nitrate has less 'fuel'-NH3 in the same compound.

Quote:

Right now I'm thinking Diaminesilver (I) bromate, Ag(NH3)2BrO3, should be anhydrous, and quite insoluble, so should precipitate from AgNO3/NH4OH + NaBrO3.

How can I be sure that Ag(NH3)2(+) is precipitated with bromate and not simply Ag(+)? I once made AgBrO3. That is almost insoluble in water and can simply be precipitated. When mixed with e.g. magnesium, you get a very powerful mix, but this is something different than a compound, which is energetic on its own. Is the ion Ag(NH3)2(+) stable on storage in the solid state? Ammoniacal silver forms fulminating compounds in aqueous solutions, which are insanely sensitive and even a wrinkle on the surface of the liquid may set it off! How about the stability of the solid stuff?

Quote:

Oh, and if your nitrated cotton burns like that, it has serious issues :(

I think that my comparison with nitrated cotton wool was not very clear :) . The only thing I was comparing is the flame and the kind of noise produced. Luckily I only need a propane torch to ignite the cotton wool :D .




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[*] posted on 7-10-2005 at 12:49


Quote:
Originally posted by woelen
WIth 'hydration' you mean water, attached to the copper ion, instead of ammonia, or do you mean hygroscopic nature, in the sense that the compound is not really dry?

I dont think theres an aquo ligand, but as I said, I've seen no definate answer. Cu(NH3)4(NO3)2.xH2O would be my bet.
Quote:
How can I be sure that Ag(NH3)2(+) is precipitated with bromate and not simply Ag(+)?

Since they are both likely clear/white. Take some, walk out into the sun and see if it explodes :P Thats what I'd expect. I dont think you will have a problem distinguishing them!
Quote:
Ammoniacal silver forms fulminating compounds in aqueous solutions, which are insanely sensitive and even a wrinkle on the surface of the liquid may set it off! How about the stability of the solid stuff?

Only the dry precipitate is vehemently explosive, not the solution. It shouldn't form so easily in a non-heated solution, just dont leave it overnight.
Quote:
I think that my comparison with nitrated cotton wool was not very clear :) .

heh.. yes. Someones gota work on their analogies ;)

EDIT:
Quote:

<b>Copper (II) ammine Nitrates</b>
Several complexes of general formula, Cu(NO3)2. xNH3. yH2O, are listed in Ref 2, pp 179-82. Izzo (Ref 1, p214) lists the following blue signal light compn contg one of the complexes: K chlorate 53, “nitrato di rame ammonicale” 26, charcoal 16 & sulfur 5%

Re/s:
1) Izzo (1950), 214
2) Gmelin, Syst Nr 60, TIB, Lfg 1 (1958), pp 179-82

That doesnt indicate either way, only thay water is involved. the refrence from: <i>Gmelin-Krauts Handbuch der Anorganischen Chemie, Verlag Chemie, Berlin,8th ed (1928-1958)</i> would shed some light on it.

[Edited on 7-10-2005 by Axt]
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