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Author: Subject: Exotic Primaries - Complex Salts
Taoiseach
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[*] posted on 5-4-2008 at 03:27


Where did you hear about it? I also doubt it exists.

There seems to be an "zinc acetate-peroxide complex" tough:

http://www.freepatentsonline.com/4172841.html
http://www.freepatentsonline.com/5152996.html
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[*] posted on 7-4-2008 at 17:20


Yesterday I did electrolysis of an ammonium nitrate solution with copper electrodes in hopes of getting TACN. After an hour or two at ~5 volts and 1 amp, I filtered the solution and ended up with CuOH in the filter and a very deep blue-violet solution in the container. I assume this is either a tetraamine copper or tetraamine copper nitrate solution.

You add acetone to precipitate it, right? Flame tests will follow after precipitation.




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[*] posted on 8-4-2008 at 01:11


Quote:
Originally posted by Taoiseach
Where did you hear about it? I also doubt it exists.

There seems to be an "zinc acetate-peroxide complex" tough:

http://www.freepatentsonline.com/4172841.html
http://www.freepatentsonline.com/5152996.html


I don't remember where I heard about it.

The acetate complex seems interesting and easy to make. As far as I understand dissolve some zinc in acetic acid, remove the excess piece of Zn, and then add some H2O2 and heat it so the complex precipitates. Then just filter it, wash and let dry. I will try today and post the results.

Is there perhaps some similar copper complex?



[Edited on 8-4-2008 by Zinc]




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[*] posted on 9-4-2008 at 04:16


Unfortunately I wont be able to make the complex as I have trouble to make zinc acetate. My Zn doesn't want to dissolve in 80% acetic acid.



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[*] posted on 9-4-2008 at 23:47


Just make some Zn(OH)2 and react that with acetic acid to get your acetate.
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[*] posted on 10-4-2008 at 05:45


Don't you make Zn(OH)2 by reacting a zinc salt with ammonia?



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[*] posted on 10-4-2008 at 06:27


Check the solubility of zinc acetate (dihydrate), you need enough water to get all of it into solution. I think it's about 1 g/2 cc I think you are going to want to dilute the acetic acid a bit.

Also try touching a bit of platinum, gold, silver, or even nickel, iron, or copper to the zinc while it is in the acid.

Another thing you could try is to treat the zinc with a little HCl, to get it reacting, then quickly rinse and drop into warm acetic acid.
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[*] posted on 12-4-2008 at 13:16


Today I added some more acetic acid (quite a lot has evaporated) and diluted it with some warm water.



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[*] posted on 16-4-2008 at 20:11


@zinc
Were you successful in making the ZAP yet?




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[*] posted on 17-4-2008 at 00:57


Not yet. As my attempt to make Zn acetate failed. Today I am going to dissolve Zn in HCl and later precipitate the hydroxide with NH4OH (first have to buy that). Then dissolve the hydroxide in acetic acid.



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[*] posted on 17-4-2008 at 02:03


Be careful when you precipate with NaOH because zinc is ampother! If you add too much, the precipate will redissolve:

[Zn(H2O)6]2+(aq) + 2OH-(aq) ---> Zn(OH)2(s) + 6H2O(l)
Zn(OH)2(s) + 2OH-(aq) ---> Zn(OH)42-(aq)

Na2[Zn(OH)4] is well soluble.

If you have sodium carbonate, use that! You will get basic zinc carbonate plus quite some CO2 bubbling. Zinc carbonate does not redissolve in excess sodium carbonate and it will be easier to neutralise your acetic acid with it. Just add zinc carbonate until no more is dissolve and no more CO2 is formed, then filter & evaporate the solution.
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[*] posted on 17-4-2008 at 12:05


Very good. I will then use that method (which is better for me as then I don't have to buy NH4OH and I already have sodium carbonate).

Today I put some Zn in HCl to dissolve and tomorrow I will precipitate the the basic carbonate.




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[*] posted on 18-4-2008 at 12:59


Right now I am filtering the precipitated Zn carbonate. When it filters I will dissolve it in acetic acid and add 30% H2O2 to precipitate the peroxide complex.



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[*] posted on 18-4-2008 at 13:24


When it filtered I dissolved it in an excess of acetic acid and added some 30% H2O2. Nothing precipitated. Only the solution turned to a brown (but transparent) color. Does anyone know why did it happen?

And one more question, is that complex explosive? As the patent doesn't say that it is.




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[*] posted on 26-4-2008 at 09:52


I may have made some TACN by adding a large excess of NH4OH to a CuSO4+NH4NO3 mixture. It became deep blue, almost violet. Some copper metal was precipitated, but was then formed into CuOH. I filtered to get just the solution. Can you precipitate TACN with rubbing alcohol?



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[*] posted on 4-5-2008 at 05:30


I think that it can but I never tried.



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[*] posted on 5-5-2008 at 00:49


TACN should be insoluble in ethanol but copper(II)nitrate is soluble. I doubt you can precipate TACN from a solution containing [Cu(NH3)4](2+), SO4(2-) and NO3(-) ions. You might be able to get a mix of the tetrammine sulfate and nitrate tough.
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[*] posted on 29-5-2008 at 02:17


I just made some tetraamminecopper(II) persulphate.

When I put some of the dry material in a test tube, and heat the test tube, it explodes with a small 'Poof' sound.
White smoke evolves and a light green residue remains.
This residue dissolves in dilute hydrochloric acid. Small amounts of gas (bubbles) are evolved while it dissolves.
Now who knows what reaction is taking place when this compound explodes/decomposes? I have no idea.
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[*] posted on 29-5-2008 at 04:06


The persulphate ion oxidizes the ammonia in the cuprammine complex, but the compound is highly oxygen deficient, so the explosion is not powerful.



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[*] posted on 29-5-2008 at 05:21


Yes, I know the persulphate is oxidising the ammonia, but I can't figure out what's really happening... What is the equation?
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[*] posted on 29-5-2008 at 05:42


You can't give a precise equation of this. There are so many reactions.

For the oxidation part, you could write: 2NH3 + 3[O] --> N2 + 3H2O

Here, the [O] comes from the persulfate ion: S2O8(2-) --> S2O7(2-) + [O]

The persulfate ion then with the water formed builds two bisulfate ions, free pyrosulfate certainly will not exist under these conditions with ammonia and water present. These bisulfates consume other ammonia molecules and the heat of decomposition also certainly will expell some ammonia from the complex as well. This explains why the solid becomes light blue/green, the tetrammine complex is destroyed.

Most likely, there also will be some unreacted persulfate as well. This explains the bubbling when it is added to hydrochloric acid.

[Edited on 29-5-08 by woelen]




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[*] posted on 22-6-2008 at 14:17


is there tetramminecopper(II) picrate? :o
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[*] posted on 22-6-2008 at 23:35


Well, yes there is. However I don't see any reason to pop my eyes out over it.
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[*] posted on 26-7-2008 at 06:52
The Combustion of the Salts of Tetraamine Copper (II).


Not a free download yet, but thought I would pass along this citation

http://www.ntis.gov/search/product.aspx?ABBR=AD779649

http://stinet.dtic.mil/oai/oai?verb=getRecord&metadataPr...

http://stinet.dtic.mil/stinet/jsp/docread.jsp?K2DocKey=http%...

Another related thread on TACN
http://www.sciencemadness.org/talk/viewthread.php?tid=2187&a...
and this post
http://www.roguesci.org/theforum/showpost.php?s=a13507bed910...

______________

Just a thought,
It occurs to me that formaldehyde will condense with a coordimated metal amine complex.
Assuming coordination is not completely destroyed releasing the metal oxide, this would add
fuel to the oxygen rich compound.


A Textbook of Inorganic Chemistry Ed. J. Newton Friend
Vol X The Metal Amines M. M..J. Sutherland 1928
This I must have obtained on this forum but the location eludes me so download here
http://www.keepmyfile.com/download/df912e2298535

Explosive Properties of Metal Ammines
Previuosly provided by Roscoe Bodine, here
http://www.sciencemadness.org/talk/viewthread.php?action=att...

Related to my conjecture above

Attachment: Reaction between Formaldehyde and Ammonia.pdf (763kB)
This file has been downloaded 1002 times

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[*] posted on 27-7-2008 at 02:53


Interesting stuff, thx 4 the upload!

I wonder if an explosive complex might be obtained by heating Ca(NO3)2 in a steam of dry NH3. Bis-en-copper(II)bromate might also be obtained this way.

I believe there is some kind of water of hydration in TACN and TACP. Both salts dont burn readily even when completely dry. However, when heated carefully in a steam of dry air for some time their blue color shifts towards a deep violet color and these violet salts DO burn/explode readily. In moist air I observed that my putative anhydrous TACP turns deep blue again after a short time. Also I once left a small bottle of TACP in a very hot spot in the sun (not a wise thing I know :cool:) and droplets of water deposited inside and the salt turned violet. When put in a cold place again the droplets disappeared and the color gradually shifted towards the familiar blue again. Freshly precipated tetammine-Cu-persulphate also forms blue needles. These dont burn very well. After washing with ethanol and heating in a stream of warm air however a violet powder is obtained which explodes from flame and impact readily.

TACN will decompose in open air into green inert junk when its not completely dry so dont try heating it until its carefully washed with anhydrous ethanol.

Btw Bisethylenediamine-copper(II)-perchlorate easily precipates from solution when ethanol is added. Its insoluble in ethanol and thus can be obtained easily in a perfectly dry state. Forms violet needle-shaped crystals and explodes readily from impact however it is slightly hygroscopic.

Slightly off-topic but might be of interest anyways: There is a potassium-chlorate-tartrate double salt which is said to be explosive. I made some of this by mixing stoichiometric hot solutions of potassium chlorate and potassium tartrate. First little cubes started to crystalize which did not show any energetic properties - I suppose this was the tartrate alone. Then plate-like crystals appeared which when ignited with a match burned instantaneously with a little flash. I did not test impact sensitivity tough.

Here's some more double salts you might want to try:

Calcium-acetato-perchlorate: 2/50 mol Ca-acetate are dissolved in 50ccm H2O and 1/50Mol 50% HClO4 is added. The sol is evaporated over H2SO4.

Barium-sodium-acetato-nitrate: 54g Ba-acetate and 34g sodium nitrate are dissolved in 120cc hot H2O and left to evaporate @RT. First Ba(NO3)2 will crystalize; the double salt forms long prisms and explodes upon heating.

Theres also a lead-sodium-acetato-nitrate double salt which should be easy to prepare: 15,2g lead acetate and 3,4g sodium nitrate are disolved in 80ccm H2O and left to evaporate at RT. The double salt forms small leaflets and cannot be recrystallized from water w/o decomposition.
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