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UnintentionalChaos
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[*] posted on 30-12-2006 at 15:10
CuO (experience question)


Those of you that have made CuO by:

Cu(OH)2 -> CuO + H2O

What color does the powder generally end up? I thought it should be a dark black, but mine came out a brownish gray. I can think of no other compound it could be/ be contaminated with. It is MUCH finer than another batch (made by roasting some as of yet unidentified copper compound (I suspect oxychloride though)), though and suspends itself in water for up to an hour. The other batch is the expected pitch black, but is too large to suspend.
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[*] posted on 30-12-2006 at 15:21


mine has brown almost black..
i made mine from cupric sulphate and lye excess.. put in a 3 liter PET bottle and washed/decanted several times to remove any lye (which can eat your metal pan ) or sodium sulphate... the suspension in a pan reduces extremely the original volume when heating to vaporizes the water...

[Editado em 30-12-2006 por Aqua_Fortis_100%]




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[*] posted on 30-12-2006 at 18:35


Copper, Cu(I) or CuCl2(anh.) impurity?

Copper oxychloride smokes when I calcine it.

Tim




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UnintentionalChaos
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[*] posted on 30-12-2006 at 21:12


It was in a magnesium sulfate electrolyte :o Mg(OH)2 contamination? I tried putting in vinegar because I figured any magnesium hydroxide would dissolve almost immediately to magnesium acetate while the CuO would take a while to turn to copper acetate. No color change after filtering out the remaining CuO. :( I am aware of a small Cu2O impurity, but this does not explain the color. It's medium gray with a little brown tinge when dry. I did electrolysis of pieces of copper scrap in a magnesium sulfate electrolyte, decanted the liquid, added a large volume of water, settled, decanted, and repeated this 4 more times before boiling the properly "light blue fluff" for an extended period of time in clean water.

PS: Calcined it way hotter than it should need for way longer than I thought necessary, and yet, no change. :(

[Edited on 12-31-06 by UnintentionalChaos]
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[*] posted on 31-12-2006 at 03:19


Magnesium (as hydroxide) would ppt on the cathode. If it tends to fall off, then sure, it could be in there.

Did your electrolyte end up colored?

Tim




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UnintentionalChaos
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[*] posted on 31-12-2006 at 12:57


Solution was crystal clear. Anyway, I don't have much in the way of a current source, so it takes a really long time to produce even a small amount of Cu(OH)2.
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[*] posted on 2-1-2007 at 17:56


Ok...I posted this elsewhere but...
When electrolysing MgSO4 with copper electrodes, you do not get the expected Cu(OH)2. You get a whole mess of various Cu(x)(OH)(y)(SO4)(z) compounds which ppt out in the cell. These basic sulfates do not decompose nicely to CuO like Cu(OH)2 does.
In my experience, one cannot use an electroylte with doubly charged ions in it, or such things happen. Best is a KNO3 solution, from which pure Cu(OH)2 precipitates from. And if you run it long enough it gets hot enough to turn it into CuO:P, if it gets to boiling temp you get nitrate reduced to ammonia as well.




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[*] posted on 2-1-2007 at 18:48


And I just managed to get hold of some KNO3 as well as a much higher amperage power supply! Thanks a lot!
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[*] posted on 3-1-2007 at 04:01


I know this is kind of off topic, but if I can just put in my two cents worth. :)
I've only ever used electrolysis for chlorate prep. (since I can do it no other way) because electrolysis is expensive, time consuming, messy and inefficient IMHO. Production of Sodium is another example of when electrolysis is a great method, but for the production of a metal oxide, I'd just go with tried & true reaction of strong hydroxide solution with concentrated Cu(II) solution. Simple, one step reaction that has worked for me every time giving a very fine (dust-like) precipitate which is as pure as your solutions (<i>i.e.</i> can be very pure indeed!).
So yea, sorry for the unsolicited advice ;)
- Ramiel

[edited a p.s. in just for kicks]
Relevant linkage:
<a href="http://www.sciencemadness.org/talk/viewthread.php?tid=271">Can't Make CuO</a> [by electrolysis] - old 4 page thread, many methods discussed.
<a href="http://www.sciencemadness.org/talk/viewthread.php?tid=127">Exotic thermites and analogues</a> - even older thread, if you can wade through all 9 pages, there's some interesting info there too.

[Edited on 3-1-2007 by Ramiel]




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[*] posted on 3-1-2007 at 04:08


A shameful waste of hydroxide though...

Tim




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[*] posted on 24-1-2007 at 04:42
Just a thought


Hi, I'm new here and not the most advanced chemist but I wonder if a -hot and concentrated- sol. of Sodium Carbonate would react with a solution of Cu(x)Cl(y) to form a copper carbonate / copper hydroxide mix from which the desired CuO could then be obtained by heating.

??
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[*] posted on 24-1-2007 at 08:13


Possible. Boiling with NaOH produces black material (CuO), but I don't know if carbonate is basic enough to attack the oxychloride.

Tim




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[*] posted on 24-1-2007 at 09:54


I get a brown black with the hydroxide and the carbonate of copper, less brown with the carbonate though.
that`s in a 25 ml crucible at propane bunsen temps held for 20 mins with the lid on.
no gray material though?




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