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S.C. Wack
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I'd imagine that chlorine hydrate can be made to react with anything.
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blogfast25
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Is 'anything' not a bit too broad? Certain metals will not be attacked appreciably, others so slowly it isn't a practical method.
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Endimion17
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Has anyone tried to make very pure lead from the salts obtained? For example, a nice lead plate using electrolysis, for element collection.
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blogfast25
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Quote: Originally posted by Endimion17  | | Has anyone tried to make very pure lead from the salts obtained? For example, a nice lead plate using electrolysis, for element collection.
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I made lead by electrolysing molten PbCl2 with copper electrodes when I was about 16 but I've no idea how pure it was.
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S.C. Wack
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| Quote: Originally posted by blogfast25 | | Is 'anything' not a bit too broad? Certain metals will not be attacked appreciably, others so slowly it isn't a practical method.
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Obviously "made to react" is a small, off-topic comment, (I could have added that I also found PbSO4 in quite small crystals covering the electrodes
of a very much dying battery, but this was already pointed out) which does not exactly mean adding water to chlorine hydrate, nor was I speaking of
some practical amazing all-inclusive method for dissolving every substance known despite the use of anything. It was an attempt to point out that
chlorine and water can be concentrated.
It is already known that no one appreciates brevity and hidden layers of meaning.
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blogfast25
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You're just to clever by half... 
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sxl168
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| Quote: Originally posted by Endimion17 | | Has anyone tried to make very pure lead from the salts obtained? For example, a nice lead plate using electrolysis, for element collection.
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For most of my purposes, I don't really need purity, however if I do, I will get Lead dissolved in solution and add a sulfate to the solution to
precip. PbSO4. Hot solutions speed this up a lot and produce larger particles. There are very few insoluble sulfate salts, so you should have rather
pure PbSO4 after thorough washing. I do believe that BaSO4 is used in small quantities in batteries for seed crystal sites and so that would be the
main contaminate. Do note that if sodium is present in moderate or high concentration, this will not work as PbSO4 is soluble in said solutions. From
PbSO4 use Sodium Carbonate or Bicarbonate to convert it to PbCO3. From there you can turn it into the product of your choice.
As for plating out Lead, I've done that but I don't know of its purity and it also forms as a loose sponge mass/dendrites that is probably >90%
electrolyte. Takes a while to flush out all the electrolyte and dry it before melting. I'm not aware of any method that produces compact deposits
outside of a Fluroborate electrolyte. I'd definitely like to know if anyone has gotten a compact deposit besides the use of a Fluroborate electrolyte.
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dann2
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| Quote: Originally posted by sxl168 | | ........... Do note that if sodium is present in moderate or high concentration, this will not work as PbSO4 is soluble in said solutions. From PbSO4
use Sodium Carbonate or Bicarbonate to convert it to PbCO3. .................... |
Are you saying that Lead Sulphate is soluble in a solution of Sodium Sulphate?
That does not make sense to me.
Dann2
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sxl168
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My bad for not proofreading before posting. Meant Sodium Chloride there.
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dann2
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Interesting method using sugar to dissolve Lead Acid battery parts here:
http://www.sciencemadness.org/talk/viewthread.php?tid=20175
Lead Nitrate can be prepared with Ammonium Nitrate + Litharge (PbO). The PbO is added to a solution of AN and boiled whereby the Ammonia goes away and
Lead Nitrate is left.
This was suggested by Plante1999.
PbO can be obtained from battery PbO2 by calcining (heating strongly) (Plante1999)
Dann2
[Edited on 31-5-2012 by dann2]
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blogfast25
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Thanks. I've been meaning to try that!
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plante1999
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| Quote: Originally posted by dann2 |
Lead Nitrate can be prepared with Ammonium Nitrate + Litharge (PbO). The PbO is added to a solution of AN and boiled whereby the Ammonia goes away and
Lead Nitrate is left.
Dann2 |
I just make this process yesterday, and posted it in PbO2 anode thread this morning, few hour later the process is already in lead salt thread...
Please give your reference next time (the reference is me).
I never asked for this.
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MR AZIDE
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| Quote: Originally posted by garage chemist |
PbO2, lead dioxide, is very easily made by electrolyzing 20% H2SO4 with two lead electrodes. At the cathode hydrogen is evolved, at the anode PbO2 is
formed as a dark brown powder.
The electrolysis can be continued until the entire anode is converted into PbO2. The PbO2 is isolated by filtering the solution, washing and drying
the PbO2.
PbO2 is a powerful oxidiser, capable of forming very energetic pyrotechnic mixes, especially with powdered metals. |
Excellent method ...Ill need to try this one........I did have some nice chocolate brown Lead (IV) Oxide from and old accumulator, but this sounds a
nice reaction.
Ammonium Chloro Plumbate (NH4)2.PbCl6
Adding PbO2 to ICE COOLED concentrated about (30% ish) HCl, PBO2 dissolves without oxidising the HCl to , to form a lead tetra chloride ligand. PbCL4
-2.
If I remember, the solution turns a yellow colour, but if the temp rises the PbCl2 will crystallize, and the unstable-ish ligand releases chlorine....
I think I remember reading that addition of ammonia/ammonium chloride to the ice cooled, Pb Cl4 complex should precipitate out ammonium chloro
Plumbate.
PbO2 + 4HCL ----> PbCl4 + H20
PbCL4 + 2Cl- ------> PbCl6 -2
then
2NH4+ ----> PbCl6 -2 -------> (NH4)2.PbCl6
Says if this is added to ice cool H2SO4 then PbCL4 as a heavy yellow oil, hydrolysed with H2O......
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blogfast25
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Your method is correct, MR A. The PbO2 must be freshly prepared though. (NH4)2PbCl6 is yellow. (NH4)2SnCl6 also exists.
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MR AZIDE
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The PBO2 I used was from the mesh on an old accumulator, which may have been contaminated with sulphates.
Ive found a big lump of lead sheet I found years ago, ( about 3mm thick and about 40 by 30 cm.
I going to try electrolysing the H2SO4 with Pb electrodes, to see how much PbO2 I can get........
Dont know what fun can be had with the ammonium chloro plumbate yet.
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blogfast25
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Not much. As you wrote, with cold (IIRW), dry, concentrated sulphuric a dark oil of PbCl4 separates out.
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MR AZIDE
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I HAVE just electrolyzed a strong NaCl solution with 2 lead electrodes, in a 100 ml beaker.
Using a MOT Tx in reverse, so the supply is 24 V.
Now, PbOH is supposed to be produced which is white, but at first, chlorine gas was being emmited, and the solution quickly has turned orange, then a
dark brown precipitate has formed, which is settling at bottom of cell.
IS this precipitate likely to be Lead(IV) Oxide, or is it possible that it is a Lead Chlorate, is the Cl gas was mixing with the solution.? What
colour are the LEad chlorate's,? Im assuming they are insoluble.
The elecrolysis, has now after a few mins, stopped producing any Cl gas, the Cathode still fizzing away.., and Now white PbOH is being formed at
anode, with no gas evolution.
The current is falling due to the inhibition of the insolubility of the coating of Pb(OH)2,
IF the anode is wiped clean, the current is aver 2 Amp but drops to aony about 40mA.
Question is, why is the brown precip, now not happening, and its Pb(OH)2 .??
Its now disconnected, I think Ill repeat this tommorrow in a U-tube to keep the elecrtodes separate, and see what happens.
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blogfast25
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| Quote: Originally posted by MR AZIDE |
I HAVE just electrolyzed a strong NaCl solution with 2 lead electrodes, in a 100 ml beaker.
Using a MOT Tx in reverse, so the supply is 24 V.
Now, PbOH is supposed to be produced which is white, but at first, chlorine gas was being emmited, and the solution quickly has turned orange, then a
dark brown precipitate has formed, which is settling at bottom of cell.
IS this precipitate likely to be Lead(IV) Oxide, or is it possible that it is a Lead Chlorate, is the Cl gas was mixing with the solution.? What
colour are the LEad chlorate's,? Im assuming they are insoluble.
The elecrolysis, has now after a few mins, stopped producing any Cl gas, the Cathode still fizzing away.., and Now white PbOH is being formed at
anode, with no gas evolution.
The current is falling due to the inhibition of the insolubility of the coating of Pb(OH)2,
IF the anode is wiped clean, the current is aver 2 Amp but drops to aony about 40mA.
Question is, why is the brown precip, now not happening, and its Pb(OH)2 .??
Its now disconnected, I think Ill repeat this tommorrow in a U-tube to keep the elecrtodes separate, and see what happens. |
Did you mean Pb(OH)2? The precipitate is PbO2. Lead chlorate would be white, I'm quite sure of it.
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MR AZIDE
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had a bit of difficulty in looking up lead chlorates/ perchlorates, but they are freely soluble in water.
I think what happened is the NACL was concentrated enough, that Pb(OH)2 was formed, and immediately reacted with the Cl gas, maybe changing the
Pb(OH)2 to PBO2 .
I ve thrown it away now anyway.
I had much more interesting results electrolysing some HCL with Pb electrodes today, which I may post in the technochemistry bit.
here www.sciencemadness.org/talk/viewthread.php?tid=20284
[Edited on 1-6-2012 by MR AZIDE]
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blogfast25
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| Quote: Originally posted by MR AZIDE |
I think what happened is the NACL was concentrated enough, that Pb(OH)2 was formed, and immediately reacted with the Cl gas, maybe changing the
Pb(OH)2 to PBO2 .
I ve thrown it away now anyway.
[Edited on 1-6-2012 by MR AZIDE] |
Check the half-potentials to see if:
Pb<sup>2+</sup> + Cl<sub>2</sub> === > Pb<sup>4+</sup> + 2 Cl<sup>-</sup>
... is possible. Dunno off the top of my head, TBH...
Edit: I checked. This oxidation appears not to be thermodynamically favourable, chlorine isn't strong enough. But hypochlorite is and some of that may
have formed with your electrolysis.
[Edited on 1-6-2012 by blogfast25]
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MR AZIDE
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as long as the Cl2 gas was liberated , the probable Pbo2 was produced, as definately hypochlorite will be being produced.......this oxidised the lead
to from +2 to +4, .......
PbO2, Ive just read can be produced by shaking a solution of a hypochlorite with a suspension of Pb(OH)2 in water.
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Lambda-Eyde
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| Quote: Originally posted by blogfast25 |
Check the half-potentials to see if:
Pb<sup>2+</sup> + Cl<sub>2</sub> === > Pb<sup>4+</sup> + 2 Cl<sup>-</sup>
... is possible. Dunno off the top of my head, TBH...
Edit: I checked. This oxidation appears not to be thermodynamically favourable, chlorine isn't strong enough. But hypochlorite is and some of that may
have formed with your electrolysis.
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I had a paper on producing Pb(AcO)<sub>4</sub> from Pb<sub>3</sub>O<sub>4</sub>, acetic acid and acetic anhydride.
The yield could be maximized by oxidizing the remaining Pb<sup>2+</sup> with chlorine gas IIRC.
This just in: 95,5 % of the world population lives outside the USA
Please drop by our IRC channel: #sciencemadness @ irc.efnet.org
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blogfast25
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| Quote: Originally posted by MR AZIDE |
PbO2, Ive just read can be produced by shaking a solution of a hypochlorite with a suspension of Pb(OH)2 in water. |
No need for shaking , see the other thread on battery lead and my results.
Hypochlorite easily oxidises Pb(OH)2 to PbO2.
[Edited on 2-6-2012 by blogfast25]
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MR AZIDE
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I see your source of NAOCl, was bleach.......is this like the cheap stuff you can buy in supermarkets.?
Ive seen like the cheap own brand stuff in the supermarket, and I read the labels just says '' contains sodium hypochlorite'', but it never says what
concentration the sodium hypochlorite is.
Ive never got round to buying any to play with.
are most of these thick /thin bleaches( as they call it,) basically NaOCl in plain water?,,,, are there many additives........is the solution
colorless of slightly yellow?
If so Id like to try at some point making KClO3 via nurdrage's method........
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blogfast25
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| Quote: Originally posted by MR AZIDE | I see your source of NAOCl, was bleach.......is this like the cheap stuff you can buy in supermarkets.?
Ive seen like the cheap own brand stuff in the supermarket, and I read the labels just says '' contains sodium hypochlorite'', but it never says what
concentration the sodium hypochlorite is.
Ive never got round to buying any to play with.
are most of these thick /thin bleaches( as they call it,) basically NaOCl in plain water?,,,, are there many additives........is the solution
colorless of slightly yellow?
If so Id like to try at some point making KClO3 via nurdrage's method........
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Get 'no frills' thin bleach: 4 - 5 % NaClO (sodium hypochlorite). Weak concentration, strong oxidiser. Ca(ClO)2 ('pool shock') is 100 % (solid) but
harder to get.
Thick = thin + glycerine. Avoid!
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