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Author: Subject: Refining mercury from cinnabar
blogfast25
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[*] posted on 24-12-2011 at 06:30


Quote: Originally posted by vmelkon  
Then the biggest problem = Ca(OH)<sub>2</sub> doesn't dissolve much in water.


Except... that's not a problem at all:

Ca(OH)<sub>2</sub>(aq) + Na<sub>2</sub>CO<sub>3</sub>(aq) ==== > CaCO<sub>3</sub>(s) + 2 NaOH(aq)

The high insolubility of CaCO<sub>3</sub> drives this equilibrium entirely (quantitatively) to the right. It just takes a little bit of time and some gentle heating, starting from a suspension of Ca(OH)<sub>2</sub> in water. It's a nice classroom experiment to make a NaOH (or KOH) solution by means of a displacement reaction.

[Edited on 24-12-2011 by blogfast25]

<!-- bfesser_edit_tag -->[<a href="u2u.php?action=send&username=bfesser">bfesser</a>: subscript]

[Edited on 3.8.13 by bfesser]




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blogfast25
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[*] posted on 24-12-2011 at 06:52


Quote: Originally posted by jsc  
LOL, you envision building a Castner cell to make lye?



A Castner cell doesn't use mercury, it electrolyses molten NaOH. Member 'len1' constructed one of these and reported extensively about it on this board (search for it). 'Not in a miliion years'? Who is sounding dumb now, eh?

[Edited on 24-12-2011 by blogfast25]




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plante1999
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[*] posted on 24-1-2012 at 16:25


I will buy this in a few day:

http://www.ebay.ca/itm/Grounded-Cinnabar-Crystal-Tiny-pieces...




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[*] posted on 24-1-2012 at 16:35


Quote: Originally posted by jsc  
LOL, you envision building a Castner cell to make lye?

There are much, much easier ways to make lye. The basic approach is to heat chalk (calcium carbonate) in a furnace at 1000C to convert it to lime (calcium oxide). Add water to make lime water (calcium hydroxide). Then combine with washing soda (sodium carbonate) to make lye.

Or you could buy lye for 50 cents a pound or whatever it is. Its cheaper than sawdust.

All of this is irrelevant of course because anyone who is dumb enough to not know this sort of thing will never in million years be able to make a Castner cell. You realize that requires machining right? Have you ever even TOUCHED a lathe in your life? Probably not.

Here's another tip: don't breathe mercury fumes because that will make you even dumber than you already are.

I advise taking up a hobby that doesn't involve heavy metals or sharp objects.



What the f*ck is your problem jsc? Do you get off on picking on young kids online who are trying to learn some chemistry? Cause it makes you sound like an idiot. I think you need to be civil or stfu, personally.

--------------
Quote: Originally posted by plante1999  
I will buy this in a few day:

URL to cinnabar


Oh, and good luck plante. Can't say it's the best way to get mercury, but it's a good history lesson. Be careful and use ventilation and proper technique and I'm sure it will be a success.

[Edited on 25-1-2012 by Bot0nist]




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[*] posted on 24-1-2012 at 16:47


i was just going to mention the same link on ebay about the cinnabar! beat me to it!!



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plante1999
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[*] posted on 25-1-2012 at 15:47


Wich process should I use(read the whole tread to see wath I talk about) :

Iron/zinc powder with cinnabar

Leaching with iodine tincture / hypochlorite

MnO<sub>2</sub> / Ca(ClO)<sub>2</sub> dry oxidation

<!-- bfesser_edit_tag -->[<a href="u2u.php?action=send&username=bfesser">bfesser</a>: subscript]

[Edited on 3.8.13 by bfesser]




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plante1999
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[*] posted on 25-1-2012 at 17:34


I just purchased 25g of cinnabar:

It should take 2-4 weeks to arrive.


http://www.ebay.ca/itm/Grounded-Cinnabar-Crystal-Tiny-pieces...

[Edited on 26-1-2012 by plante1999]




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[*] posted on 26-1-2012 at 09:55


cool ! let us know how it goes



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[*] posted on 26-1-2012 at 12:49


Quote: Originally posted by plante1999  
I just purchased 25g of cinnabar:

It should take 2-4 weeks to arrive.


http://www.ebay.ca/itm/Grounded-Cinnabar-Crystal-Tiny-pieces...

[Edited on 26-1-2012 by plante1999]


That 'Grounded Cinnabar' doesn't look very fit for purpose to me... :(




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[*] posted on 26-1-2012 at 15:38


I will grind it to powder when I will get it. I think I will use a 1/2 inch glass tube as an retort and the reaction of iron and cinnabar to make the mercury. I will heat with a propane torch and I will wait for a minus 20 celcius day to use the snow as the cooling condenser. I will condense the vapor in a water filed beaker (to catch mercury vapor).

Question: Does mercury will coaless in a single ball or it will make a miror in the condenser?

Thanks!!!




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[*] posted on 27-1-2012 at 20:58


No, it does not coat. It will form many small balls at first and as they get heavy, they will flow down because of gravity and bind with other small spheres. Try to collect all the small droplets at the end of your experiment.
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[*] posted on 31-1-2012 at 02:55


I don't know if you have much experience with distillation but there are a few important rules to remember : the condensation tube should be long, the longer the better.
Keep the temperature of the condenser close to the mp of the distillate (if you can)
Joints should be tight. Make sure they don't come apart.
Use a fan on a low setting to blow any vapors away from you (even if you are outside)

Also, you might want to get some dry ice for the receiving end of your setup.
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[*] posted on 31-1-2012 at 04:48


Thanks for your support! I will probably make a retort with a glass tube, I will melt one end of the tube and I will make a long condenser. I do not have dryice but I could get -40degree C with HCl and snow.



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[*] posted on 2-2-2012 at 17:29


@ blogfast.

Wath is wrong with my cinnabar? How do YOU would synthesis mercury from cinnabar?

I am thinkink to a new process to make mercury from cinnabar Al and Hg<sup>++</sup> salt from amalgation of [Al] with Hg<sup>++</sup> salt and subsequand reaction of cinnabar with Al amalgam to produce more mercury and Al<sub>2</sub>S<sub>3</sub>.

<!-- bfesser_edit_tag -->[<a href="u2u.php?action=send&username=bfesser">bfesser</a>: subscript/superscript; "al"]

[Edited on 3.8.13 by bfesser]




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[*] posted on 3-2-2012 at 15:05


I finnaly got my cinnabar , It is a fine red powder which is realy heavy.

Now I want opignon of every one for a prosses to make mercury metal from the cinnabar.

Thanks!!!




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[*] posted on 7-2-2012 at 16:31


Today I tried the famous silver tarnish removing experiment which is: ading a silver piece on Al paper in a NaHCO<sub>3</sub> sol.

Reaction (without intermediate) :

3 Ag<sub>2</sub>S + 2 Al --> 6 Ag + Al<sub>2</sub>S<sub>3</sub>

So I tried the same thing but replacing the Ag<sub>2</sub>S by HgS + C powder (for electrical conductivity) And I aded boiling hot NaHCO<sub>3</sub> sol. and there is no reaction... How can I make this process work?HgO battery use HgO + C powder as the anode and zinc powder as the cathode.

Thanks all for your support! I need help!

Edit: maybe the cinnabar and the carbon was too coarse...


Now I will attempt this process:
http://www.google.com/patents?id=miQ4AAAAEBAJ&pg=PA2&...

[Edited on 8-2-2012 by plante1999]

<!-- bfesser_edit_tag -->[<a href="u2u.php?action=send&username=bfesser">bfesser</a>: rxn. eqn. cleanup]

[Edited on 3.8.13 by bfesser]




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[*] posted on 8-2-2012 at 04:19


This method would be easier and not involve high temperatures and boiling mercury:
HgS+AcOH (or any other acids forming soluble mercury salts)====>Hg acetate+H<sub>2</sub>S (do this outside or in a fume hood!), then add Cu, Fe or any other non-noble metal to precipate Hg/electrolyse the solution. Then pour off the water in the solution when finished.

<!-- bfesser_edit_tag -->[<a href="u2u.php?action=send&username=bfesser">bfesser</a>: subscript]

[Edited on 3.8.13 by bfesser]
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[*] posted on 8-2-2012 at 05:18


... I have heard that cinnabar disolve in Cl<sub>2</sub>/HCl sol. , maybe I will try this...

[Edited on 8-2-2012 by plante1999]

<!-- bfesser_edit_tag -->[<a href="u2u.php?action=send&username=bfesser">bfesser</a>: subscript]

[Edited on 3.8.13 by bfesser]




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[*] posted on 8-2-2012 at 05:24


That would work, but only 7 grams of mercuric chloride is soluble in 100mls of water at 20 degrees celsius.
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[*] posted on 8-2-2012 at 06:41


If you are precipitating mercury from a solution of its salts, be sure to use a metal that does not amalgamate with the mercury, like iron.



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[*] posted on 8-2-2012 at 07:22


Quote: Originally posted by LanthanumK  
If you are precipitating mercury from a solution of its salts, be sure to use a metal that does not amalgamate with the mercury, like iron.

Mercury doesn`t amalgamate with iron thats why it is used here.

Mercury amalganation of gold
Quote:

Never try to distill (retort) Mercury in a glass retort, as it will shatter. Mercury retorts are made of strudy iron.


The tip with not using glass might be worth to be considered.
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[*] posted on 8-2-2012 at 07:57


Don't try chemical reduction of HgCl<sub>2</sub> with iron in aqueous solution, it doesn't work. The only thing you'll get is Hg<sub>2</sub>Cl<sub>2</sub>, a white powder which is insoluble and won't further react with the iron.
I have had enough opportunity to mess around with the aqueous chemistry of mercury during my experiments with dental amalgams. It is a huge headache. Always avoid bringing Hg into aqueous solution if possible! Mercury is best isolated and refined by distillation.

The method that I would choose if I had to make Hg from HgS is distillation with iron filings. Use an excess of iron, mix well with the HgS and put some extra iron above the mix before distilling.
HgS will sublimate unchanged (pitch black sublimate with red spots) if the vapors don't contact a reducing metal.
Distill in a long horizontal test tube stoppered with glass wool under the fume hood. The Hg will collect as droplets in the upper, colder area of the test tube. This is how I distilled the Hg from my amalgams.

<!-- bfesser_edit_tag -->[<a href="u2u.php?action=send&username=bfesser">bfesser</a>: subscript]

[Edited on 3.8.13 by bfesser]




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[*] posted on 8-2-2012 at 11:26


This was my setup that I used to distill mercury from dental amalgams- the pictures are from 2006!
I would still do it the exact same way today if I had to work on this scale. This was a batch of 20g amalgam, yielding 10,6g mercury.

Test tube with added "step" to physically separate the amalgams and condensation space, stoppered with cork and glass wool:
Amalgame1.jpg - 61kB

Close-up:
Amalgame-2.jpg - 42kB

After starting to heat the amalgams with the burner, mercury is beginning to condense:
Hg-Kondensation.jpg - 47kB

Distillation finished:
Destillationsende.jpg - 46kB

Mercury coalesced by tapping and swirling the test tube:
Hg-recycled.jpg - 46kB

The test tube was heated with a bunsen burner at full power, and the cooling was entirely convective. No mercury escaped, I obtained a near 100% yield.




[Edited on 8-2-2012 by garage chemist]




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[*] posted on 8-2-2012 at 11:47


Brilliant as usual garage chemist. I was wondering how you were keeping the reactants and product separate in your "long test tube."



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[*] posted on 8-2-2012 at 11:59


The amalgam residue (mainly Ag and Sn, with some Cu) sintered together to form a hard cake, which wasn't even wetted by the Hg any more after cooling. I used the highest possible heat (dull red incandescence) towards the end of the distillation.
The "step" that I formed into the test tube through softening in a flame did a good job of keeping residue and distillate apart.
In this test tube I distilled the Hg from all my 180g of amalgam residues.
By the way, this is the exact same setup that I have used many times to make white phosphorus from red.




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