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Marvin
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My apologies for forgetting the 'o'.
From the sodium persulphate MSDS....
"Unstable. Strong oxidizer. Contact with combustible material may cause fire. Incompatible with combustible material, strong reducing agents,
strong bases, alcohols, aluminium, magnesium. Protect from moisture. "
I'm not convinced I'd try to keep organic peroxides very long, but this strikes me as fractionally less insane if the alcohol is dry.
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Axt
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<a href="http://ww1.altlist.com/~58717/pulse.altlist.com/images/complexpersulphates.jpg">Heres</a> the reference from the journal on
ethylenediamine "stabalised" persulphate, theres not much that hasn't already been said but its always better to see the original. Ive tried to form a
complex using urea with no luck.
Below is tetramminocopper permanganate, the silver salt burns simularly, with dull flame and gouts of fluffy residue.
<center><img src="http://www.sciencemadness.org/scipics/axt/tetramminocopper-permanganate.jpg">
<a href="http://www.geocities.com/roguemovies7/index.html">Movie</a></center>
<br>
[Edited on 9-12-2005 by Axt]
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chemoleo
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Complex Cu - persulfates (with ammonia, hydroxylamine, ethylenediamine)
I had a go at various persulphates, and I have to say I am quite impressed with them (compared to the i.e. copper tetramine nitrate)
A copper sulphate solution was prepared (no stoichiometric quantities given as this was a testrun), and to this, a saturated ammoniumpersulphate
solution was added. No significant colour change, except that the colour became lighter due to dilution. Note that ammonium, rather than Na
persulphate was used.
The same thing was done vice versa, i.e. to copper sulpahte solution, either Hydroxylamine (base, H2NOH), ammonia NH3 or ethylendiamine NH2-C2H4-NH2
was added.
In either case, with an excess of the respective base, in case of
1) the hydroxylamine, the solution turned a deep turbid green (when it contained just CuSO4), with visible signs of fine
precipitation. I am not sure at all what this is, the green stuff. As soon as the ammoniumpersulphate was added, lots of bubbled formed, and the
greenness disappeared, leaving me with a blue solution again. I believe that the action of the persulphate is to oxidise the hydroxylamine, destroying
both in its course and leaving me with CuSO4 solution once again. I don't think the hydroxylamine/persulphate system is a workable one.
2) the ammonia, , the solution turned an even deeper blue (slightly purple hint), and crystallisation ensued once it was put into an
ice batch. I found it is actually quite soluble, so if you do the experiment work with minimum amounts of water. As axt said, it forms fine
needle-like crystals.
3) the ethylenediamine, the solution turned a deep violet, and IMMEDIATELY forms masses of violet needle-crystals once again. The
colour is distinctly purple, easily told apart from the ammonia complex from above. Also, the ethylenediamine persulphate complex is a lot less
soluble - nearly all is crystallised, and the solution above is only slightly purple. Great stuff to work with, really easily isolated!
Edit: I just read the original article on the ethylenediammine complex, and I can't really confirm this. It seemed no more sensitive than the
amine salt. The description of it being purple and sparsely soluble fits though. Yet again they state it decomposes to leave a blue residue, while
mine leaves a brown snake (see below). Hmm. Are they colourblind? Also (see below) I didn't observe these explosive properties. Maybe I ought to
try with their quantities, but I don't see why this would make a difference. Comments?
Below is a picture of the two on the filter paper, it was first washed with cold water, and then washed with ethanol (96%). No adverse reaction with
the ethanol, as I said above I'd have been surprised if there had been (plus the article from Axt confirms this). The top pic is the
ethylenediame complex, the bottom the ammonia one.
<center>
</center>
Stability: In solution/crystals in the original reaction mix (which still contains excess complexant), both solutions are fine (after
two days storage), no visible colour change, bubbles etc. I think I can keep it there for a while, in the fridge. The dry powder, in case of the
ethylenediamine complex turns green overnight, so definitely not stable. Also it doesn't burn anymore. The ammonia complex seemed fine.
Flammability, Friction etc: ABSOLUTELY WICKED STUFF! The ammonia complex burns very fast, instantaneous, with a small whoosh/pop,
with a BEAUTIFUL GREEN FLAME, leaving a small green residue. The ethylenediamine complex burns nearly equally well (but definitely less rapidly), and
leaves a snake of a brown substance that is sticky and soft. Quite funny to watch, the stuff burns and produces an extremely fast moving brown
snake... anyway, Axt, it seems you were right in your prediction that the ethylenediamine complex is not as powerful. Both need yet to be tested under
confinement, though.
Anyway, both burn well, and both don't seem particularly friction sensitive. In case of the ammonia complex, after deflag. it smells of ammonia
(surprise).
To sum it all up:
DEFINITELY A MUST to anyone who is interested in these salts. So far this was the fastest/best of the copper variety I have played with, and
incredibly easy to make. In greater amounts, I could definitely see this as a weak primary. THe only downside I can see is durability, so store in
aqueous solution before use, then filter and wash with ethanol. Use right after its dry. Have fun 
PS I wonder what other bases (aside from hydrazine) I could test. Ideas anyone?
[Edited on 10-10-2004 by chemoleo]
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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Axt
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Nice 
As I said before, I tried with urea, but no colour change nor precip, though I was using K persulphate so I had to use a lot more water then you would
be using. (NH4)2S2O8 should be better and easier to find anyway (circuit board etchant), actually I just bought some today.
Try putting it in a tube and lauching a "snake" into the air  , I
never noticed a green flame from the ammonia complex, have to make it again just to see it. At least they have novelty value.
Maybe its zinc salt (if possible) should be next on the list to try. There is sweet few primaries that can be made easily from OTC chems, the
persulphates may be one of them.
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Axt
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Talking of complex persulphates, what of the other peroxy complexes! its a whole branch that hasnt been touched on. check P185 vol 8 of PATR;
(NH3)5Co-O-O-Co(NH3)5(NO3)5
Co2H30N15O17 --> 2CoO + 15H2O + 12.5N2, nice balance! Though it lists no refs/synth nor properties but one can imagine its quite energetic!
It doesnt list the copper salts but it does list the tetramminozinc persulphate so yep, it can be done, "explodes on heating or impact".
Very interestingly, Ca persulphate itself is listed as "sensitive to shock, explodes violently", I assume syth is as easy as Ca nitrate +
ammonium persulphate.
I've tried triamminochromium tetroxide before (starting with CrO3) but couldn't get a precip, should be easier to start with ammonium
dichromate. PATR gives it good properties.
So, theres lots of interesting ones!
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Axt
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| Quote: | Originally posted by Axt
12.5N2 |
7.5N2 
Mellor 9 (1939), 795 for K2O6V ... anyone? looks deadly.
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mark
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AXT
If you wouldn’t mind would you please tell me where you got your potassium persulphate? I have reagent grade catalogue however this stuff would be
extremely expensive to buy at $130.00 Au for 500g. Thank you.
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Ium
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You will want Ammonium Persulfate not the Potassium salt. Solubility of Ammonium salt is many times higher according to references.
This should be enough to help you to find a source .
Google Search
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The_Davster
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Well, I am in a good mood now so I might as well help him out a bit more...
Froogle
[Edited on 31-10-2004 by rogue chemist]
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mark
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I live Australia so froogle is basically useless. I have done numerous searches on google and found nothing about sources or common materials that
contain this chemical. I always search before posting but a lot of times my not very extensive knowledge holds me back. I really wish to try the salt
because I don’t want to play with the usual Organic peroxides, I like to experiment with unusual substances to help get a large knowledge of the
world around me.
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chemoleo
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Well, come on, 4 posts on ammoniumpersulphate availability, where the Na-derivative is available by any electronics supply shop. It's not like
it's massively tricky to obtain. Or are you going to discuss availability of ammonia in the next four posts? A single U2U would suffice instead.
If you want to discuss making persulphate, check other threads on persulphates, or create one.
If this kind of thread dilution was to happen in other threads as well, we would be discussing peripherals most of the time. So please try to
avoid this.
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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KemiRockarFett
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Thought about the persulfates that they may be explosive due to the bonding situation, so way should not ammoniumperoxidisulphate and
ammoniumpersulphate have explosive properties ?
Reading in Federof:
Ammonium Peroxodisulfate Explodes violently on addition of Ag salts.
About the peroxidisulphate of Ca it says:
Calcium Peroxodisulfate, Sensitive to shock; explodes violently.
Peroxides are often fast primarys so I wonder where to read about initiating properties about these peroxi sulphates and other inorganic peroxi
compounds.
Have somebody tried to detonate ammoniumperoxodisulphate ?
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Axt
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OK, just got some ethylenediamine, since chemoleo has reported that the persulphate precipitates easily from solution (relative to the amine) my
thoughts were that the more energetic complexes may be easily isolated from an aqueous solution as well.
TACB is very sensitive, 2.5x more sensitive to impact then MF, but it can't be made in aqueous solutions. It wont precipitate nor can it be
evaporated out without losing its NH3. So I set out to attempt Bis(ethylenediamine)copper (II) bromate. But alas, it doesnt precipitate, maybe I was
being a bit optimistic especially with the S2O4 in solution. So I tried evaporating it out. Its been 40°C outside the last few days, so no problem
getting it dry.
The extract explodes with a bang in nearly any amount. 1/4 matchhead worth will sound like a cap gun when ignited in the open, even though its half
composed of the sulphates.
Na2SO4 seems to be the first thing to precipitate in ethanol, so this looks like the way to get the relatively pure bromate complex.
The bromate/sulphate extract explodes at a drop of 0-5cm (comparable with the peroxides), but doesnt seem sensitive to friction. Its been sitting in
the sun for 3 days now with no decomposition.
There is a <a href="http://www.geocities.com/roguemovies7/index.html">movie</a>, but its only 0.2g ignited in open.
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chemoleo
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That's interesting, becuase I tested tetraamine /ethylenediamine periodate / copper complexes. As far as I remember, complexing worked well, but
after a while I seemed to get fluffy precipates which looked more like hydroxides than anything else, as soon as I added ethanol(or acetone) to
facilitate precipitation (the complex remained soluble). This fluffy precipitate has to be tested though, yet.
I guess I will try this with perchlorate at some point.
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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mark
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Feeling a bad about my stupid question I am trying rectify the situation. To day recently tried to prepare calcium persulphate. 5 grams of calcium
nitrate was added to a solution of 5 grams of ammonium persulphate in 40ml of hot water (70 degrees). The solution was then chilled in an ice bath
until a fluffy suspension was noticed in the liquids this was filtered out. The filtrate is still drying. I’ll edit this with a movie link in a
couple of hours to see if anything happens when I put a propane torch to it.
The stuff didn't deflagrate unless you just want a movie of a bottle cap burning. So no movie sorry.
[Edited on 1-12-2004 by mark]
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mark
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I had success using the ammonium persulphate used the same method as Axt except using 30 ml of ammonia solution made by bubbling ammonia gas through
water. The good thing a bout ammonium persulphate is I only needed 75ml of hot water to dissolve the ammonium persulphate other than the 200ml for
the potassium persulphate. I got what looked like an excellent yield although I took some out of the filter and dried it on paper (most of the yield)
and before it was fully dry most of decomposed into the same gunk as when you light a pile. However, the bit left on the filter was watched with
mentholated sprits and showed no sign of decomposition. Also, lighting relatively large amounts amount of this explosive seemed very un-energetic,
merely just burning instantaneously. I also confined a smallish amount in a old antenna tube (1 gram) and it busted the top open with a very light
report.
Over rated I think.
Back to calcium persulphate. I had done the same procedure as last time except using 10 grams of each in 40 ml of hot water. Same precipitate except
much denser and cloudier it still didn’t burn. So maybe another calcium source?
Edit by chemoleo: You do realise that Ca/NH4 persulphate aren't exactly complex salts? Besides this they are very unlikely to fall into the
category 'primary'.
[Edited on 3-12-2004 by chemoleo]
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t3sla_trooper
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Excuse me for excavating this old thread, but has anyone actually tried using the tetramine copper persulphate as primary ?
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mark
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I have. I have pressed into several tubes (antenna, straws, etc) used as filler in a Polumna (Sp?) None of which gave a detonation or even a half
decent report. I have also ignited whole batches (10g to 10g ratio) and got a small noise but defiantly no detonation. It’s a nice novelty but if
your to close it splatters you with this little green residue that stings a lot. Have fun by the way wash your yield with ethanal other wise it has a
habit of decomposing if it contains water.
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t3sla_trooper
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can you please make one more test with unpressed tetramine copper persulfate?
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mark
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Test complete. No detonation, or primary chracterisitcs noted upon ignition.
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The_Rsert
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| Quote: | Originally posted by Axt
OK, just got some ethylenediamine, since chemoleo has reported that the persulphate precipitates easily from solution (relative to the amine) my
thoughts were that the more energetic complexes may be easily isolated from an aqueous solution as well.
TACB is very sensitive, 2.5x more sensitive to impact then MF, but it can't be made in aqueous solutions. It wont precipitate nor can it be
evaporated out without losing its NH3. So I set out to attempt Bis(ethylenediamine)copper (II) bromate. But alas, it doesnt precipitate, maybe I was
being a bit optimistic especially with the S2O4 in solution. So I tried evaporating it out. Its been 40°C outside the last few days, so no problem
getting it dry.
The extract explodes with a bang in nearly any amount. 1/4 matchhead worth will sound like a cap gun when ignited in the open, even though its half
composed of the sulphates.
Na2SO4 seems to be the first thing to precipitate in ethanol, so this looks like the way to get the relatively pure bromate complex.
The bromate/sulphate extract explodes at a drop of 0-5cm (comparable with the peroxides), but doesnt seem sensitive to friction. Its been sitting in
the sun for 3 days now with no decomposition.
There is a <a href="http://www.geocities.com/roguemovies7/index.html">movie</a>, but its only 0.2g ignited in open.
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Axt, how have you prepared this stuff exactly?
Because it looks very powerful and interesting. I'm pleased to get an answer.
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Axt
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I dont have the amounts used anymore, I think I simply mixed the stoichiometric quantities to see if anything would precipitate, but nope.
So,
2M sodium bromate
2M ethylenediamine
1M copper sulphate pentahydrate
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The_Rsert
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| Quote: | Originally posted by Axt
I dont have the amounts used anymore, I think I simply mixed the stoichiometric quantities to see if anything would precipitate, but nope.
So,
2M sodium bromate
2M ethylenediamine
1M copper sulphate pentahydrate |
So, you have mixes satturated solutions of 2M SB with 2M EDA and 1M CS in water.
And than, you've evaporated the water and extracted the bromate complex from the sulphate complex with ethanol. Right?
Or?
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Axt
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Yes, but the ethanol should extract the bromate complex leaving the <i>sodium</i> sulphate, but this isn't confirmed. The movie you
see is the raw mix of crap after evaporation.
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K9
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What was the process for tetramminocopper permanganate? Would it just involve the addition of a potassium permanaganate solution or is there more?
Thanx.
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