TACC, TACN, and tetramine copper perchlorate

[kingspaz]

well I was searching for posts about TACC and its possible brothers (TACN and TACP)but i didn't find any real big discussions or information about these explosives or how they can be made. they have the advantage of being made from very common materials. i like to work with the bare minimum of materials (like making everything myself and only buying things if absolutely necessary). I was wondering if copper chloride could be used instead of copper sulphate? i think it can be made by electrolising a salt solution with copper electrodes (the chlorine from the electrolysis will react with the copper)
also another post brought up the point of not using copper to contain AN because of a possible formation of TACN. does anybody know a way to do this on purpose? I would also like to know what results anybody has had making TACC or its brothers as I'm thinking of dreaming of some very soon.
thanks

[PHILOU Zrealone]

I have some cristalls of TACN and TANN laying in my basement lab...dark blue-green to black cristalls difficult to get dry explode on heating just after melting in its cristallisation water!
I have made those by mixing copper nitrate solution with an excess of ammonia solution in ethanol!
Perchlorates should be more sensitive and feasible the same way!

Another good way to make TACN and TANN would be to make a hotsaturated solution of NH4NO3, stir it while incorporating Cu(OH)2 or CuO (or Ni(OH)2- NiO).
CuO + H2O --> Cu(OH)2
Cu(OH)2 + 2NH4NO3 <==> Cu(NO3)2 + 2NH3 + H2O
Cu(NO3)2 + 4NH3 --> (NH3)4Cu(NO3)2
You should end up with TACN,CN,AN

In situ making of this!
mix dry Cu(NO3)2 + dry (NH4)2CO3
Cu(NO3)2 + (NH4)2CO3 <==> CuCO3(s)+ 2NH4NO3
(NH4)2CO3 <==> 2NH3 + H2O + CO2
Cu(NO3)2 + 4 NH3 --> TACN
Thus after a while
Cu(NO3)2 + 2(NH4)2CO3 --> TACN + 2CO2 + 2H2O



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[J]

This has got me thinking about making Cu(NO3)2 from CuSO4. I first thought of reacting NH4NO3 with CuSO4, but the products (Cu(NO3)2.3H2O and (NH4)2SO4) both have almost the same solubilities at 25 deg. C. However, K2SO4 has a much lower solubility than Cu(NO3)2.xH2O, so how about heating a solution of KNO3 and CuSO4? I worked out the reaction equation (assuming the reaction will take place) to be:

CuSO4.5H2O + 2KNO3 = Cu(NO3)2.3H2O + K2SO4 + 2H2O

The solution could then be boiled down until the K2SO4 precipitated, and the Cu(NO3)2 could be left in the solution for the intended purpose above. I'm not quite sure about the waters of hydration, but I doubt it matters if the Cu(NO3)2 is left in the solution.

I'm not much of a chemist, so I'd appreciate it if people would correct any errors (or point out any fundamental flaws ;-)) in this idea.

J

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[PHILOU Zrealone]

Could work if solubility of K2SO4 is much lower than the one of KNO3; it could also help if Cu(NO3)2 is also less soluble than the original CuSO4!!!!

Another idea would be...with:
1)
NaOH or Na2CO3 and HNO3(dil)

2NaOH(aq) + CuSO4(aq)--> Cu(OH)2(s) + Na2SO4(aq)
Na2CO3(aq) + CuSO4(aq)--> CuCO3(s) + Na2SO4(aq)
Cu(OH)2(s) + 2HNO3(aq)--> Cu(NO3)2(aq) + H2O
CuCO3(s) + 2HNO3(aq)--> Cu(NO3)2(aq) + H2O + CO2(g)

Because Cu(OH)2 and CuCO3 are unsoluble compounds!

2)
Ca, Ba nitrate

CuSO4 (aq)+ Ca(NO3)2 (aq) -->CaSO4(s) + Cu(NO3)2 (aq)

Because Ca and Ba sulfate are unsoluble salts!

Let me remind you that unsoluble means that it is very little soluble but stil soluble a little!
Conclusion:
Nothing is really unsoluble!
"Not even this problem!" http://theforum.virtualave.net/ubb/smilies/smile.gif http://theforum.virtualave.net/ubb/smilies/wink.gif http://theforum.virtualave.net/ubb/smilies/biggrin.gif

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[Cipolla]

Copper carbonate only exists as double salts with other carbonates or copper hydroxides. The pure compound doesn't appear.

[kingspaz]

thanks guys. does anybody know what colour Cu(OH)2 is? and what colour NaOH is? i think i made some accidently when i was trying to make copper chloride.
thanks again.

[Cipolla]

Cu(OH)2 is an insoluable dark blue solid which decomposes yielding CuO. NaOH is colorless, but you should know this.

[kingspaz]

i thought copper carbonate does exist alone. i'm sure we did an experiment in school with it. it decomposed to copper oxide and carbon dioxide when it was heated. the reason i don't know the colours is because i've never seem them. i thought that the Cu(OH)2 would be blue with it being a copper compound and i also thought that the NaOH would be clear but i was just checking.
thanks guys

[PHILOU Zrealone]

Copper carbonate (blue sky to pale turquoise blue) exists so does the mixte copper carbonate-hydroxyde -emerald green to deep blue when cristallised (see malchite/lapis lazuli) when uncristallised it is pale turquoise green (in french we say "vert de gris" green of grey or copper rust that forms on all copper containing alloys!

Copper hydroxyd is deep blue sky when sunny day!

NaOH is colourless!

"From taste and colors we should never discuss!" French idiom!

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"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"

[J]

Is TACN less sensitive to shock, friction and heat than TACC? By the same account, does TANN have about the same sensitivity as TACN?

Also, could the reason for the low sensititivy of these compounds compared to other primaries be due to the waters of crystalisation?

J

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[PHILOU Zrealone]

Much less sensitive than TACC!
About the same sensitivity for TACN and TANN!

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[gcic]

PHILOU Zrealone, you said that you possess some cristals of TACN. So I`d like to know, please, how long someone could probably store TACN and what would be the best conditions to store it? Would it be better to store it in ethanol or acetone (is it soluable in it?) or in dry form?

According to Philou the cristals melt before there occurs an explosion. So I doubt if you could initiate it by using a fuse.
Did anyone test this?

And concerning the sensitivity: I am afraid that I don`t know anything about TACC`s sensitivity. As a consequence I cannot imagine the sensitivity of TACN. Does anyone have a comparison to other (primary) explosives ?

THX for your information!

[kingspaz]

kitchen improvised blasting caps says that TACC has about the same sensitivity as lead azide. i would say that this is a fairly reliable source as it is a good book. even so another opinion would be best.

[This message has been edited by kingspaz (edited June 19, 2001).]

[PHILOU Zrealone]

My cristals were dryed at 50C in open air; they for sure contain a lot of water- to dry them completely for use, I would need a strong dryer like dry MgSO4/CuSO4 and a large container used in labs (I don't have one so it is a bit a problem for me to get them very dry).
You can store them like that in film canishers because with their water of cristallisation they are rather insensitive to shock and flamme.

Solubility in ethanol and aceton is very low even lower in ether.

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[gcic]

Thank you very much for your answer!!
You said that the cristals aren`t completely dry. That`s okay. But how do you detonate TACN as a primary? I mean, it wouldn`t be very reasonable to detonate a primary explosive (TACN) with another primary explosive (e.g. lead azide), would it?
Is it possible to ignite it with a glowing copper wire, which glows about a second? I don`t know, how much heat this device produces, but it must be several hundred degrees celsius, if you ask me. And a rapid increasing temperature should workto detonate it. Do you agree??

[PHILOU Zrealone]

When the stuff is confined and well dried no problem at all to set it off.
For my test I heat them in the open on an aluminium sheet...they melt bubble and then flash (like nitrocellulose).When enclosed in the same Al sheet (several layers) and trown in a fire ....bang!

A detonator or a wire must set it off.

The only problem is getting it dry and to keep it that way.

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[kingspaz]

could you set it off with a chlorate/charcoal primer of some sort? would it burn hot enough to set it off? just a thought.

[J]

I can confirm that getting TACC to dry is very difficult :-(

J

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[kingspaz]

thanks for all the info guys. has anybody here tried making tetramine copper perchlorate? it should be more powerful than TACC because more gas would be produced. it could be worth looking into.
on my other post about setting off TACN with a chlorate priming mixture i should have explained my logic. if the chlorate mixture burns (chlorates burn hot) then it will melt the TACN next to it. this small amount of TACN will detonate setting the rest of the TACN off.

[J]

The problem with that is that the damp part won't detonate, only the small amount that's been heated. That's my understanding anyway.

J

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[Mr Cool]

I *think* a chlorate/charcoal primer will set it off in a cap. A temperature rise that high and that sudden is good at setting off most primaries.

[J]

Even when not completely dry?

J

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[Mr Cool]

It won't work when it's soaking wet, but a *bit* of moisture shouldn't matter.

[kingspaz]

i left a penny to soak in a strong AN solution and now (after a week) the solution is dark blue. i think i have made a very small amount of TACN so i'll leave it another week and then evaporate the water off and collect the crystals. i won't put it on a stove or anything, just the conservitory. i'll try and find a quicker way of doing this over the next couple of weeks.

[Alchemist]

Hello all,

Say PHILOU ,

Have ya experimented to find out at all what is more senitive tetramine (Copper, Nickel, or Cobalt), Nitrate / Chlorates?

Anyone else experimented with these. I have some Tetramine Nickel Nitrate about done so I'll let ya all know when it's done!

[Mr Cool]

I don't know about the cobalt salts, but I think the order of sensitivity is (highest first): TACC, TANC, TACN, TANN. I haven't made the nickel salts, but that's the impression that I get from reading other people's results.

[PHILOU Zrealone]

Precisely for a same metalic cation chlorates more sensitive than perchlorates more sensitive than nitrates!
For the metal effect no general rules... it is the case for all primaries... sometimes one is fairly insensitive while the other is very sensitive, sometimes it is the contrary.
Always be aware of that.

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"Life that deadly disease sexually transmitted".
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[kingspaz]

well nobody had much to say about the penny soaking in AN solution but i hope you should have something to say now http://theforum.virtualave.net/ubb/smilies/smile.gif. i decided to find a quick method of making TACN from metallic copper and AN. what i did was heat copper wire in a boiling saturated AN solution. i boiled this for about 3-5 minutes (it was just to see if it worked so nothing was measured). i let the solution cool and AN started to crystalise so i added a very small amount of water to so it redissolved (i think if i boiled it less then i wouldn't have had to do this) anyway i left it to stand and returned to it 2 days later. i was pleasently surprised to find TACN crystals all over the copper and floating on the surface in a very, very dark blue solution. i tested some that i scraped off the surface by lighting it. it melted, turned a brownish colour and made a 'pop' noise. i will continue test when the solution evaporates in the conservitory then i will also work out the exact amounts of copper an AN to use and times and things. i'll probably have it done in a couple of weeks due to wet weather.

i'm also going to try tetramine copper perchlorate after my holiday in a few weeks.

[This message has been edited by kingspaz (edited June 27, 2001).]

[Alchemist]

Hello all,

Sorry kingspaz,

I am doing the exact experiment, both with Copper and also Nickel. Seems that yours is closer to done than my experiment. I'll be sure to let you all know how the Nickel comes out.

*** To bad Cobalt is so expensive, have some interesting formulas for ammonium hexanitrocobaltate !

[kingspaz]

Alchemist, i'm glad your doing the same thing so if one of us has problems then maybe the other person can explain them or somthing. i've also had a thought on TACP (tetramine copper perchlorate). i thought maybe it would be possible to react sodium perchlorate with TACN solution to get TACP and NaNO3. it would be much simpler to make TACN and then convert it to the perchlorate other than making the TACP from copper sulfate, NaClO4 and ammonia. the perchlorate should be the best performer out of all of them as it will should be more water resistant, have more power due to extra gases made, and it will be more sensitive than the TACN.
heres my equation for making TACN i think its wrong because it looks wrong but i'm bad at equations so can someone please correct it.
5NH4NO3 + 2Cu ----> 2Cu(NH2)4NO3 + H2O + H2 + 4O2

thanks guys

[Mr Cool]

Maybe this:

4 NH4NO3 + 2Cu --> Cu(NH3)4(NO3)2 + Cu(NO3)2 + 2H2

I'm not entirely sure if this is right (is TACN Cu(NH3)4(NO3)2?). Also, I'm not sure about it forming gaseous hydrogen, but I can't see any other way it could work, unless it formed Cu(NH4)4(NO3)2, but then each of the ammonium groups would be +1, the Cu would be +2, and each of the NO3's would be -1, resulting in a charge of +4!! Have I overlooked something here?

[PHILOU Zrealone]

Beware of the perchlorate!!! While making it:
Don't heat it to evaporate the water simply allow to evaporate slowly by natural evaporation at medium heat!

Since sensitivity is in the order:
Chlorate> perchlorate> nitrate
NH4ClO3> NH4ClO4>> NH4NO3
NH2-NH3ClO3> NH2-NH3ClO4>> NH2-NH3NO3
Cu nitrate hydrazinate is so unstable that it decompose imediately; Ni nitrate hydrazinate is a precipitae complex more sensitive than the original hydrazine nitrate (HN has about the same sensitivity as amonium perchlorate). Ni hydrazine perchlorate is more satble but is so sensitive that it can explode in water solution by little agitation!

From all this we can conclude that metal derivatives of an aminated oxidiser salt are more sensitive than the original salt.
TACC> NH4ClO3
NiNH> HN
TACN> AN
TANN> AN
CuPH> NiPH>> HP

My guess then for TACP (tetraminocopperperchlorate not cyclotriacetonperoxyde!) and TANP is:
TACP>TANP>NH4ClO4 ...

By the way:
2HClO4 + Cu(OH)2--> Cu(ClO4)2 + H2O
Cu(ClO4)2 + 4NH4OH --> Cu(NH3)4(ClO4)2 + 4 H2O

or
2NH4ClO4 + Cu(OH)2 + 2NH4OH--> Cu(NH3)4(ClO4)2 + 4H2O

You can also use CuO!



------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"

[PHILOU Zrealone]

Higher sensitivity to shock, friction and heat!

------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"

[PHILOU Zrealone]

Good trial Mr Cool, but no...I'm sorry to disappoint you http://theforum.virtualave.net/ubb/smilies/frown.gif .
Cu reacts because of air superficial oxydation into CuO, Cu(OH)2 and CuCO3 (and mixes of all)....that oxydation is slow in the open due to the unsolubility of the layer but stil it does it.
When in water...especially salted or acidic water corrosion occurs much faster and thus layer after layer all the Cu is solubilised as its deep blue complexated form.
NH4NO3 is an acidic salt...reason why this happens.If you make it in an enclosed vessel almost no TACN will form you need air (oxygen dissolved in the liquid media is consumed by the oxyd layer and turns into water after reaction see in a previous post of mine).
No free hydrogen thus.

------------------
"Life that deadly disease sexually transmitted".
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[Mr Cool]

Right, I see now.
Thanks.

[Mr Cool]

Right, I made a solution of 32 grams of NH4NO3 in c. 25mL of water. I heated it up to c. 80*C, and added 13 grams of copper, in the form of very fine uncoated wire, 40 s.w.g. I think it was. Nothing happened, as expected. Then I remembered the need for oxygen - so I poured in a few mL of 9% H2O2, while it was at about 45*C. Lots of bubbling due to the copper and heat, a small amount of dark insoluble precipitate (looks like a colloid, but it's coagulating) formed which I suppose is CuO, and the solution INSTANTLY TURNED DARK BLUE. I'll leave it for a while to see what happens, all that copper should react eventually. I will then bubble NH3 through it to convert the Cu(NO3)2.
Results will end up on my web site so if you want to know what happens then have a look at it in a few days time.

A similar compound, recipe from FEMFEP.

Trishydrazinezinc(II)Nitrate

To a solution of 5.0 grams of zinc nitrate in 25 ml of ethyl alcohol was
added a solution of 1.7 ml of 95 percent hydrazine in 5 ml of alcohol. The
precipitate that immediately formed was collected on a filter an washed
with ethyl alcohol. After drying for 2.5 hours at 90 centigrades the
product weighed 4.45 grams.

It says nothing else about it.

In the UK, pre-1990 copper coins are an alloy of copper and nickel, they should work quite well to make this primary. If the two compounds form crystals together, then I have a theory that it might make it more sensitive than with just one sort of metal ion. I think that if the metal ions are a different size, then they will fit together less well in the crystal lattice, and therefore make it easier for the compound to decompose. Just a thought.

[kingspaz]

thanks mr cool, i was thinking of bubbling ammonia through my next batch and also using H2O2. with my first batch i'm having trouble separating the TACN from excess AN and the Cu(NO3)2. i will over come this somehow on my next attempt in a couple of days. it should be easier to separate due to there being no Cu(NO3)2 left because of its conversion to TACN. could addition of acetone force the precipitation of the TACN? i think it would but then it would also force the precipitation of AN....

[This message has been edited by kingspaz (edited July 02, 2001).]

[J]

I recently attempted to produce TACN by electrolysing an almost saturated solution of NH4NO3 with a copper anode. The result was a dark blue solution, and a considerable amount of Cu(OH)2. NH3 gas was given off throughout the process (which I left on for about 14 hours).

A sample of this was placed in an evaporating dish made of Al, and boiled over a flame (alchohol burner) untill a thin film was observed on the surface of the solution. When allowed to cool, the solution solidified into a blue/white solid. When small amounts were heated on Al foil, it became liquid again and gave off a dense steam. Just before the solution was completely evaporated, there was a quiet 'pop' and a black burn mark was left on the Al foil.

I won't pretend I completely understand what's going on, but I believe TACN formed in the solution. Also present in the solution were NH4NO3 and Cu(NO3)2 (I think).

Now for the questions:

1. Are my assumptions correct?

2. If so, can anyone think of a way to separate the TACN from the other components in the solution?

One more thing: I used a length of Nichrome wire as the cathode. This was covered in a solid 'bubbly' substance at the end of the reaction, which was hard to remove. Most interestingly, a tiny dark purple crystal was present just above the solution. When heated, this burnt quickly with a pop. Could this be TACN, or even TANN (the Ni in the wire reacting)?

J

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[Mr Cool]

Purple? I suppose it could be TANN, I'm not sure what colour that is. But what else could it be?!
That will be making TACN, not sure how you'd seperate it from the other things.
My method (copper + AN + H2O2 + NH3) seems like it would be good if CuO or Cu(OH)2 was used instead of the Cu, to speed it up.
So next time I'll mix 2NaOH and CuSO4 to get Cu(OH)2 and Na2SO4.

What is the longest anyone here has stored TACN or TACC?

[Donutty]

Mr Cool, I tried your method but no solid was produced. The blue solution turned dark red/brown when I accidentally added too much 17.5% H2O2. I left it over-night and it had returned to it's original blue colour. Lots of large needle-like crystals had formed at the bottom of the jar and were obviosuly insoluble in the solution. I tried washing them with water but they dissolved! http://theforum.virtualave.net/ubb/smilies/frown.gif

[Alchemist]

Hello gang,

I just finished experiments with tetramine copper nitrate and also tetramine nickel nitrate. The nickel was a VERY GREEN/BLUE color crystals and the copper was A VERY DEEP BLUE color crystals.

It was stated "J" used Nichrome wire . You probably made a VERY small quantity of

Tetramine Chrome Nitrate, I believe this would be PURPLE. Just a guess though!

[This message has been edited by Alchemist (edited July 03, 2001).]

[Mr Cool]

Was it CLEAR dark red/brown? Because if it was cloudy/opaque then it might just be all the CuO floating around. I also get what I assume to be Cu(OH)2 as a green precipitate after a while, from CuO and water. Try washing those crystals you get with acetone, TACN isn't soluble in that apparently. Although large needle-like crystals sounds like it might be NH4NO3, cloured by the solution.
This method is WAY too slow with copper metal I've decided, it'd be best to use a basic copper compound. Or react CuSO4 with Ca(NO3)2 to get Cu(NO3)2 and insoluble CaSO4, which you can filter out. If Cu(NO3)2 is soluble in acetone, then it'd be great. Just bubble NH3 through it and you'll get TACN precipitating. Carry on until the solution is clear, and filter it. Drying will be easy due to the acetone. I'll try this, using Cu(OH)2 and H2SO4 to make CuSO4.

[PHILOU Zrealone]

One single problem Mr Cool Aceton reacts with ammonia to make imines and polymers of it!

Donuty: why the hell did you try to dissolve those cristalls in water TACN and TANN are very soluble in it...why didn't you simply filter them off and make some tests with it like flame sensitivity? What was the color of those cristals-dark blue or light blue?

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[Donutty]

I did do some flame tests on them...my conclusion - NH4NO3. I foolishly tried to wash them using water http://theforum.virtualave.net/ubb/smilies/frown.gif

However...I also had some dark blue crystals form on a copper coin. I tested these by heating on Al foil over a flame. They started to bubble and deflagrated with a 'puuup' and lots of smoke. A black scorch-mark was left where the crystals once were.

[Donutty]

I.e. I got the same result as you J

[Lagen]

Hey Mr Cool: I think that what you're getting as the green ppt is a mixed copper hydroxide and carbonate (the hydroxide picks up CO2 from the air, as it is acidic). Pure hydroxide would be blue. When I make mine it's deep blue, but soon decomposes to give a mixture of CuO (brown to black) and the above substance (the CuO gets a greenish shade). I'm told the mixed hydroxide-carbonate should decompose on heating to give back CuO, so does mine - when I boil it, it turns black again.

[kingspaz]

well some very good news at last folks. two days ago after reading some replies on this topic i decided to try a slightly different method to the last one i tried. i did the following (the measurements after the ones in step 1 are aproximate):
1. dissolve 10g AN in 30g 9% H2O2 then add 30g copper wire.
2. bring this to the boil (water boiling not H2O2 decomposition - can look similar)
3. leave this to drop to about 70*C.
4. add additional 10g H2O2 and stir vigourously.
5. boil for a minute.
6.leave for 2 days (i was surprised the solution only turned slightly light blue after the 2 days)
7. add 20g 9% ammonia solution.

well thats what i did. the result i got was that i now have TACN crystalising out of the solution. the reason i didn't use much AN is because it is a left over product along with Cu(NO3)2. because i used little AN the result was it was all used up. the addition of more than enought ammonia solution resulted in no Cu(NO3)2 being left. together this makes a solution of only TACN. i will be filtering and evaporating left over water tomorrow and will hopefully test the crystals on the same day http://theforum.virtualave.net/ubb/smilies/smile.gif
p.s. thanks for all the help guys!!! http://theforum.virtualave.net/ubb/smilies/smile.gif http://theforum.virtualave.net/ubb/smilies/smile.gif http://theforum.virtualave.net/ubb/smilies/smile.gif

[This message has been edited by kingspaz (edited July 05, 2001).]

[J]

After the two days, how much of the wire was oxidized? This is something I will try :-) I might bubble anhydrous NH3 instead of using NH3 solution, this would minimise the amount of extra water added.

J

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[kingspaz]

i'm not sure how much wire was oxidised after the 2 days but i could see it had been corroded. i'm not sure if all the AN has been used up but i'll see later as i filtered the crystals that precipiated this morning and left the dark blue liquid in the conservitory to evaporate. hopefully i should be left with lots of TACN. i think while it was sitting in the shed additional water evapourated as the shed does get very hot. also i think i may have added a small amount of additional H2O2 after sitting for 1 day. i'm sure this procedure could be perfected as i just made it up on the spot pretty much. hopefully if the TACN is dry enough later i'll try to detonate a small amount in a pen lid or something.

[This message has been edited by kingspaz (edited July 06, 2001).]

[Alchemist]

Hello gang,

You know what's strange about TACC, TACN, tetramine copper perchlorate, and etc., is that I can find no mention of them in CHEM books , patients, etc.. Nothing on there properties, uses, or anything else. Has anyone else FOUND anything about them?

After we get a good crop of these we need to figure out some good uses and properties!

[kingspaz]

i'd say i have about 5-7grams of TACN some still in solution though but crystilising as the water evaporates. i tried to set some off today but i don't think it was dry enough as it only fizzled. i filled a party popper handle loosley with it and put a charcoal/chlorate priming mixture on top. afer ignition it fizzled a bit and that was it. i have also done some searching for them so i can find some properties but theres absolutely jsck shit about them. all i found was copies of KIBP. i'm off on holiday on tues so i'll try and get some dry enough and i'll post back my results.

[Mr Cool]

Water content is a problem. The explosive thing in a party popper would probably set it off by itself when dry.
I have one idea about keeping it dry: dry it, and then mix it with glass microbubbles (to keep density low) and polyester resin, and casting it into little cylinders that could be slipped into a detonator. I don't know how well this would work, if at all, but it could be worth a try. Or pushing the mixture through a sieve to granulate it.

[kingspaz]

good idea mr cool. i was thinking of senitising it with KClO3. also i don't think its as bad as NH4NO3 or NaClO3 when it comes to moisture absorbing. i could be wrong though because i've only had some for one day.

[the_wingman]

hey PHILOU
In the first section you've stated that TACC is more sensitive than ammonium chlorate. I wonder if this is really true because NH4ClO3 is supposed to be very!!! sensitive. Otherwise, if you're right, why noone uses NH4ClO3 as primary?

[Mr Cool]

I've just made diaminezinc nitrate and diaminezinc chlorate, I'll let you know the results when they're dry. Well, actually I don't even know if I have made them because they're both in solution.
DAZN is used to phase stabilise AN composite rocket fuels, I doubt it will be sensitive, but I think the chlorate might be.

[Mr Cool]

So far I've heard of copper, nickel, chromium, cobalt, silver and zinc being used as the metal. You can make the nitrate, chlorate or perchlorate (or any other, but they might not be explosive, e.g. sulphate), and the ammonium or hydrazinium compound. That makes 36 variations!
What about using methylamine instead of NH3 or N2H4? Or hydroxylamine, etc etc etc etc etc etc. The possibilities are pseudo-endless!

[kingspaz]

36!!! thats plenty enough to play with!!! i'm not sure if there are problems with the TACN i made. i think it may decompose back to ammonia and copper nitrate, not very sure at all though. i spilt a bit outside accidently and the next day it was light blue. i'm not sure about this but i've left some to dry further in the conservitory and when i come back from holiday in a couple of weeks i'll see if it has decomposed.

[Anthony]

Or if it proved to be unstable, exploded taking out conservatory window, the neighbours thinking something was up (you've gone away so they're looking over your house for you) call the police, who realise that an explosion has occured and investogate the cause. They find lots of evidence that the resident was illegally manufacturing explosives. By the time you come back it's all been in the paper and the police great you at your door to read you your rights - you never know!http://theforum.virtualave.net/ubb/smilies/smile.gif

Interesting thread, easy though these explosives appear to me to make, they seem to have lots of disadvantages. Do you think they have any practical uses?

[Mr Cool]

Not very energetic, don't detonate easily from flame, many are hygroscopic, become dead-pressed...
Yes, many disadvantages! But so simple!
I think that if it is possible to use methylamine instead of ammonia then they might be more energetic, due to the carbon as fuel, and using a less reactive metal like silver may help. Chlorates are the least stable of the three oxidising units, so maybe dimethylaminesilver chlorate would be useful? But you'd have to find a source for silver, which is actually quite cheap if bought at bullion value, and make the methylamine so it becomes less simple!

[kingspaz]

well i've been thinking maybe TACN could be well suited as an explosive for use in exploding incedary gel as when TACN melts it explodes. if i mixed this with the napalm i use (high AN and oil content) then i have a primary and secondary in the napalm. well its a possibility. i have to say though i don't think TACN doesn't absorb moisture that easily. from the past few days its just been sitting there out in the open (indoors) and doesn't seem to have abosrbed any extra moisture as it still flows easily. i think maybe a small amount of graphite could help keep it dry once it is dry.

[Alchemist]

Hello all,

At his point, it seems to me that we need to start experimenting with some fuels to use with these compounds. Maybe different metals (Al,Mg,Ti,Zr,etc.), carbonous compounds,
boron,etc.

Also I agree with Mr. Cool in more experimentation with the Ammonium,amines,amides,hydrazinium,hydroxamines,et c.,compounds would afford may hundred or even more such compounds.

I have at present been looking for information on the making of Hydroxamine Hydrochloride or Sulfate. If anyone has any information on these, please email me. Thanks!

[kingspaz]

well after looking at my TACN after 2 weeks on holiday it seems to have decomposed. the other stuff i have that was sealed in a film container has shown no signs of decomposition. the stuff left out to dry for to weeks seems to have decomposed to copper nitrate (well if Cu(NO3)2 is light blue then it has decomposed - TACN could be light blue when thouroughly dried). does anybody have any ideas how to sensitise it?

[Lagen]

I store mine under acetone, in a sealed container. The acetone becomes black with the dissolved TACN, but it lasts for ages. When it is reduced to a small particle size (not too fine however, preferably by recrystalization) and thoroughly dried you should have no problem setting it off. There are 3 things that cause it to deteriorate: water, loss of ammonia and heat. Use a desiccator with some strong drying agent, and a larger batch of TACN - I use about 10% of the desiccator volume, the air in the desiccator becomes saturated with ammonia and there is no decomposition.

As to the colors: most people call TACN very dark blue, well it is, with a bit of purple, especially in passing light, but thick layers and big crystals are black, with purplish lustre, not unlike permanganate. If you have a sky blue color then it's most definitely copper nitrate. I *think* that even copper nitrate is not stable, mine slowly converts to a turquoise powder very much like copper hydroxide.

TACN also exhibits some crystal shape variations: when crystallized slowly (like for a week) the crystals are needle-like (sometimes hair thin). If done faster, they are rectangular plates, like calcium nitrate. Fast crystallization (like 6 hours) from a very heavy solution produces granular, almost black crystals. I don't know which system they belong to, guess it's triclinic. They have triangular surfaces on them.

[This message has been edited by Lagen (edited July 30, 2001).]

[Hex]

We had a Postgrad in our lab last month trying to make nitrates of Copper (to replace non-energetic copper salts as burn rate catalysts for AN rocket motors) and he had a hell of a time. The only useful way of getting it is as a complex with N2O4. But this is so moisture sensitive that I can't see any practical use for it.

<font face="Verdana, Arial" size="2">Originally posted by kingspaz:
well I was searching for posts about TACC and its possible brothers (TACN and TACP)but i didn't find any real big discussions or information about these explosives or how they can be made. they have the advantage of being made from very common materials. i like to work with the bare minimum of materials (like making everything myself and only buying things if absolutely necessary). I was wondering if copper chloride could be used instead of copper sulphate? i think it can be made by electrolising a salt solution with copper electrodes (the chlorine from the electrolysis will react with the copper)
also another post brought up the point of not using copper to contain AN because of a possible formation of TACN. does anybody know a way to do this on purpose? I would also like to know what results anybody has had making TACC or its brothers as I'm thinking of dreaming of some very soon.
thanks</font>

[kingspaz]

thanks guys http://theforum.virtualave.net/ubb/smilies/smile.gif

[PHILOU Zrealone]

For those who haven't a clue about complexation.
All what we have discussed here are complexing metals...and we are playing with the more usual and cheaper (Ni, Cu) complexes of iron are unstable and hydrolyses fast to carbonate and hydroxyde.
If you want to try exotic materials like Ruthenium or what go ahead but it is hell expensive.
Ni and Cu and Co (about the same price as gold so forget it) can make amino complexes. they can complexate 6 nitrogens and keep two anions near them.
So basically simply mix a concentrated solution of Ni, Cu nitrate, nitrite, chlorate, perchlorate, permanganate with all the possible amines oflow molecular weight(ammonia,hydroxylamine, urea, hydrazine, methylamine, dimethylamine, diaminoethane,...in excess; this heats a lot so care) add some ethanol and ether when reaction has finished (complexes of Cu and Ni are soluble in water but less in ethanol-ether mix). Evaporate and cristallise.
With nitrite, chlorite, chlorate, hydrazine, permanganate it is better to cristallise under vacuum without too much heat because a detonation can occur very fast since those complexes are more sensitive!


------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"

[PHILOU Zrealone]

Ahh yes!
Thus complexes are not possible with all metals they need special orbital organisation to be able to do it.
Examples of Ni/Cu complexes:
*Ni=Cu=M
*ClO, ClO2,ClO3, ClO4, NO2, NO3,MnO4,=Ox(-1)
*NH3, CH3NH2, NH2NH2, NH2OH,single amines =A
*NH2-CH2CH2-NH2, NH2-CO-NH2, NH2-CO-CO-NH2, diamines =AA

General formula:
(A)6M(Ox)2 or M(Ox)2.6A
ex: (NH3)6Ni(ClO4)2 or Ni(ClO4)2.6NH3

(AA)3M(Ox)2 or M(Ox)2.3AA
ex: (NH2CH2CH2NH2)3Cu(NO3)2 or Cu(NO3)2.3NH2CH2CH2NH2

------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"

[PHILOU Zrealone]

Not all metals can complexate amines, they need special orbitals organisation.
General formulas of complexes are:
*(A)6M(Ox)2 or M(Ox)2.6A
where A is a monoamine compound like NH3, NH2OH, NH2-NH2, CH3NH2,...;M is Cu, NI or Co; and Ox(-1) is ClO, ClO2, ClO3, ClO4 (or the iode-bromine equivalents), NO2, NO3, MnO4
Ex: (CH3NH2)6Ni(ClO4)2 or Ni(ClO4)2.6CH3NH2
*(AA)3M(Ox)2 or M(Ox)2.3AA
AA is a diamine like NH2CH2CH2NH2,NH2-C(=NH)-NH2, NH2CONH2, or NH2COCONH2 (the last two can be complexate by the oxygen or by the N).
Ex (NH2CH2CH2NH2)3Ni(NO3)2 or Ni(NO3)2.3NH2CH2CH2NH2.

------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"

[Lagen]

PHILOU, could you shed some light as to the explosive properties and stability of the complexes with respect to the various amino compounds used? I am thinking about urea complexes in particular - could they be more storage stable than the ammonia ones? Any of them could be hydrolysis proof? Should I just try? Is that too many questions?

[fightclub]

According to old Urbanski (Vol. 3), Friedrich and Vervoorst* discovered Cu(NH3)4(ClO3)2, it appeared to have detonator characteristics, but has not found use in practice. Because in air it rapidly lost ammonia [losing its explosiveness: Cu(NH3)4(ClO3)2 --> <-- Cu(ClO3)2 + 4 NH3]. And in the moist atmosphere it hydrolyzed easily.

*Friedrich W., Vervoorst P., Z. ges. Schiess-Sprengstoffw. 21, 49 (1926)

You can expect TACC to be as sensitive as or more sensitive than lead azide. I think TACC crystals are more of a purplish solid.

I am not sure about the hydrolyses mechanism but it might be: Cu(NH3)4(ClO3)2 + 4 H2O -->
4 NH4OH + Cu(ClO3)2 and maybe: 4NH4OH + Cu(ClO3)2 --> 2 NH4ClO3 (dangerous!) + Cu(OH)2 (pale blue) + unreact. NH4OH (?)


TACN also decomposes within time: Cu(NH3)4(NO3)2 --> <-- Cu(NO3)2 + 4 NH3
Some properties at alt.engr.explosives


[This message has been edited by fightclub (edited August 08, 2001).]

[fightclub]

One last thing: the heat of explosion of TACN is [probably] either:

Cu(NH3)4(NO3)2 --> Cu + 6 H2O + 3 N2 + 588 cal/g

or

Cu(NH3)4(NO3)2 --> CuO + 5 H2O + 3 N2 + H2 + 513 cal/g

going on its heat of formation of -196.55 kcal/mol. Compared to:

Mercury fulminate: 427 cal/g
Lead azide: 368 cal/g
Triacetone triperoxide: 500 cal/g


"The things you own end up owning you."

[This message has been edited by fightclub (edited August 09, 2001).]

[Lagen]

fightclub: as to the explosive decomposition of TACN, I think the second reaction (with the CuO end product) is more likely. TACN leaves a black scorch mark, which I assume to be CuO.

Regarding the hydrolysis of TACN: Some time ago I made an experiment - I left a few small crystals exposed to the air. After about 2 days they changed color from very dark blue/purple to light blue, but preserved their crystalline appearance. After another 2 days they turned into a light blue to greenish powder. I assume this to be Cu(OH)2+CuCO3. This is my guess at what happened:

TACN loses ammonia (easily detectable...):
Cu(NH3)4(NO3)2 --> Cu(NO3)2 + 4 NH3
With moisture from the air, the copper nitrate forms a solution and tends to transform into Cu(OH)2, as that is less soluble:
Cu(NO3)2 (l) + 2 H2O (l) --> Cu(OH)2 (s) + 2 HNO3 (l,g)
Basic Cu(OH)2 reacts with acidic CO2 from the air:
Cu(OH)2 + CO2 --> CuCO3 + H2O
So the overall imaginary equation would total to:
Cu(NH3)4(NO3)2 + H2O + CO2 --> CuCO3 + 2 NH3 + 2 NH4NO3
The conversion won't be perfect, as Cu(OH)2 only converts partially to CuCO3. Also, at some point there will be an equilibrium. I'm not saying it's absolutely correct, there's very little about TACN in the literature.

[fightclub]

Interesting input Lagen! I also will go with the second one. I was doubting the 1st equation because looking at the decomposition equations of other similar metal complexes they tended to involve metal oxides in the equation.

[PHILOU Zrealone]

Lagen, just try! It is cheap to try!
I assume storage stability will be improved over NH3 since NH2-CO-NH2 is non volatile and staying arround!
From now on I have made some Ni/Cu complexes of NH2-CH2-CH2-NH2 and NH2-CH2-CH2-OH and I'm quite happy with them except they cristallise very slowly (too slowly) in big dark cubic shapes (5mm side)(containing a lot of water). So on burning test they melt, evaporate water and flash/deflagrate.
I will make myself a desicator to go further in dehydration!
I don't agree with your equations
NH4NO3 is kind of acidic so CuCO3 will turn back to the complex!
In a well closed container almost no decomposition has to be detected on dried samples!

------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"

[Mr Cool]

Has anyone tried complexes with methylamine yet? I keep on thinking about it, but so far I haven't got round to trying it.
If you have, do you have any results to share?

[tvs17]

This is maybe a stupid question, but why is it sometimes needed in making this kind of complexes that the reaction is carried out in non-aqeous solvents like EtOH, and not just water. Does it has something to do with the H2O ligands around a, for example, Cu+ ion?
And another time it's just OK to do it in aqeous solutions.

For example, I tried making TACN, I made an Cu(NO3)2 solution (which was still quite acidic because I made it by dissolving Cu wire in dil. HNO3), where I added some ammonia 8%. First it turned purple, then light blue(some suspension), and then, while adding more ammonia, a beautiful deep blue solution was formed. I evaporated the water under vaccuum at 50 dC, dark blue crystals where obtained. When heating some crystals slowly on a piece of aluminium foil, the crystals melted with some smoke and little pufs. The crystal-water was released. Short after that, a puff with a small green flash was observed. But when trying to confine it by wrapping it in several layers of Al foil, and throwing it in a fire, there was only a strong puf. Nothing more. I tried this several times.

Does the description of my experiment sounds like I've made TACN, or did there went something wrong? It seems that the description of the burning properties match with other posts...

Edit: After reading all the messages a bit more well, I conclude that the substance I have is probably TACN.
I read from another post that you add EtOH for solubility properties of the solvent, but in books about synthesizing other complexes, and also for example at Mega's site TACC synthesis, the insist using anhydrous solvents like MeOH or THF. So why is this?
But still I don't understand why my TACN won't detonate. I've stored a few grams in a deexiscator for a week with conc. H2SO4, so it should be quite dry.




[This message has been edited by tvs17 (edited September 03, 2001).]

[tvs17]

Yesterday I tried to make the urea derivative of copernitrate, so TUCN. There didn't was a real visual reaction. I vaccuum evaporated the solution, but it became to viscous and didn't crystallise. So I added some water and I will just dry it know in a vacc deescitator with H2SO4. I will tell you some results when it is dry enough.
I just added some excess urea solution to a conc. Cu(NO3)2 sol. And then I added some EtOH/Et2O mix.
Do you think it would work that way?

[tvs17]

I just tested the TUCN by heating it on a sheat of aluminium. It bubbled just like the TACN, with severall puffs and a lot of smoke. The reaction seemed to be more vigorous than when heating TACN. But there was no flash at the end. When it is completely dehydrated I will try this another time.

I am making cobaltnitrate at the moment, to try to make TACN(well, TACoN). And I will also try cobaltchlorate(TACoC).

Another question, why can zinc form ammonia complexes, while I read it is not possible in one of Philou's posts?

[tvs17]

One thing I am still wondering about is, what the real structure is of the aminecobaltnitrate. Because in CRC I mainly find hexa-amine cobalt complexes. I don't have very much knowledge about complexation so I will have to do something about that.
But does anyone know which complex probably will form when reacting Co(NO3)2 with NH3(aq)? HACN ?I can also try to make some things with Co3+ salts.

I made some Co(NO3)2 by the reaction between CoCO3 and dil. HNO3. Beautiful red solution. I will let it vacc. evaporate and than wash it and evaporate again. But I already tried with some very acidic(HNO3) Co(NO3)2 solution, by adding ammonia. First it turned pink, then red, then lighter red, and finally brown. Much cobalt complexes are brown so this is probably good.
I will evaporate also this solution and let you know some results..

[This message has been edited by tvs17 (edited September 05, 2001).]

[tvs17]

I tried some of the (tetra/hexa?) amine cobalt nitrate, but it only smoked a little and not much more than that, leaving a black (probably CoO) residue.. I also suspect that the amine cobalt nitrate is quite unstable, because a strong smell of NH3 is noticed.
However, I expect more of the chlorate...
And I will also try it with non-acidic Co(NO3)2 again, to make sure no side-reactions have occured.

[tvs17]

Is nobody working anymore on this kind of complexes? Or what is the reason I get no replys.

Once again, does anyone know which complex is formed when reacting cobaltnitrate with ammonia(tetramineCN, hexamineCN)? Is it brown? Stability? Anyway, it seems that this TACoN or HACoN(or whatever it is), does not have any explosive properties. It only smokes a little, leaving it's crystalwater.

However TUCN, does show some more interesting properties. It kinda flashes, not as extreme with TACN, but it does. I didn't have time to test the dehydrated salt yet, but I suspect maybe some more vigorous decomposition.

I will also try to make a complex with nitrourea! That should maybe have more interesting properties!

I didn't come yet to the TACoC or TACoP. I will have to make cobalt(per)chlorate and that shows some difficulties. But maybe with an solvent like MeOH, parallel to the coperchlorate prepation.

Philou said that cobalt was as expensive as gold, but I find this untrue. In ceramic supply stores you can easily buy quantities of cobalt salts like CoSO4.xH2O, Co2O3(3+ salt!) and CoCO3. They cost about 6-9 USD/100 g, depending on the cobalt content.
BTW, at the ceramic supply stores you can also buy nickel and coppersalts, quite easily!

Edit: I know now that cobalt will get six NH3 ligands around itself.
So, Co(NH3)6(NO3)2

[This message has been edited by tvs17 (edited October 04, 2001).]

[Alchemist]

Hello all,

Tvs17, check out U.S. patents 6,241,281,and 6,039,820 for info on metallic ammmine complexes like Copper, Cobalt, and Nickel.

------------------

[KZpyro]

I was wondering if Ammonium chloride and potassium nitrate were mixed together with water to make a solution, would Ammonium nitrate and potassium chloride be formed through a double replacement reaction? If so would it be possible for a potassium nitrate/ammonium chloride solution to react with copper to produce TACN?

[kingspaz]

i think that should be possible because the NH4 and NO3 ions will be in solution as in an ammonium nitrate solution. i'm not 100% sure though.

[J]

Whilst searching for info on TACN on google, I found an old post on rec.pyrotechnics. It gave a procedure that consisted of adding Ammonia solution to Cu(NO3)2 solution in alchohol until it turned alkali. I tried this, using 9.5% household ammonia.

I added 10mL of NH3 solution to around 100mL of Cu(NO3)2 solution. This was made by adding 5g of CuSO4 and 6.5g of KNO3 to the alchohol and boiling for 30 minutes.

The results are nothing at all! After a night, most of the solution has evaporated, with no crystals forming. My guess is that the TACN is dissolved in the water from the NH3 solution.

My recent attempts to make TACC have also failed. I've concluded that the air is just too damp at the moment, and the TACC is just absorbing moisture (and CO2, I get CuCO3 forming) from the air. The last time I made it was during the summer. Leaving the solution to evaporate in the house is not an option due to the NH3 <img border="0" title="" alt="[Frown]" src="frown.gif" />

[kromsson]

No one seems to have mentioned it so here it is.
It is easy to make TACN by the kilo, using Ca(NO3)2 which is a very common fertilizer (Norwegian Saltpeter), and CuSO4 which is quite common:

Ca(NO3)2 + CuSO4 -> Cu(NO3)2 + CaSO4.prec.

Prepare a solution of Ca(NO3)2 and CuSO4 (the weights are easy to calculate from mol. weights) and the CaSO4 will precipitate immediately on mixture of the solns.(actually it is like very fine powder suspended in the solution).

After filtering you have a soln of Cu(NO3)2 into which, when you add NH3 soln, you get a beautiful colour transformation (from light sky blue to deep blueof the ocean).

Dry this and get the beautiful crystals.

I have prepared Cu(NO3)2 also by HNO3 directly on Cu wires.

HOWEVER!!

I didn't manage to detonate TACN by the use of HMTD, although TACN was well confined and pressed in a copper tube (usually used for rocket engines), and about 15gr of HMTD used (200gr of TACN).

This is possibly because these salts are actually complexes with water.
I think TACN is actually Cu(NO3)2(NH3)4.(H2O)6
Still, I doubt its explosives properties, as I haven't seen them mentioned in any books.

[DBSP]

I might try the TACN method you described. I have about 25kg of
Ca(NO3)2 and I can buy CuSO4 at an agricultural supplier near me.
I have no idea of where I'll find any NH3 though, I've neve seen it around here, maby a paint shop might have it.

[J]

NH3 is sold as Household Ammonia Water. I've seen it everywhere from hardware stores to supermarkets (it's a general purpose cleaner). You can also generate it as a gas using an Ammonia fertilizer and NaOH.

From earlier on in this thread, Philou mentioned that it must be totally dehydrated to detonate. Try drying it at around 50 degrees C for a few hours, this works with TACC.

Did the TACN just precipitate out? What quantities did you use?

[DBSP]

I know that the pharmacy sells it but I don't think that they have it in stock, you'll probably have to order it and I don't want to do that. The paint stores might have it behind the counter, they shuld have it there. Because I've never seen it in the shop itself. I know they keep the HCl behind the counter so the NH3 might be there to.

In a H2O solution, NaOH+NH4NO3-->NH3(g)+H2O+NaNO3(aq) Is this right? Isn't this kinda dangerous considering the toxity of NH3(g)

[J]

Yes, it is dangerous. And it's pointless for TACN anyway if you can get the Ammonium Hydroxide (household stuff is 9%).

[kromsson]

The TACN precipitated after heating the solution for soome time.
If you heat the TACN in high temp. the NH3 will depart from the complex molecule which is obvious from the VERY strong NH3 smell (there's always that smell on the crystals, but rather weak), and the change in colour from dark blue to light blue.

I am not yet convinced it will detonate.

The quantities were stoichiometric, (even calculated the exact water weight for the water complexes and it worked out alright through the equations), I don't remember exactly, but the final product was about 300gr (HNO3 + Cu) and 1kg (Ca(NO3)2).

[kromsson]

Actually, here's a justified question:

If it was so easy to make TACN, then why aren't terrorists using it often?

There would be nothing left above 30cm from ground at some places, if it was so easy to prepare...

[shooter3]

I'm not sure about this, but I remember reading that TACN should not be pressed into the det. shell. The shell should have about 5 Grams loaded AND be loose in the shell. Also TACC doesn't work unless made without water. With one exception I've not been able to get TACC to work. FWIW.

[J]

TACC is a tricky beast, I've detailed my experiments with it on my website. Preventing water entering the solution from the NH3 generator, coupled with finding a dry area to precipitate the crystals, seems to be the key to success or failure. Drying isn't that difficult.

Some useful info I found on Google:

<a href='http://groups.google.com/groups?hl=en&selm=1994Oct2.094418.12382%40hpcvaac.cv.hp.com'>Some references to papers</a>

<a href='http://groups.google.com/groups?q=TACN+group:rec.pyrotechnics&hl=en&selm=f7.2253.1806.0NFA9FD4%40mpoli.fi&rnum=5'>Procedure taken from chemistry book</a>

<a href='http://groups.google.com/groups?hl=en&selm=01bc72d9%241fd12080%24b06484a9%40default'>Another reference + info</a>

<a href='http://groups.google.com/groups?q=TACN+group:rec.pyrotechnics&hl=en&selm=780555396.102snx%40moonwatcher.avrtech.com&rnum=2'>Mixing with other Oxidizers to increase power</a>

<a href='http://groups.google.com/groups?q=tetramine+copper+nitrate+group:rec.pyrote chnics&hl=en&selm=1992Sep18.180051.20939%40hpcvaac.cv.hp.com&rnum=5'>Evidence of several different complexes, including a Diamine</a>

From these articles:

Explodes at 210 degrees C
Specific Gravity of 1.91
Brisance: 17.2g sand crushed

It seems that it is easily deadpressed, and it will deflagrate unconfined. I assume it needs to be confined loosely in a detonator, like TACC. The last link has evidence of several different complexes, each with varying properties.

[kingspaz]

also from my experiments with TACN it is clear to me that the dehydrated form must be made. the sample i have is still deep blue and has no signs of decomposition which is good since its almost a year old!....not that its much use...maybe it could be dehydrated with calcium chloride or somthing.

[the_unbound]

-

<small>[ May 20, 2002, 06:33 PM: Message edited by: the_unbound ]</small>

[the_unbound]

- please delete -

<small>[ May 20, 2002, 06:35 PM: Message edited by: the_unbound ]</small>

[the_unbound]

Tetramninecopper(||) _______________________ Hexamminecobalt
Nitrate [Cu(NH3)4(N03)2____________________ (|||)nitrate _________________________________[Co(NH3)NO3)3

Color: Dk blue crystals Yel- __________________________________orange prisms
Molecular Weight
255,7 347,2

Impact Sensitivity by
BAM Mehtod with 2kg
Weight, mkg
0,75_________________________ 1

Trauzl Test
10g Sample, cc
240___________________________ 235

Compression Test
By Kast Method, mm
3,2____________________________ 2,8

Detonation Rate,
3500_____________________________ 3000
By Dautriche Methode
2800______________________________ 2700
M/sec

Initation with Cap No.3
positive____________________________
positive
Ditto with Cap No 8
positive_____________________________ positive

Friction Sensitivity
by BAM Method
No action at 12Kg_____________________ No action at 16Kg

Crackles at 16Kg______________________ Crackles at 24Kg

Preperation
By mixing cooled coned
of ammonia,Cu nitrate
or by passing NH3 gas
thru finely pulverized
Cu nitrate


carbon

AMMINE OR AMMONIATE
AND COORDINATION
(Ammoniakat in Ger and Ammoniacate in Fr)
The complex compds in which ammonia
(NH,) functions as a neutral group are very
numerous and frequently very stable. They
belong to the so called “coordination”
compds, known since beginning of the 19th
century but not properly systematized and
explained until 1893 when Alfred Werner
introduced his theory. In his theory, now
nearly universally adopted(with slight modi-
fication, such as by Sidgwick and Lowry,
etc), there are two types of valencies: a)
prirnary (principal, main, ordinary or ionic)
and b) secondary (auxiliary or non-ionic),
now called “coordinate covalence”. The dif-
ference between ionic and non-ionic valences
is not as great as Werner at first supposed,
and is one of degree rather than of kind. The
same kind of anion radical or molecule may
be held by either or both types of valence.
There is, however, an upper limit for both
types of linkages. In case of non-ionic
linkages, the maximum number of atoms,
radicals or molecular groups, which can be
directly connected with central atom(metal),
is called the “coordination number” of this
atom. This number is for most metals six,
but it can be also four, five, three and two
for the same metal(as for instance Co). For
Mo the “coordination number” was reported
to be eight
In writing the formula of a “coordinated
complex”, the "coordinated group”, called
“nucleus” or the “first sphere” is enclosed
in square brackets, while the acid radicals
are placed outside in the so-called “second
or ionization sphere”. For instance in the
formula [M Rm] xn, M is a metal (such as Cd,
Co, Cr, Cu, Fe, Hg, Mn, Ni or Zn), R is a
non-ionic(neutral) radical(such as NH3, H2O,
ethylenediamine, diethylenetriamine, pyridine,
etc), m is “coordination number’; of M, X is
a negative(acidic) radical(such as C 1-, CN-,
NO2, NO3, C103, C104, IO3, etc) and n is
number of monovalent acidic radicals. An
example of this type of complex is the compd
[CO(NH3)6] (NO3)3, in which the electro-
valence of the nucleus is 3 (positive), the
same as for the Co atom. If one or several
NH, groups are replaced by neutral groups,
such as H2O, the electrovalence of the
nucleus remains the same, as for instance
in the compd [co(NH3)5 H2O] (N03)3 If how?
ever, one or several negative(acidic) radicals
replace neutral radicals in the nucleus, the
electrovalence of the nucleus is reduced-
one positive valence less for each negative
valence introduced. For instance in the
compd [co(NH3)5 Cl] (N03 )2 the electrovalence y
of the nucleus is two and in the compd
[CO(NH3)3 C13]0 it is equal to zero. If the
negative valency in the nucleus exceeds
the positive valency of the central metal, as
in the compd [CO(NH3)2 (NO2)4]-K+, the
nucleus as a whole becomes negative and has
to be associated with a corresponding number
of positive ions(such as K) outside
In naming the complexes, the constituents
of the nucleus are taken first(starting with
the acid radical or extra neutral radical, if
any present, and followed by the neutral
group and metal) and then comes the name
of the radical outside the bracket. For in-
stance, the compd [CO(NH3)5 cl] (N03 )2 is
called “chloropentammine cobalt (HI)
nitrate” and the compd [Co (NH3)5 H2O] (N03)3
is "aquopentamminecobalt (III) nitrate”,
etc
Ammonia can form many “coordinated
complexes” with the above mentioned metals
and these complexes, called “ammines” or
‘ammoniates” are among the most important.
Usually divalent metals form complexes with
four NH, groups, while trivalent metals
usually coordinate with six NH3 groups. There
are, however, many exceptions
Many metal ammines are explosive and
those which were investigated in various

countries from that point of view are listed
in tables A, B, C, D, E, F&G
It should be noted that until Werner’s time,
complexes were usually designated by names
denoting color: luteo for yellow, Purpureo
for purple-red and roseo for pink. Some
compds were called praseo to designate
their green color
As a rule, the colors of Co and Cr ammines
are largely independent of the nature of the
metal, but depend on the number of neutral
and acidic radicals. For instance hexammines
are yellow(luteo), chloropentammines are
purple-red(purpureo) and aquopentammines
are pink(roseo). The compd [Co (NH3)4 Cl2]C1
is green(praseo) and the compd [CO(NH3)4-
(NO2)2]C1 is called the /lavo- or coceo salt
Preparation of ammines. Most ammines can
be prepd by passing NH3 gas into a coned
soln of a metal salt, such as chlorate,
iodate, perchlorate, etc, as for instance:
Cd(ClO3)2 + 6NH3 + [Cd(NH3)6] (Cl03)2
CU(Io3)2 + 4NH3 + 2H2o + [cu(NH3)4] (I03)2 . 2H20
co(c104)3 + 6NH3 + H2o+ [co(NH3)6](Clo4)3 . H2O
A detailed description of prepn of hex-
amminecolbalt (III) nitrate is given in Refs
33 and 41 and prepn of some other ammines
may be found in Refs 3,7,9,10,11,11a,12,13,
14,15,16,17,19,20,21,22,24,25,26,30,31,34,
35,40,43,47,48,54,55,56,57,58,59,62,63,and
65
Explosive properties of metal ammines
were studied by many investigators and ref-
erences are given in the tables A,B,C etc
The NavOrd Rept 5639 (1957) (Ref 69) was
not available to be utilized for this work
It seems that the most important ammines
from the point of view of explosiveness and
stability are chlorates and perchlorates. Their
potential energy and velocity of deto-
nation are usually between those of primary
expls, such as MF and LA, and aromatic
nitro compds, such as TNT. The chlorates
are definitely more sensitive than the per-
chlorates, The expln temps of some ammo-
niates were reported to be higher for confined
than for unconfined samples
According to Friederich and Vervoorst
(Ref 11, p 49) the chlorate and perchlorate
complexes decomp with explosive violence,
when heated, and the reactions proceed as
follows:
[M(NH3)4] (c1o3)2+ MCl2 + 2N2 + 6H20
[M(NH3)6] (c103)2 + MCl2 + 3N2 + 6H20 + 3H2
[M(NH3)4] (C1O4)2 + MCl2 + 2N2 + 6H20 +02
[M(NH3)6] (clo4)2 + MCl2 + 3N2 + 8H20 + H2,
where M represents a suitable metal
Uses: Some metal ammines were patented
for use as primary explosives. This ex-
cludes those which are unstable at ambient
temps (evolve NH3) and are too hydroscopic
(See Tables A to G, pp A277 to A282)
References on Ammines: 1) A. Werner,
ZAnorgChem 3, 267-330 (1893), “Beitrag zur
Constitution anorganischer Verbindungen, ”
2) R. Escales, SS 2, 413-14 (1907) [According
to R. Escales, the “Kupfernitrat-Ammoniak”,
listed here in table E as “tetramminecopper
(II) nitrate” and abbreviated as CuTAN, was
proposed in 1887 by A. Nobel, BritP 16920,
for use as follows: a) CuTAN 4, AN 91 &
TNT 5% b) CuTAN 5, NG 30-35, Na nitrate
30.5 & meal 39.5% c) CUTAN 10, NG 48, CC 2,
NaN03 30, WM 9.6 & soda 0.4%. The first of these
belonged to the class of “AN explosives”,
the second to ‘ ‘carbonates” and the third to
“gelatin-dynamites”. The firm G.Roth of
Austria used the compns contg CuTAN 30-40,
K nitrate 42-25, sulfur 10-7.0 & Al 18-28%
for filling some blasting caps] 3)R.Salvatori,
Chem Ztr 1910, 1444 & CA 5, 1568(1911).....

....

Tetramminecopper (||)chlorate: This compd is able to initint. TNT

Tetramminecopper(||)nitrate : purple, ignited by flame but not by fuse
(This sensitve expl. may form by the action of AN on Cu in presence of moisture

<small>[ May 20, 2002, 06:47 PM: Message edited by: the_unbound ]</small>

[xyz]

Has anyone cosidered Tetramine copper permanganate? Could it be possible fo form this?

[Madog555]

im sure u could, the question is if u would want to, NH4MnO4 is supose to be very unstable chemicaly, but not extremely sensitive.

[xyz]

From my experiences with KMnO4 it is a lot more stable than people say, and it has only gone wrong once when we deliberately ground a small amount with some sulphur and magnesium to see if it would spontaneously combust.

[Mr Cool]

I know one of the main advantages of the explosives in the title of this thread is that they're easy to make, which this one isn't really, but:
I've just succeeded in making a few centigrams of what I suppose is di(nitroguanidino)silver (I) nitrate.
I used a very rough method, I just added a few mL of conc. nearly boiling AgNO3 to a few mL of conc. nearly boiling NG solution. When cooled to 5*C, a layer of short, stubby pale yellow crystals had ppted on the bottom of the glass (for some reason the yield seems to suck, I think it must be quite soluble). I've dried a few and ignited them, they burn much more violently than any of the others I've tried. The main portion of the crystals is drying now, I may not have enough for them to make the DDT but I'll try...

[da man]

Sorry to bring up a new topic, but i didn't want to start a new one for this.
Does anyone know if TACC can be made from potassium chlorate, instead of sodium chlorate? I can't see why it wouldn't work, but in the 5 different places i have seen the TACC synthesis, they all use sodium chlorate? Solubility in alcohol isn't a problem so why is it never used?

Also, has anyone successfully used TACN in detonators yet?

Thanyou!

<small>[ July 22, 2002, 12:05 AM: Message edited by: da man ]</small>

[kingspaz]

Na an K are in the same group in the periodic table and compounds of each are often interchanged in industry such as NaCl and KCl. they have very similar properties so changing between NaClO3 and KClO3 shouldn't affect the reaction. you will however need a lower mass of NaClO3 as the Na ion has a lower mass.

[blazter]

Indeed TACC is a tricky beast. Lately i've had some rather vivid dreams that i thought i'd contribute to this thread.

In my dream, i dehydrated a fairly large quantity of copper sulfate pentahydrate (root killer) in a pan on low heat on a hotplate. This was to be used as the dehydrating agent in the drying bottle of the aparatus (very similar to the one described on J's page). Unfortunatly this turned out to be the first mistake (more on this later). The CuSO4 that was actually used in the EtOH solvent was dehydrated by carefully heating in a crusible. 8.5g of dehydrated (white) CuSO4 was added to 360ml of denatured alcohol solvent. 13g of KClO3 was gently heated over a lightbulb to drive off any residual moisture and then added to the EtOH solvent.

I find it interesting that none of the procedures i have read mention dehydrating the CuSO4 which usually seems to come in a blue hydrated form. This seems to be fairly critical because some of the water in the denatured alcohol solvent was sucked up by the CuSO4 forming a light powder blue color. The little bit of the hydrated CuSO4 did not seem to react to form Cu(ClO3)2.

The CuSO4 / KClO3 solution had to sit for about 45 mins while something else was going on, when i returned the solution was a beautiful lime green color. Because it seemed that most of the reaction had already occurred, the solution was not boiled for very long(and besides it smelled REALLY bad)

Another mistake that was made is that the Cu(ClO3)2 solution was filtered warm, and it appeared that KClO3 precipitated upon cooling.

The ammonia generator was a little slim on chemical in hindsight as well. there was only about 56g of NH4Cl on hand(produced by neutralizing household ammonia with HCl) to this an excess of NaOH was added.

the NH3 was bubbled though the cool Cu(ClO3)2 solution, for at least 15 minutes. as the apparatus was working the NH3 generator was producing CONSIDERABLE heat and the drying bottle was also getting very hot. It seemed that the NH3 was being absorbed as well as the water in the drying bottle, by the CuSO4! Never the less some NH3 still managed to bubble through the copper chlorate solution and at around 15 minutes it began to turn a darker purpleish color. Due to time constraints, the apparatus was left overnight and upon returning the copper chlorate solution had turned back to the same lime green color :( . my guess is that the ammonia that had been gained just left the solution as it sat around.

The CuSO4 in the drying bottle had pretty much all turned a purple color, unlike the hydrated form which is more of a blue color. as the media was emptied a VERY strong smell of ammonia was noted and the purple color rapidly dissappeared and it was left a powder blue color. Next time MgSO4 will be used instead because to the best of my knowledge, it does not react with the NH3. Anyone smarter than me care to correct me on that?

Anyways, the copper chlorate solution was left to evaporate and all that was left was a fine, slimely looking precipitate :( .

I've been thinking why not directly add the NH4Cl directly to the copper chlorate solution? would the ethanol not dissolve/ionize the NH4Cl into NH4+ and Cl- ? the whole bubbling process seems to be a horribly ineffiecent process to me. If anyone has any comments/suggestions on how to do this procedure better i'd appreciate it.

[firebreether]

It should be obvious not to use CuSO4 in the drying bottle, as the reason you can form TACanything is because Cu2+ + 4NH3 -&gt; [Cu(NH3)4]2+

[Polverone]

Recently I've been preparing different metal nitrates from ammonium nitrate and the corresponding metal carbonates or hydroxides. With some metals this works fairly well just in hot concentrated aqueous solution. With other metals I have used molten anhydrous NH4NO3 (all experiments so far conducted on very small scale). I have found that "copper carbonate" from a ceramics supplier dissolves with a little bubbling and not too much difficulty in molten NH4NO3 to make beautiful blue liquid. When solidified, this material did not behave differently from pure NH4NO3, so far as I could tell (simple burning tests), likely because of the relatively low amount of copper nitrate/TACN in the mass.

While experimenting with bizarre pyrotechnic formulas lately I tried a mixture of (coarsely) powdered NH4NO3, 300 mesh Al, and CuO. I was hoping for a shortcut to a decent green flame. It burned, and gave a nice green flame, but it burned very irregularly, with violent popping, until it blew itself out with a loud pop. On reignition it did the same. I'm guessing this is because of local sensitization of ammonium nitrate by copper compounds formed in situ, or even TACN formed in situ. Or some bizarre combination of factors. Some time I'd like to try a mix like this with a detonator. With a core of a more reliable mixture to keep it going, it might actually make a decent pyrotechnic effect, but I'm not sure it is safe.

I've seen some different patents that used small amounts of copper salts to sensitize ammonium nitrate for explosives. So far all of the patents I've seen (sorry, didn't write down the numbers) specified just mechanically mixing a small amount of the sensitizing salt in with the material. It seems to me that you could get the most intimate mixture possible by melting the AN and then introducing the salt, pulverizing the solidified mass, and continuing as usual.

[tmp]

Copper nitrate is easy to prepare from copper sulphate and calcium nitrate.

Here is the reaction:

CuSO4 + Ca(NO3)2 --> Cu(NO3)2 + CaSO4

In this metathesis reaction the relatively insoluble
calcium sulphate precipitates out of the solution.

Filter out the calcium sulphate.

Evaporate the solution to get dry copper nitrate.

Grind up the dry copper nitrate and place in
anhydrous alcohol.

Run the ammonia gas generator through this
solution.

This will produce TACN.

[DBSP]

If you had read the whole topic you would have noticed that what you mentioned already has been discussed. Except the fact that you use NH3(g) instead of liquid ammonia.

[blindreeper]

Would TACN provide the same primary explosive properties of TACC? I have masses of CuSO4 and Ca(NO3)2. I would like to have another primary other than AP or just somthing more exotic and just to say "hey I have made that!"

[DBSP]

When reading this thread you notice that if any very few people have managed to detonate it. I've made it once and I still have a sample left of it. It doesn't burn very well but if subjected to a hot flame it burns with a bluish flame.

The problem semes to be that it as stated elswere in this thread formes complexes with water which makes it very hard to detonate.

[Kid Orgo]

If I'm not mistaken, earlier in this thread there was mention of silver styphnate is less sensitive than mercury styphnate, where in the case of silver fulminate vs. mercury fulminate, the reverse is true. Why is this? Or am I mistaken?

[tmp]

To DBSP:

I read the entire thread before posting. I'm sorry if
I offended or bored anyone. It seems I need to
read the threads more carefully.

The post demonstrates a simpler method for
manufacturing Cu(NO3)2.

I use ammonia gas to limit the formation of copper
hydroxide. While not totally dry gas, it reduces the
amount of Cu(OH)2 that is precipitated.
Ammonium hydroxide produces much more.

My research can be expensive and I want to keep the
costs down.

In response to another post inquiring about TACN:

Reference: CRC 52nd Edition 1971 - 1972

Name: Copper (II) tetramine nitrate
Formula: [Cu(NH3)4](NO3)2
Atomic Weight: 255.67
Crystal color/shape: dark-blue, octagonal
Density: 1.91
Melting Point: decomposes 210C explodes
Solubility in Water: Soluble at all temperatures

Take it with a grain of salt because even the best sources of
information can be inaccurate.

[bubbling_beaker]

hi i had made a post describing my accidental making of TACN and was told off for it so i removed it but i think it is appropriate to bring back to life so i will.
i was trying to dehydrate AN on a pan which contained copper in it and then the AN melted and started going green then eventually went a dark blue and then i stopped the flame and scraped some of this blue salt out and burnt it on a large flame then it started to bubble and fizzle and made the whole flame green so i got happy because i thought i made Cu(NO3)2 and thought i could use it in certain coloured comps so i attempted to make more and repeated the process described but this time i let the AN react with the pan for too long and then it started to fizz and and i smelt the formation of NH3 and the reaction was getting very feirce so i just dumped some water on it and it ceased. Now i read this topic and another concerning TACN and now i know that i had TACN forming and alot of it and therefore this method could be used to obtain good results by eg the slight addition of water to make a viscous slurry and advisably exess copper powder then adding more water and filtering and drying off the filtrate..the possibilities are great what do you think? could this way help avoid the problem of the lack of oxygen? feed back will be nice , thanx
-bubbling_beaker-

[kingspaz]

let me quote DBSP 'The problem semes to be that it as stated elswere in this thread formes complexes with water which makes it very hard to detonate.' thus the use of water in its preparation must be avoided.
the use of water will not work for another reason, the AN melts at a much higher temperature than water boils at.
also, can you please not construct ridiculously long sentences otherwise people will get pissed off reading it.

[Ollie Snowie]

I read somewhere about adding sawdust to flash in large firecrackers to make them burn faster (I'd have thought it would do the opposite). Anyway, I was wondering if you could do the same thing to TACC and it's relations to prevent them from deadpressing. Sort of like microspheres but more accessible to newbies. Or else you could dissolve the salt in something other than water, soak it into cotton wool and let it dry. the question is, Would this work? I haven't had much success with any of these salts so I can't try it for myself. If one of the decomposition products is copper oxide then the cellulose rich filler would reduce it, making CO2 and water vapour, adding to the gas volume and increasing the intensity and maybe speed of the shockwave. I'll try it when I get some more reagents.

[kingspaz]

i think TACN is a bust. even if it could be prepared in its anyhdrous form i doubt it would have any useful pwer output. the main problem with TACC isn't its dead pressing but rather preparing it anhydrously as in making TACN. in my opinion these explosives only warrent interest for messing about with and not actual use. there are easier and much more powerful primaries to make.

[Ollie Snowie]

O.K, Here's what I did:
Last weekend I made a small methylated spirit burner with a coil of platinum wire above a wick soaked in methylated spirits. I lit it, and when the platinum was red hot I gently blew it out. The wire carried on glowing from the heat given out by the calalytic oxidation. I then suspended the entire setup inside a coke bottle and put some ammonia water in the bottom of it to see if it would make NO2. Alas, I only noticed the horrible smell of NH3 - no NO2. I think the concentration of the ammonia was too low, or the ammonia could have neutralized the NO2. I'm a pessimist, so I chose the first option, where no NO2 was formed in the first place.
I then left the bottle for a few days and, when I retunned, the entire (copper) tube that was holding the methylated spirits was blue! I scraped some of the blue coating off and burned it - it fizzed and made sparks - just like the TACN I made before, however, when wrapped up and heated, nothing happened. I took more of these crystals and roughly mixed them with an equal volume of potassium nitrate, wrapped the mixture up, and heated it again. This time it fizzed like it did in the open air, but more violently. This leads me to think that I made tetraminecopper ethanoate.
I am currently doing a test with copper penny left in a bottle of ammonia water and methylated spirits, which I open every day to let air in. Every day, just before I open it, I notice that the sides of the bottle are collapsed, and I hear a small hiss every time I open it. The solution turned a deep blue colour in the first day and the colour is still getting darker.
I will do more tests, with:
A) copper and methylated spirits.
B) copper and ammonia water.
C) copper, ammonia water and platinum catalyst.
D) copper, methylated spirits and platinum catalyst.
E) copper, ammonia water, methylated spirits and platinum catalyst.

[EDIT - Tetraminecopper ethanoate or whatever was formed here does not seem to be hydroscopic, but still behaves like anhydrous TACN when mixed with potassium nitrate and burned.]

[Dr_Pind]

I wasn't able to determine whether TACN was hygroscopic, or if it was only containing crystal water.
Does the TACN precipitate when formed?
In other words; is it possible to precipitate TACN hydrate out of an aquatic solution, so that one wouldn't have to boil of excess water to precipitate the TACN?

[tmp]

I read somewhere on the web that TACN is sometimes used in detonators
because it is relatively inexpensive to manufacture. I have to agree with
Kingspaz that it is probably a bust for most applications because other
primaries such as acetone peroxide are more easily made. Even the method
I'm using with ammonia gas and anhydrous alcohol presents problems
because it's a bitch to keep water out of copper nitrate. Time to move on !

[Rosco Bodine]

TACP is easily made by mixing a warm concentrated solution of copper nitrate with a warm concentrated ammonium hydoxide solution of ammonium perchlorate .TACP is a moderately sensitive secondary explosive which has good power and good stability so long as the material is kept from contact with liquid water . TACP is not at all hygroscopic and will remain stable exposed to the air outdoors even during rainy weather so long as it is not directly wetted by condensation or liquid water . On contact with liquid water TACP is decomposed immediately and uneventfully by hydrolysis . TACP crystallizes directly from synthesis in a desirable crystal form and purity . The crystals are very beautiful in color , an intense deep sapphire blue quite similar to granulated "cobalt glass" , very reflective and prismatic crystals . The synthesis of TACP is actually worth doing just to see these sparkling little beauties which are distinctly unforgettable . Many years ago I made a batch of TACP and I still remember the jewel-like beauty of TACP crystals , blue-violet cubes having a granulation size similar to table sugar . Upon ignition in the open the TACP deflagrates and produces a bright "electric blue" blue-white colored light . The TACP crystals can be compressed in a detonator capsule and intitiated by a primary . TACP is slightly more sensitive to initiation by lead azide than is picric acid , and is nearly as powerful . Warming the dried TACP crystals in a beaker heated by a hot water bath , sufficient to melt paraffin chips , the warm TACP crystals can be stirred with a dowel and glazed with molten paraffin to form a compostion which is optimum at 2.75 per cent paraffin . The warm mixture is dumped onto a paper plate for cooling , and the cooling paraffin glazed crystals will separate easily . This percentage of paraffin was found by experiment to improve the sensitivity to initiation of TACP and to improve its compression loading characteristics , as well as to provide an improved resistance to moisture .

Synthesis of Tetraammine Copper ( II ) Perchlorate

EXPERIMENTAL :

120 grams of ammonium perchlorate and 280ml of ammonium hydroxide 26 degrees Baume ,( 28-29 per cent of solution weight is NH3 ) are combined in a glass jar of 800ml capacity ,having a threaded lid , and the container is lightly sealed , but not so tightly as to prevent a slight leakage of any excess pressure of ammonia as the ammonia solution is heated . The solution of the ammonium perchlorate will require placing the jar into a pan of hot water , and warming and stirring will dissolve all of the ammonium perchlorate . This can most easily be accomplished using a magnetic stirrer , avoiding the fumes of ammonia which will be evolved if the container must be opened for manual stirrring . Periodically swirling the sealed container is another option . While the mixture is warming and dissolving , prepare a solution of copper nitrate according to the following method .

Place 56 grams of basic copper carbonate into a 500 ml beaker and add 25 ml water , stir into a paste . Add dropwise , with stirring , cautiously and slowly due to effervescence , 68 ml of concentrated nitric acid 68 per cent . A dark blue transparent , hot solution of copper nitrate will result when all of the acid has been added , and the evolution of carbon dioxide has ceased . By the time this copper nitrate solution has been prepared , the other solution of ammonium perchlorate should be fully dissolved .

Remove the ammoniacal ammonium perchlorate solution from the warm water bath , and place it in a cool water bath . When the temperature of the ammonium solution has lowered somewhat , loosen and remove the lid and while stirring quickly pour into the stirred solution the warm copper nitrate solution . A strong evolution of ammonia will accompany the immediate exotherm as the complexation reaction occurs . The temperature of the dark purple colored reaction mixture will suddenly rise to nearly the boiling point while offgassing a lot of excess ammonia . Allow a minute or two for the excess ammonia to fume away and the temperature to begin its fall , then cap the container snugly to prevent further loss of ammonia . The reaction is rapid and within a few minutes a substantial precipitation of TCAP crystals will begin to appear in the gradually cooling mixture . The hot reaction mixture should be allowed to stand without stirring for no longer than ten minutes , or very large crystals will appear , 4 to 5 mm cubes will grow at an astonishing rate in the mixture unless it is stirred up very well at least every three or four minutes while cooling . Ice should be added to the cooling bath to increase the rate of precipitation . With regular stirring of the cooling mixture nearly all of the precipitated crystals will be produced in a surprisingly uniform crystal size , which is easily filtered from the mixture when the precipitation is complete . It is imperative that the crystals not be rinsed with water . Alcohol may work okay but has not been tried . The TACP crystals are not themselves hygroscopic , however the reaction liquid which wets the freshly filtered TACP crystals IS very hygroscopic and must be blottered away from the crystals as much as possible , or else the atmospheric moisture attracted to the residual "mother liquor" will begin to decompose the TACP . It is essential to get the freshly filtered TACP crystals free from the residual moisture within a few minutes , and this is easily done by simply placing the coffee filter on a fresh stack of dry paper towels until the filtered crystals are substantially free of liquid and only slightly moist , no longer like a wet "mud" but more like a freely crumbling "damp sand" of loose crystals . The crystals should then be spread out in a thin layer upon paper to air dry . Yield of dried crystals is 115 grams , about 72 per cent of theory .

There is a color shift about the crystals which will be observed occurring from the time the crystals are first filtered from the reaction , and when the crystals are completely dry .The freshly filtered crystals are a darker violet blue sapphire color , and the finished drying crystals are a distinctly lighter and brighter blue very much like "cobalt blue" . The color change is accompanied by loss of ammonia , which suggests that the initial product is partly or fully the hexammine complex , which reverts to the tetraamine complex on exposure to the air by loss of ammonia .

The above procedure is not optimized , so the yield may be improved by refining the proportions or method . This synthesis is simply reported as being one approach which does produce usable yields of crystalline TACP suitable for use as an explosive . The potential usefulness of TACP has not been the source of extensive experiments by me , but it may have usefulness with nitromethane or other energetic fuels , due to its positive oxygen balance . The ease of synthesis of TACP makes it interesting . The effectiveness of TACP as a detonator base charge has not been tested by me on actual charges . The comparison to picric acid relates to witness plate observations for two gram charges initiated by lead azide . A better real world test of detonator effectiveness would be to see how efficient two to three grams are at initiating lightly confined urea nitrate .
In my experience , only a "persuasive" detonator impulse gets that job done well .

[Marvin]

Nows thats a post for sore eyes.

I would think what youve made is specifically tetraaminocupric perchlorate dihydrate. This should be dark blue, low solubility. I would speculate that the lightening of colour is due to hydrolysis at the surface of the crystals, or maybe just to loss of ammonia.

How sensitive is this to shock, crushing, grinding etc? Do you have problems if the crystal sizes get too big or are you basing this on properties of other primaries?

[Rosco Bodine]

Could you please cite the specific reference for the existence
of this hydrolysis senstive material as a dihydrate when speculating ?

The product shows no loss of moisture on heating , BTW .

The material is relatively insensitive to crushing or cautious grinding .
It is sensitive to impact and initiation , somewhat more than picric acid .

PATR rates its power somewhat lower than is in accordance with my personal
observation . The figures I would have to check , but IIRC the figure given
by PATR was about 80 per cent of TNT in power , I would put it somewhere
between TNT and picric acid in brisance based upon the size of the hole
blown through steel by two grams in a cap base charge .

There will be a few megacrystals formed from the supersaturated hot reaction mixture just before an avalanche precipitation of much smaller crystals of uniform size . This is no significant problem . I simply made the observation that the more desirable mesh of crystals for use as an explosive are easily obtained by stirring of the cooling reaction mixture . If you want a great many larger crystals for some reason , then let the mixture sit undisturbed while cooling and bigger crystals you will see there .

Solubility is an irrelevant term for TACP , because on contact with liquid water TACP decomposes completely to copper oxide and other things . So there is no real "solubility" for TACP in water , as it is decomposed on contact with water .

TACP is definitely not a primary explosive , but is a good
secondary high explosive .

[Marvin]

The brief description in Mellor matches the compound youve described well, though there is a typo in the name. The one reference given for the compound is, coincidentally enough,

H. E. Roscoe, Liebigs Ann., 121. 355, 1862.

It is sparingly soluable, or it wouldnt ppt under the conditions youve described, the fact that pure water decomposes it isnt surprising. From other examples we know that anhydrous tetraamino copper(II) compounds do not form from Aq solution and that the usually dihydrated salts that do form, as this is I'm sure, always lose either ammonia or ammonia+water on attempted dehydration. The only way to make the anhydrous compounds involves anhydrous salts and dry ammonia gas, or presumably liquid ammonia.

We know the tetraamine copper(II) complex cannot be the light blue compound, because tetrahedral copper (II) has to be darkly coloured for symmetry reasons. This is the 'real' reason behind why adding excess ammonia to copper sulphate solution turns the mixture dark blue/purple. The octahedral water complex has a symmetry forbidden transition in the visible region, which is why it only absorbs very weakly. Add ammonia and allthough the ligand changes it shouldnt affect the absorbtion bands that much, but becuase it forms a tetrahedral complex instead, the same transition is now fully allowed by tetrahedral symmetry and the solution becomes very strongly absorbing.

From your description of deflegration in the open I assumed it would go high order when ignited strongly confined and thus make a useful primary explosive, does it not do this?

[Rosco Bodine]

Marvin ,

Regarding the DDT capabilities when strongly confined , actually I did
not test for that . In the open even several grams ignited merely burn ,
although the burning is quite rapid and makes a crackling snapping growl
of a noise , as if the potential for transitioning could be there . I think
I did test it with light confinement in an open tube and it merely flashed
like rocket propellant . It appeared to be a rapid enough burn that no
nozzle would be required , just an end burning grain in an open tube
would probably do the trick . I think it would probably DDT but the
size of the charge would probably be large , but that is just my guess and
it might go DDT beautifully with strong confinement . When I was stepping up
the initiating weights of lead azide to quantify the sensitivity , there were
incomplete detonations with a couple of the tenth gram initiating charges .
That would seem to be plenty of azide to get a DDT capable material to go
high order in a cap casing if it just needed a bit of confinement to go . Since
that didn't happen , I would say that the DDT capabilities are not present for
a detonator sized charge . Bigger charges could cook off nicely , just like
regular ammonium perchlorate can do .

It is good to keep in mind that when syntheses are done for publication ,
samples of proposed materials are often made by awkward methods merely
for the purpose of justifying a particular identification by using methods which
exclude other possibilities . These methods are used for producing what are
most certain to be "authenticated samples" as standards for comparison .
But the anhydrous methods used on those references never can be taken to
mean that the same material can't also be synthesized under much less
restrictive conditions . I believe that to be the case here with my proposed
synthesis . The product is soluble in the ammonium hydroxide solution of
precursors from which it forms and the byproducts of the reaction ,
and indeed there is water in that solution . But that reality cannot be taken
to indicate that the TACP is therefore "soluble in plain water" nor can it be
speculated that because a substance crystallizes from a water containing
solution of precursors that it must be a hydrated salt . Directly observe
the absolutely instantaneous decomposition of TACP crystals upon contact
with plain water and you will see why it is unlikely that the compound actually
contains that same water which is its own destruction if one more bit of it tips
the stability balance .

A more modern reference is B.B. Wayland and W.L. Rice
Inorganic Chemistry vol 6 , No. 12 ( Dec 1967 )
pg 2270-2272

If it isn't really TACP , how about we just call it
"pretty purple 'splosiv stuff" :D
or , we could split the difference and call it
copper pentaammine perchlorate maybemonohydrate .

[Zeitgeist]

Interesting.....

So, let me get this straight, using CuSO4 solution in EtOH, we dissolve in a nitrate or permanganate at a 1:2 mol ratio and bubble in NH3 ?

Or do i need to start from Copper Nitrate ?

So do you need NH3 gas? Could you use, say, (NH4)2SO4 and NaOH in the solution?
How about crappy household ammonia solution?

I'm really only interested in the Nitrates and Permanganates, chlorate is a bitch to get here.

[Mumble]

Actually refluxing has to be done. Just heating and replacement of boiled EtOH is acceptable. The copper salt formed will dissolve into the alcohol. Filter to remove excess Copper sulfate or x Sulfate. I don't know about the other salts, but the Chlorate turns the alcohol solution neon green. Quite a neat color.

For the best product Ammonia gas has to be used. Also all reagents should be quite dry. Water kills any use the compounds may have. One may want to keep them under solvent until they are to be used. Ammonia solution can be used, but like it says, water kills the usefullness. If you just want to make them for bragging rights use Ammonia solution by all means for ease and lower risk.

If you do want to use the compound actually, might I recomend decomposition of Urea. It it quite dry just by itself. No wash bottles needed.

[Zeitgeist]

OK , I've got some solid copper nitrate now, which is good,

Does having water present just make it less able to detonate because it is so hard to dry, or does it stop the complexation by complexing itself to the copper?

I added 5% aq. ammonia to Cu nitrate, got Cu(OH) which then dissolved to the rich blue colour tetramine complex - but when i started boiling it i just ended up with brown Copper Oxide precipitate.

Also, i tried mixing KMnO4 and CuSO4 to make Cu(MnO4)2, 2:1 mol ratio in aqueous solution, but black-brown Copper Oxide and/or Mn(IV) oxide precipitated out, any ideas how i can make this ?

[Marvin]

Mixing ethanol and permanganate would not be a good idea.

Water forms a complex, which is all hydrates salts really are.

If you make copper nitrate in aq solution this will be hydrated, it is not possible to dehydrate this to make the anhydrous salt. If you use dry ammonia though you can make the anhydrous ammonated salt.

Copper sulphate doesnt dissolve in alcohol.

I have doubts about the feasability of making amminated permanganate compounds, do you have a reference or is this speculative?

[Hubert]

This is movie- 200g [Cu(NH3)4](NO3)2 tetraamino copper nitrate TACN

http://www.pirotechnika.one.pl/Proby/[Cu(NH3)4](NO3)2.mpg

I dont smell NH3 in TACN.
This is very persistent and look good.
We can see more in this video.

[Rosco Bodine]

I have doubts about the feasability of making amminated permanganate compounds, do you have a reference or is this speculative?


http://mihailru.freeservers.com/

The page will only display correctly with your browser
using UTF-8 decoding , and the language plugin for cyrillic characters ,
as the page is in Russian .

[kryss]

I've found Copper Nitrate difficult to prepare pure - easy enough to make a conc solution but its so soluble you end up with a thick syrup when you try to evaporate off the water. Heating it more just gives off nitric acid - producing a basic nitrate. I probably need to add a solvent to reduce its solubility - but i suspect its reasonably soluble in methanol and isopropanol as they didnt seem to do much. Plus I've read that Copper can form adducts with alcohols - in Mellor. Took a sample aount of the solution and added excess ammonia and precipitated with isopropanol - lots of purple solid. I think this is one of the copperammine nitrates, but probably not fully ammoniated or nitrated. Air dries easily enough - doesnt smell strongly of ammonia but melts//burns then goes up in a puff of smoke - more smoke than anything else.Interesting though.

I'm trying the Copper Chlorate - 4g CuSO4.5H2O and 3g KClO3 refluxed in a milk! bottle with Methanol. Solid loses the blue colour, liquid goes apple green colour. This might be due to the water in the copper sulphate being extracted into the methanol, and excess methanol complexing with the Copper. Should be easy enough to tell.

[Macgyver]

Has anyone here successfully used TACN to initiate something else, for example ANNM?

I have made some TACN, but it seems that I need something else to initiate the TACN, because on its own it is not particularly flame sensitive.

Maybe mixing part of it with black powder would work?

[KemiRockarFett]

According to the subject Tetraamminecoppernitrate, than you add ammonia to the water solution of coppernitrate the ammonia will become a stronger induced dipol, due to coppers elektronegativity, than water is dipol and therefore the ammonia complexbonds to copper and as you have noticed the colour will be dark blue and that Marwin tried to explain with MO theori.
Then you have your Tetraamminecoppernitrate you suspect it to have two crystalwater left and if it is in that way its no problem at all. In Federoff you can read that the substance was used with aluminum and KNO3 and sulfur and I think carbon in blasting caps. The eventually crystall water will react nicely with the aluminium and give a lot of energy.
Summary: dont try to use the complexsalt as it is, use it in a mix and the result is a perfect sheap safe and easy blasting cap.

[meselfs]

I've found Copper Nitrate difficult to prepare pure - easy enough to make a conc solution but its so soluble you end up with a thick syrup when you try to evaporate off the water. Heating it more just gives off nitric acid - producing a basic nitrate. I probably need to add a solvent to reduce its solubility - but i suspect its reasonably soluble in methanol and isopropanol as they didnt seem to do much. Plus I've read that Copper can form adducts with alcohols - in Mellor. Took a sample aount of the solution and added excess ammonia and precipitated with isopropanol - lots of purple solid. I think this is one of the copperammine nitrates, but probably not fully ammoniated or nitrated. Air dries easily enough - doesnt smell strongly of ammonia but melts//burns then goes up in a puff of smoke - more smoke than anything else.Interesting though.

I'm trying the Copper Chlorate - 4g CuSO4.5H2O and 3g KClO3 refluxed in a milk! bottle with Methanol. Solid loses the blue colour, liquid goes apple green colour. This might be due to the water in the copper sulphate being extracted into the methanol, and excess methanol complexing with the Copper. Should be easy enough to tell.
It has a suprisingly low melting point, around 150 C (can't remember exactly but definitely around there). Around 220 C it decomposese.
So, try putting a thermometer in and keeping the temp around 180, hold it there for a bit and it should be totally anhydrous.

[hereno]

Has anyone ignited TACC out in the open? how does 1g burn unconfined?

TACC is said to be the only common complex that will function as an initiating explosive, so it would be nice to give other complexes something to scale them by. How much is required for unconfined detonation?

[TheArsenist]

Ha, I've just boiled some Cu powder in a HNO3 solution for a couple of hours to make Cu(NO3)2. I thought about making it by boiling Cu powder in a NH4NO3 solution, and that was before I knew that Cu(NO3)2 combined with NH4 formed an explosive :) Good thing I went with the HNO3 solution.
I just want to make cu(NO3)2, and I saw that somebody said that its possible to make by mixing CuSO4 (aq) with Ca(NO3)2 (aq). Are you shure about that? What color is the solid that forms in the mixture? I believe that you need someting like AgNO3 in order to make CuSO4 into Cu(NO3)2.
Are you shure its possible to make a cu(NO3)2 solution just by mixing Ca(NO3)2 (aq) and CuSO4 (aq) and filtering out the white and solid CaSO4?
I don't have any Ca(NO3)2 at the moment but I have plenty of Mg(NO3)2 so would that work aswell? Probably not since MgSO4 has a high solubility in water. Which other procedures of making Cu(NO3)2 do you know?

[The_Rsert]

Has anyone information about tetraminecopper persulphate?
(Soloubility in water and alcohol, information about synthesis?)
I have just seen the video on http://www.geocities.com/roguemovies7/
It looks powerful...

[Marvin]

Did it take 2 weeks for someone to authorise TheArsenists post?! I'm a little confused.

I dont follow why you needed to boil the copper in the acid. The last time I tried dilute nitric and copper it merrily dissolved producing NO.

Mixing solutions of copper sulphate and calcium nitrate will work, but beware that garden fertiliser grade calcium nitrate often also contains some ammonium nitrate. One wonders if thats what its made from. The precipitate should be white calcium sulphate, leaving copper nitrate in solution.

You cant make anhydrous Cu(NO3)2 by any process using water. The hydrate will be made which decomposes if you try to make it anhydrous. TACN can be made anhydrous using dry enough ammonia from the hydrate as stated allready.

If you are stuck for calcium nitrate, mixing sodium or potassium nitrate with calcium chloride as hot concentrated solutions and filtering still hot should dump out NaCl or KCl. By working out the math, how much sodium nitrate to calcium chloride, and what volume of liquid you need to keep most of the calcium nitrate produced this should work. You can then use calcium nitrate to produce the copper nitrate in the cold. Filtering will be a pain, use more water than you need and resign yourself to a longer concentration step at the end. My copper nitrate was a blue solution when cold and dilute, and green when hot/concentrated.

I dont know if magnesium nitrate will work, it depends on if copper sulphate (low solubility) or magnesium sulphate (fairly low solubility) will crystalise first.

[The_Rsert]

Tetraminecopper(II)persulphate is quite powerful,
not hygroscopic, sensitiv flame to shock an friction.

Preparation of tetraminecopper(II)persulphate:
1.)Dissolve 20g copper sulphate in 100ml of warm (not cooking) destilled water.
2.)Add 45-50g strong (25%) ammonia and wait a few hours.
3.)Make an other solution, with 20g potassium- or sodium persulphate in about 400ml (maybe less water is better) warm water.
4.)Mix the two solutions and wait some hours.
5.)Cool the solution to 0°C-2°C.
6.)Filter out the little purple needles.
7.)Dry them in an desicator until it's 100% dry.

[Marvin]

I'm not convinced any explosive that leaves a noticable post detonation residue can be considered 'quite powerful'. If its remotly powerful it should reduce itself to vapour/gas rather completely and distribute itself over a wide area.

Compaired to TACC or TACN it has a lot of reducing groups, a lot of dead weight and a single peroxide bond providing all the oxidising power. Looks like a dead loss to me in engineering terms.

[The_Rsert]

Tatraamincopper(II)persulphate synthesis with some pictures:

http://members.fortunecity.de/potatoguns/TACPersulfat.html

More pictures coming soon, until I have a new camera...
(this camera was only borrowed)

[The_Rsert]

Is bisethylenediaminecopper (II) nitrate better than the normal TACN?

Synthesis:

Bisethylenediaminecopper (II) Nitrate

1.Dissolve approximately 4 g of well pulverized Cu(NO3)2 • 3H2O, weighed to the nearest 0.01 g, in 25 ml 95% ethanol in a 250-ml beaker. Cool the solution in an ice bath.

2.Add, with constant stirring, about 3.0 ml anhydrous ethylenediamine, C2H4(NH2)2, to the ice cold solution in step 1. Ethylenediamine stinks and is very hard on skin, therefore use under the hood and take care!

3.Suction-filter off the violet-blue product, using a Büchner funnel.

4.Wash the product with two 20-ml portions of ether (CAUTION: ether is very flammable, make certain no open flames are in the vicinity). See the special sheets on recrystallization for proper washing techniques. Weigh the air-dried crystals for the purpose of estimating volume of solvent needed for recrystalization.

5.For recrystalization use a solution in which the proportions are 4.0 ml distilled water added to 100 ml 95% ethanol. You will need approximately 50 ml of this solution per ram of product to be recrystalized, so prepare a volume of ethanol-water solution somewhat in excess of that calculated for the weight of product obtained in step 4. Start out with about 40 ml of the ethanol-water solution per gram of product, and, with vigorous stirring, heat it quickly to boiling on a hot plate that is already up to temperature (setting about 4?). Once the boiling point has been reached, add small additional amounts of solvent so as to maintain the solution at its boiling point until the product just dissolves. Avoid a really prolonged period of boiling because this vaporizes the ethanol faster than water, and as the solution becomes more concentrated in water, the yield on recrystalization goes down. Because of the intense color of this solution, you may have to occasionally decant off the hot solution into a separate beaker in order to tell whether or not the crystals have dissolved; if they have not, pour the solution back into the beaker and add more solvent and heat. Repeat until the crystals just dissolve. Cool the solution to about 0ºC in an ice bath and leave at this temperature for as long as practical, then suction-filter off the crystals.

6.Dry the crystals in air. They may be left in your desk over the week spread out on a watch glass, or dried for half an hour in the oven at 55ºC.

[Jacob Kell]

As tacn could be realy easy thing to make, i would like to know how toxic it is? I didnt see anywhere in this thread evena a word about that. I am sorry if it has been answered. I wonder about AN solution/copper wire method? Are there any toxic gases produced in reaction? and the other thing, is it possible to dry it well without hard-to-get chemicals?

[The_Rsert]

I think that all the ammonia complexes are almostly harmless.
For example my tetrammine copper(II)-persulphate is inreaktive and will leave only some NH3(gas), water(gas) and copper(II)-sulphate (gas and solid) after the explsion. Only the last can be dangerous, because the copper(II)-sulphate can condense in your lungs which will be harmful.

But I think, that the hydrazine complexes are much more poisonous.
Also the ethlenediamine complexes are poisonous but not strong as the hydrazine complex salts.

Anyway, be careful, don't eat it, don't inhale the dust of it, use gloves and eyeglasses.

You can see some pics of the cupper(II)-sulphate condensation here:
http://members.fortunecity.de/potatoguns/TACPersulfat.html

[t3sla_trooper]

I'm not convinced any explosive that leaves a noticable post detonation residue can be considered 'quite powerful'. If its remotly powerful it should reduce itself to vapour/gas rather completely and distribute itself over a wide area.

Compaired to TACC or TACN it has a lot of reducing groups, a lot of dead weight and a single peroxide bond providing all the oxidising power. Looks like a dead loss to me in engineering terms.

Is i possible to put another peroxide group to that molecule to make it more powerful?

[DONMAN]

Sorry to revive a dead topic but I have an odd occurrence. I was making some TACN with ammonia nitrate and copperII chloride. I added some hydrogen peroxide as a catalyst. The peroxided then catoliticaly decomposed. There was no liberation of chlorine. About an hr later there was some brown precipitate in the tube. I can't figure out what it is, although I have yet to filter it. I was thinking maybe the peroxide and the chlorine formed a chlorate complex. That doesn't even make sense because it would be soluble unless it was saturated solution or some unforeseen impurity in my ammonia nitrate.

Any thoughts?

[dhemor_]

Sorry about the dead thread folks, but hey, tetramine copper complexes are some things I've been working at lately..
For those interested in tetramine copper persulphate, it's mainly useless. It burnt quickly unconfined, but when put in a cap I found it useless.. There was a very very weak pop.. I had used a straw, and although some of it was burnt, the only other significant damage was a few cracks..
I'll make some more soon - new job coming up.. Money! - and I'll put a video up.
For those interested, here's a vid of the deflagration of tetramine copper permanganate.. It left a very 'stringy' residue.. A better video will be put up when I get the chance.
http://youtube.com/watch?v=zWT6IwMONJA

[351q]

Sorry to revive a dead topic but I have an odd occurrence. I was making some TACN with ammonia nitrate and copperII chloride. I added some hydrogen peroxide as a catalyst. The peroxided then catoliticaly decomposed. There was no liberation of chlorine. About an hr later there was some brown precipitate in the tube. I can't figure out what it is, although I have yet to filter it. I was thinking maybe the peroxide and the chlorine formed a chlorate complex. That doesn't even make sense because it would be soluble unless it was saturated solution or some unforeseen impurity in my ammonia nitrate.

Any thoughts?

Seeing as the thread already has been revived, I'll just note a similar thing occurred to me. I was performing electrolysis of a saturated ammonium nitrate solution with a copper anode and cathode at 9v, 200mA, trying to produce tetra-aminecopper(II) nitrate. I mixed in hydrogen peroxide in attempt to increase the rate of copper hydroxide formation. The H2O2 decomposed and I believe the same brown precipitate formed. I kept the solution but took an older batch of [Cu(NH3)4][NO3]2 and mixed it with hydrogen peroxide to isolate any variables (no copper hydroxide, electrodes, etc.) but the same reaction occurred. Since my reaction involved no chlorine or chlorine salts, it must be something else. I was thinking an oxide, CuO2 maybe, until I dried out the solution and the TACN recrystallized perfectly fine. Here are pictures of the powder, unknown solution and blue-green precipitate that formed after half a week. Maybe this could be a positive test for TACN in the future?
http://i166.photobucket.com/albums/u113/lt_penguin_david/PIC_0116-1.jpghttp://i166.photobucket.com/albums/u113/lt_penguin_david/PIC_0113.jpghttp://i166.photobucket.com/albums/u113/lt_penguin_david/PIC_0114.jpg

[dhemor_]

Hmm, that is interesting.. I've never done the electrolysis method, but I'll help with what I can..
First off, there is no such thing as CuO2. Copper can be in the +1 or +2 oxidation state, so you can have Cu2O (Copper is +1), or CuO (Copper is +2).
I think it could be copper(I) oxide, as it's a brown-red solid, but Wikipedia would have told you that. It'd guess that the copper hydroxide was heated by the current to give the copper oxide, or the electrolysis of the copper hydroxide gave off the Cu2O.

[351q]

Oops, I don't know why I wrote CuO2 I must have been tired. I don't think it could be cuprous oxide because the TACN (with some ammonium nitrate remaining) only became brown when mixed with hydrogen peroxide. The original solution from the electrolysis, containing copper hydroxide precipitate, was just plain blue. But what I find is the strangest thing is that the TACN (or possibly another, very similar, copper complex) recrystallized after the brown solution was dried. So the TACN was only brown in hydrogen peroxide. I can really explain that, but maybe the TACN and H2O2 formed a complex which then decomposed after drying. This is quite a mystery.

[Ethyl]

Sorry for bringing up an old thread, but it looks like TACN can be made after all to work.
Here is 180g of it going off from 0.5g of HMTD.
http://uk.youtube.com/watch?v=QJqrsfFlrZ0