Sciencemadness Discussion Board

Refining mercury from cinnabar

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plante1999 - 3-12-2011 at 05:35

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I know that oxidizing cinnabar HgS make mercury and SO<sub>2</sub> but does somebody know a leach for leaching mercury out of it and precipitate the mercury? I want mercury to make sodium hydroxide from electrolisis and disolve gold plating...

Thanks!!!!

Please check my website in the signature!!!

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blogfast25 - 3-12-2011 at 06:22

My advice? Just don't do it unless you can buy some mercury and can use it safely.

You don't really need mercury to make NaOH and you really don't need to make NaOH as you can buy it just about anywhere.

To dissolve gold plating as an amalgam also requires being able to safely distill off the mercury to recover the gold. Are you equipped for that?

plante1999 - 3-12-2011 at 06:34

I am not intended to distill the mercury , I will disolve the mercury in nitric acid to get the gold and re-precipitate the mercury.

Endimion17 - 3-12-2011 at 10:40

Don't do it. You'll end up with at least strong acute poisoning. Dude, that means roasting cinnabar. Essentially, boiling mercury.

And the idea to make homemade lye using mercury cathode... OMG just stop right there.

plante1999 - 3-12-2011 at 10:45

Ok I won't do it... But does someone know where i can get 5-10ml of mercury metal? I can not paid more than 40$ for it.

I have found this at this time:
http://www.ebay.ca/itm/50pcs-glass-electric-Mercury-Tilt-Swi...

[Edited on 3-12-2011 by plante1999]

[Edited on 3-12-2011 by plante1999]

Endimion17 - 3-12-2011 at 11:00

The cheapest source are old mercury sphygmomanometers. Not old enough to be considered expensive vintage equipment, but old enough to be considered crap. They contain around the volume you need.

Or go to Kyiv with a sturdy bucket and a pair of very strong guys. :D

plante1999 - 7-12-2011 at 07:24

(I will not do it) But if I dry distill HgS with KClO<sub>3</sub> , MnO<sub>2</sub> or Ca(ClO)<sub>2</sub> and a condence the vapor in a CH<sub>3</sub>OH/H<sub>2</sub>O sol cooled in a Ice/HCl bath (-30 degree C) does it will make liquid mercury?


Thanks!!!

[Edited on 7-12-2011 by plante1999]

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blogfast25 - 7-12-2011 at 07:44

That’s quite an interesting question, actually! And I’ve no clear idea of the answer.

KClO<sub>3</sub>: that releases oxygen from about 400 C, whether that temperature is enough to convert HgS to HgO + SO<sub>2</sub> I’m not sure…

MnO<sub>2</sub>: SO<sub>2</sub> is actually capable of reducing MnO<sub>2</sub> in watery media to Mn (II), that’s one way of extracting MnSO<sub>4</sub> from battery gunge. But here the MnO<sub>2</sub> would have to oxidise sulphide to SO<sub>2</sub> first, which would then escape. Hmmm…

Ca(ClO)<sub>2</sub>: in watery media hypochlorite is certainly capable of oxidising sulphide to sulphur, even to sulphate apparently.

There are other oxidisers that could be considered (KMnO<sub>4</sub> and K<sub>2</sub>Cr<sub>2</sub>O<sub>7</sub> for instance).

This could be worth trying on a very small scale, provided you have adequate means to capture any formed Hg. A small test tube with a cooled (open) end would probably be enough to condense the small amounts of mercury…

I would google this thoroughly first. I suspect that the fact that there seem to be no youtube vids demontrating this possibly provides an answer to your question, though! :(

[Edited on 7-12-2011 by blogfast25]

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plante1999 - 7-12-2011 at 09:04

I have found an interresing link here , one cleam that HgS can be reduced with Fe or CaO.

http://www.chm.bris.ac.uk/webprojects2004/hooper/extraction....

EDIT:
I have read more pages and it seam that Hg could be leached from HgS with tincture of iodine ( KI , I<sub>2</sub>;)....

8 HgS + 8 KI + 8 I<sub>2</sub> --> 8 K<sub>2</sub>HgI<sub>4</sub> + S<sub>8</sub>

Generaly mercury is extracted when HgS is reacted with oxygen and condencing the mercury so , there is probably a chance that other oxydiser work.

HgS + O<sub>2</sub> --> SO<sub>2</sub> + Hg


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blogfast25 - 7-12-2011 at 09:23

Both reactions:

HgS + Fe → Hg + FeS
4 HgS + 4 CaO → 4 Hg + 3 CaS + CaSO<sub>4</sub>

… also require high temperatures to get started (or so I believe) which brings us back to not poisoning yourself with mercury vapours.

When you first popped your question, I was inclined to consider watery electrolysis of a HgCl<sub>2</sub> or Hg(NO<sub>3</sub>;)<sub>2</sub> solution, because at least that would avoid any mercury vapour at all. Whether the formed mercury would coalesce into liquid mercury I don’t know (but I suspect it does). Here’s one reference from the Journal of the American Chemical. Society that clearly suggests it is possible.

Bear in mind that cinnabar in terms of toxicity is a child’s toy compared to water soluble mercuric compounds…


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unionised - 7-12-2011 at 11:37

Quote: Originally posted by plante1999  
(I will not do it) But if I dry distill HgS with KClO<sub>3</sub>, MnO<sub>2</sub> or Ca(ClO)<sub>2</sub> and a condence the vapor in a CH<sub>3</sub>OH/H<sub>2</sub>O sol cooled in a Ice/HCl bath (-30 degree C) does it will make liquid mercury?

I'm fairly sure that most sulphides are combustible and you plan to mix them with a strong oxidant, then heat the mixture.
Are you trying to win a Darwin award?

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blogfast25 - 7-12-2011 at 12:37

Quote: Originally posted by unionised  
I'm fairly sure that most sulphides are combustible and you plan to mix them with a strong oxidant, then heat the mixture.


Inorganic sulphides like HgS or FeS<sub>2</sub> require loads of air oxygen and high temperatures + time to convert ('combust' if you prefer). Would you class these as 'combustibles'?

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unionised - 7-12-2011 at 13:43

Pyrites certainly burns.
Things like coke and coal "require loads of air oxygen and high temperatures + time to convert ('combust' if you prefer)."

I would class these as "combustibles".
Ferrous sulphide is sometimes pyrophoric
Mellor lists the reaction of copper sulphide with the chlorates of magnesium, zinc or cadmium as explosive.
(1965 vol 2 suppl 1 P584 if my copy of Bretherick is to be believed)

[Edited on 7-12-11 by unionised]

blogfast25 - 7-12-2011 at 14:00

Runaway oxidation of CuS (and by extension HgS) could lead to very quick formation of SO<sub>2</sub>, thus explosion if contained. Plausible.

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Steve_hi - 7-12-2011 at 16:32

Hi plante go to a used building supplies and try to buy mercury heat controll thermostat

plante1999 - 7-12-2011 at 18:06

Quote: Originally posted by unionised  


I'm fairly sure that most sulphides are combustible and you plan to mix them with a strong oxidant, then heat the mixture.
Are you trying to win a Darwin award?


I will not win an darwin award. I do safely my experiments ,and I am not intended to kill me, but I want some mercury so I will find a SAFE process to get some.

blogfast25 - 8-12-2011 at 07:13

For:

HgS(s) + 2/3 KClO<sub>3</sub>(s) === > Hg(l) + SO<sub>2</sub>(g) + 2/3 KCl(s)

… the Standard Enthalpy of Reaction is about - 264 kJ/mole of HgS (*). That’s quite a lot and it’s likely that once the reaction has been initiated it will briskly sustain itself with liberation of vaporous Hg (and of course gaseous SO<sub>2</sub>;). It would be worth trying this on a very small scale, using a long or extended test tube, OUTSIDE and standing upwind from the experiment.


(*) All data for Standard Enthalpies of Formation by Wolfram Alpha.

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plante1999 - 8-12-2011 at 09:06

I thinked to something interressing , why not reduce HgS powder with Al or Zn powder ... It could self sustain and make mercury vapor that can be condensed.

2 Al + 3 HgS --> 3 Hg + Al<sub>2</sub>S<sub>3</sub>

Zn + HgS --> ZnS + Hg

[Edited on 8-12-2011 by plante1999]

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blogfast25 - 8-12-2011 at 09:54

Al<sub>2</sub>S<sub>3</sub> has quite a high HoF, about - 724 kJ/mole (Wolfram Alpha). The HoF of HgS (Wolfram Alpha) is only about - 58 kJ/mole. That puts the Standard Enthalpy of Reaction for that reaction at about - 183 kJ/mole of HgS. Quite hot still.

For ZnS Wolfram gives a Standard HoF of about - 200 kJ/mole, thus for that reaction the Standard Enthalpy of Reaction would be roughly - 150 kJ/mole of HgS reduced. That's quite manageable and could be 'tamed' even further by adding a heat sink. In this case ordinary fine sand could be used, as neither zinc nor mercury are even remotely capable of reducing silica. This is definitively worth test tubing with a small quantity... Zinc powder would be required.


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plante1999 - 13-12-2011 at 09:04

Does somebody have cinnabar powder for making the test? If nobody can I will buy some in a few weeks.

vmelkon - 23-12-2011 at 10:42

Who sells cinnabar?
You could of course make it by mixing Hg and S but I'm getting the impression that you want the Hg. The best thing to do is to by a sphygmo...whatever it is called from ebay. They cost around 35$. Make sure you buy the "vintage" ones.
You can even find some for 10$.

When I bought it, it gave me 60 g of Hg.

jsc - 23-12-2011 at 12:14

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.


plante1999 - 23-12-2011 at 18:32

Cinnabar can be bougth on ebay.... I did touched a late and machined an small engine cylinder.


Neil - 23-12-2011 at 18:48

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.



Spoken like one who has snuffed far to much Hg in their lifetime.

vmelkon - 24-12-2011 at 05:22

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.



You don't need to insult people.

Making NaOH with a starting material of CaCO<sub>3</sub> is a big waste of time. You have to heat it to some high temperature and for a good while to allow it to decompose to CaO. Then the biggest problem = Ca(OH)<sub>2</sub> doesn't dissolve much in water. Then you have to dry it. NaOH is very hygroscopic. Even if you heat it to dryness, it will react with your glassware (presuming you are using glassware).

I have attempted to make KOH using mercury. It is an interesting experiment but again, a big time consumer.

If you need kilogram quantities of NaOH, I know a place in Montreal. I bought 4 Kg for 27$ taxes included. It is used for making soap.

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blogfast25 - 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]

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blogfast25 - 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]

plante1999 - 24-1-2012 at 16:25

I will buy this in a few day:

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

Bot0nist - 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]

neptunium - 24-1-2012 at 16:47

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

plante1999 - 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

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plante1999 - 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]

neptunium - 26-1-2012 at 09:55

cool ! let us know how it goes

blogfast25 - 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... :(

plante1999 - 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!!!

vmelkon - 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.

vmelkon - 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.

plante1999 - 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.

plante1999 - 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>.

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plante1999 - 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!!!

plante1999 - 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]

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weiming1998 - 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.

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plante1999 - 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]

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weiming1998 - 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.

LanthanumK - 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.

Organikum - 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.

garage chemist - 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.

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garage chemist - 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]

Magpie - 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."

garage chemist - 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.

plante1999 - 8-2-2012 at 13:56

Thanks for the idea!!! For 50g of cinnabar which size of test tube should I choose? ( I will buy this, since my cinnabar is pretty used....)

http://www.ebay.ca/itm/Powdered-Cinnabar-Crystal-50-g-Lot-Na...

[Edited on 8-2-2012 by plante1999]

garage chemist - 9-2-2012 at 10:45

I used a 18*180mm test tube for the 20g amalgam batch, and I'd recommend this size.
I wouldn't try to react all 50g cinnabar at once- make a few smaller batches out of it, that way you won't lose everything if the test tube breaks, and you can improve your setup if it goes wrong the first time.

The test tube MUST be made of borosilicate glass (Pyrex,
Boro 3.3, Duran, or similar brands of borosilicate glass- mine was a Schott Duran test tube), the ordinary thin-walled soda-lime glass test tubes like Fiolax WILL break if you try to use them for this purpose! I've had that happen to me.

Borosilicate test tubes are somewhat difficult to shape by flameworking without an oxygen-fed burner due to their high softening point. It's a good sign if you can just barely get the test tube to soften with a bunsen burner on highest heat- this shows that you've got the right kind of glass. If the test tube softens very easily and you can even melt a hole in it, throw it away and buy some higher quality glass.


plante1999 - 9-2-2012 at 15:44

Does extra-fine steel wool will work as the iron source? For the test tube and heating it is ok. by the way , where did you get your dental amalgam?

Thanks alls for your help!

garage chemist - 9-2-2012 at 20:23

I wouldn't use steel wool as the iron source, I'd think that proper mixing with the HgS could be a problem. You should get some fine iron filings first, or simply make them from a block of ordinary steel with a file.
However, you could put a little steel wool above the HgS + Fe mixture to react with any uncombined HgS vapor, and simultaneously act as a mechanical filter.

My surce of dental amalgams will remain confidential, and there's nothing more to be had. No dentist uses them any more anyway, so there's no source for any scraps.

[Edited on 10-2-2012 by garage chemist]

plante1999 - 10-2-2012 at 04:53

Thanks for the help! It will be somewhat long to make 14g iron powder with a file.... Sorry I did not want to be impersonal about your dental amalgam. I have about 7-10g of cinnabar left from my experiments how could I make a Al/HgS battery? something like that but replacing the pyrite with cinnabar: http://www.youtube.com/watch?v=gu27nYYrM4w

Cinnabar is non conductive , so should I grind it to fine powder and ad really fine carbon powder for conductivity?

Endimion17 - 10-2-2012 at 08:48

Quote: Originally posted by plante1999  
...
by the way , where did you get your dental amalgam?

Thanks alls for your help!




:D

garage chemist - 10-2-2012 at 10:12

Don't even think about asking a dentist for old amalgams that have been removed from patients teeth. These are held back in a gravity trap in the saliva suction device, and the stink from this sludge is unimaginable.
My amalgams were clean scraps from kneading the amalgam before inserting it into teeth. A fixed amount, e.g. 1g, of amalgam is prepared from a capsule containing alloy powder and liquid Hg, and the leftovers become rock hard after a short time, just like the filling itself.

plante1999 - 10-2-2012 at 17:36

I finnaly made Mercury metal from cinnabar!!! I took 3g of HgS (cinnabar) which I aded to the end of a test tube, then I aded 1.3g of steel wool on top of the cinnabar which is a great exess. I aded a rubber stoper with a hole on the end of the test tube. I made a setup where the end of the test tube was in snow and I heated to brigth yellow the steel wool end with a propane torch. The mercury condensed as a miror where the snow was. I tapped the test tube in a steel beer cap. The mercury was not coalessing so I aded dilute HCl to coaless it and it worked! I got about 0.2ml of mercury. I cannot weight it since it is too small.


Thanks all for your Help and support!!!


<img src="http://i1103.photobucket.com/albums/g469/plante1999/Photo002-2.jpg" width="600" />

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garage chemist - 11-2-2012 at 01:06

That's excellent to hear! Well done!
If you do this synthesis again, please make a picture of your setup before and after heating! I'd really like to see how the condensing mercury looks like when it is made from HgS + Fe instead of just being distilled from amalgams!
Also, please make a better picture of the mercury itself.
I'd also recommend that you redistill the mercury at least once when you have made somewhat more of it.

Endimion17 - 11-2-2012 at 02:16

Please don't encourage him to distill mercury. You have no idea how dangerous that is.

plante1999 - 11-2-2012 at 04:28

I will not redistill the mercury but I will make more from cinnabar ore. The next time I will make pictures. Im planning to react 62g of cinnabar in the next month which should give me about 4ml of mercury!! , this quantity is about what I need for making my own K,Na,Ce metal and then make hydroxide whith them. I am really happy with the results. So for making mercury from cinnabar you need steel wool, snow a test tube and stoper, propane torch and of course cinnabar.

(Now with my 0.2 ml I am making an amalgam with silver)

Thanks!

[Edited on 11-2-2012 by plante1999]

garage chemist - 11-2-2012 at 05:53

If you don't redistill the mercury, at least filter it by pressing it through a cotton plug with a syringe. It is most likely seriously impure. At least mine from the amalgams was, it formed a thick dusty oxide layer during storage.

Distillation of the Hg is not necessarily more dangerous than the preparation from cinnabar and iron- after all, it doesn't make a difference whether you are heating liquid Hg or a mixture of HgS and Fe, the result is concentrated mercury vapor in both cases, and whether this is dangerous depends on your setup and technique.

blogfast25 - 11-2-2012 at 06:10

You can purify mercury to some extent by keeping it under dilute nitric acid, I seem to recall a lab procedure consisting of dripping contaminated Hg through a column of SG = 1.1 HNO<sub>3</sub>. The contaminant metals mostly dissolve in the nitric, leaving behind purified mercury.

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plante1999 - 11-2-2012 at 06:17

In fact I purified my mercury from dilute (NH<sub>4</sub>;)<sub>2</sub>Cr<sub>2</sub>O<sub>7</sub> sol. and then i used it as a cathode in NaHCO<sub>3</sub> electrolite. I finnaly aded the mercury in distill water. It maked some effervessence, when the effervessence stoped the mercury was shining as a mirror, in fact I can see me on the droplet. this is a modified brauer process, brauer use KMnO<sub>4</sub>.

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garage chemist - 11-2-2012 at 09:32

On German Ebay there is a seller offering raw cinnabar ore rocks from Almaden, Spain by the kilogram:
http://www.ebay.de/itm/Zinnober-Almaden-Spanien-1-kg-verschi...
This is the stuff from which most of the mercury in use worldwide is being produced.
However, as the text states, this isn't pure cinnabar but rather the cinnabar-bearing rocks dug up from the ground in the mine.
I had a look in Ullmann's Encyclopedia under mercury and recent production figures from Almaden state that about 35kg of mercury are being produced from 1 metric ton of ore, e.g. the average mercury content of the ore is just 3,5%!
With 1kg of the ore costing EUR 25 plus shipping and only 35g mercury to be expected this is an expensive way to get mercury. Of course, 3,5% is just the average ore grade, this material could be a higher grade- ores from Almaden can reach 5-10% Hg and more.
Also, the large dilution of the HgS with rock means that the distillation with iron is not viable. Instead, the ore either has to be crushed and milled finely and the HgS enriched by flotation, or the crushed ore subjected to roasting with addition of air for the reaction that forms Hg and SO<sub>2</sub>.

The roasting process could be advantageously carried out in my tube furnace- a slow stream of air being pumped in by an aquarium membrane pump on one side, and the offgas led through a condenser to get the Hg.
I already have enough mercury for all my needs, so I don't need to do this, but it would be interesting nonetheless to find out how much mercury this ore contains so that other chemists who might be in need of mercury can decide for themselves whether they should make their own mercury from this material.
After all, metallic mercury is practically unavailable today except for tiny amounts from old thermometers.

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plante1999 - 11-2-2012 at 12:51

I tryed few way to make mercury from cinnabar.

Granular NaClO<sub>3</sub> + HgS: burn like flash powder when heated and release SO<sub>2</sub> + a wird gray-black coat that does not look like Hg

HgS + Air : just sublime the HgS... make a black coat of HgS.

Al + HgS : Make mercury that make black cinnabar, probably the hydrolisis of Al<sub>2</sub>S<sub>3</sub> make H<sub>2</sub>S

I tried them whith 0.1g of Cinnabar each.

[Edited on 11-2-2012 by plante1999]

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barbs09 - 12-2-2012 at 06:23

Hello, a slightly off topic but never-the-less related mercury question I would like to ask of the board: I have access to a good kg plus of mercury and would like the possibility of transporting it overseas to where I live. Shipping the liquid metal is out of the question for me, but I thought about amalgamating it with Zn powder and shipping (not aircraft) it as a plug of silver-grey coloured metal. Would this be considered a stable/inert enough form for shipping? Does anyone have any better ideas for rendering Hg more inert and passive for shipping purposes? Reacting with sulphur is also a possibility which would create material of cinnabar composition.

I am not interested in doing anything that would put anyone or any vessel at risk, nor myself in hot water.

Thoughts appreciated, Cheers ;)



bfesser - 12-2-2012 at 06:49

Just a thought, but it may be easier and safer to just find a local source.

plante1999 - 12-2-2012 at 08:07

I dont think it is a great idee to ship 1kg of Hg over sea.... Dont even think to amalgamate it with Zn , The Zn release H<sub>2</sub> on contact with H<sub>2</sub>O when amalgamed.

Zn + H<sub>2</sub>O --> ZnO + H<sub>2</sub>

[Edited on 12-2-2012 by plante1999]

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plante1999 - 12-2-2012 at 12:18

I made some mercury today from 9g of cinnabar and 5g of steel wool. here somme picture:

This is the set up

<img src="http://i1103.photobucket.com/albums/g469/plante1999/Photo004-2.jpg" width="600" />

I wanted to post a picture of the condensed mercury but the picture was realy black so I will not post it

Some picture of the mercury metal:


<img src="http://i1103.photobucket.com/albums/g469/plante1999/Photo008-1.jpg" width="600" />


<img src="http://i1103.photobucket.com/albums/g469/plante1999/Photo009-1.jpg" width="600" />

The reduction gave me 6g of mercury metal which is not bad.

In the futur weeks I will make more mercury, I hop the pictures will be betters.

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Endimion17 - 12-2-2012 at 13:03

Quote: Originally posted by plante1999  
...
So for making mercury from cinnabar you need steel wool, snow a test tube and stoper, propane torch and of course cinnabar.

(Now with my 0.2 ml I am making an amalgam with silver)

Thanks!

[Edited on 11-2-2012 by plante1999]


And a place to stay upwind.



Quote: Originally posted by garage chemist  
If you don't redistill the mercury, at least filter it by pressing it through a cotton plug with a syringe. It is most likely seriously impure. At least mine from the amalgams was, it formed a thick dusty oxide layer during storage.

Distillation of the Hg is not necessarily more dangerous than the preparation from cinnabar and iron- after all, it doesn't make a difference whether you are heating liquid Hg or a mixture of HgS and Fe, the result is concentrated mercury vapor in both cases, and whether this is dangerous depends on your setup and technique.


It is more dangerous because you have to heat the whole amount of mercury in the first tank which, if breaks, releases a stream of hot, gassing mercury. There's a video on YouTube where few guys try to distill it using an all glass apparatus. Unimaginable stupidity, on video!
Mercury is heavy, and boiling mercury, bumping, can shatter the apparatus. That simply must not happen because that would create a huge contamination of the whole room, enough for a serious hazmat scenario.

Of course, if one has steel equipment, pretty much all there is to worry about is the direction of wind.

Resonable purification can be done by agitating it few minutes with dilluted sulphuric and hydrochloric acid, leaving it overnight under the mixture, and then decanting with tap water. Next, metabisulphite bath to reduce any oxidized mercury in the disgusting layer covering the bulk metal. Short agitation with dilluted nitric acid can improve the purity. More goo could form, so again, metabisulphite bath, rinsing with tap water, then distilled water and drying with filter paper in the end.
I did that with my samples few years ago. They're stored in closed plastic containers. Still shiny. I've filled few instruments with it. No problems so far.



Quote: Originally posted by barbs09  
Hello, a slightly off topic but never-the-less related mercury question I would like to ask of the board: I have access to a good kg plus of mercury and would like the possibility of transporting it overseas to where I live. Shipping the liquid metal is out of the question for me, but I thought about amalgamating it with Zn powder and shipping (not aircraft) it as a plug of silver-grey coloured metal. Would this be considered a stable/inert enough form for shipping? Does anyone have any better ideas for rendering Hg more inert and passive for shipping purposes? Reacting with sulphur is also a possibility which would create material of cinnabar composition.

I am not interested in doing anything that would put anyone or any vessel at risk, nor myself in hot water.

Thoughts appreciated, Cheers ;)




That's around 3/4 of a decilitre. Why can't you ship it over the sea, using s ship? :)
It shouldn't be so expensive.



Quote: Originally posted by plante1999  
I made some mercury today from 9g of cinnabar and 5g of steel wool. here somme picture:

(...)



Here's an advice. Use macro on your camera. :)


Quote:
The synthesis gave me 6g of mercury metal which is not bad.

In the futur weeks I will make more mercury, I hop the pictures will be betters.


Analysis. It's impossible to chemically synthesize elements. ;)

plante1999 - 12-2-2012 at 13:07

The word synthesis is Edited. Thanks for remmenbering me that!

[Edited on 12-2-2012 by plante1999]

garage chemist - 12-2-2012 at 13:53

On the german forum, two members distilled 1kg mercury in an all-glass vacuum distillation setup, the kind that is used for general vacuum distillation of e.g. organic compounds.
This is not "unimaginable stupidity", but reasonably safe, just like vacuum distillation of other toxic compounds.
Boiling mercury does not bump. It boils smoothly even in vacuum, as these members have found out, and boiling capillaries are unnecessary.
I can search for the pictures if you want.

Endimion17 - 12-2-2012 at 16:28

Mercury does bump at 1 atmosphere. I know because I've tried to boil it outside.

It is stupidity. Perhaps unimaginable is too harsh of a term, but it is very stupid.
I'm talking about this.
http://www.youtube.com/watch?v=PwbM5ZxVBzk
http://www.joshianlindsay.com/index.php?id=85
Almost 3.2 kilograms of mercury for each of three distillations.

Mercury boils at over 350 °C, which is perhaps exceeding the safe temperature for air condensers. But they use a Liebig condenser... filled with cooled water. They were extremely lucky, it could've bursted so easily. Liebig condensers with cold water aren't designed for such scenarios. Borosilicate glass shouldn't experience rapid temperature changes over the 150 degrees interval. Just imagine, their cooling water was probably lower than 10 °C, and mercury vapor is 356 °C. That introduces a lot of strain in the glass, and especially in its joints.

They didn't have any collecting plates beneath the apparatus. If the distillation flask had broken, the hot, boiling metal would flow through the heating mantle and spill over the table and on the floor. Just imagine what kind of contamination that is. It's horrifying!

Also, they keep a shitload of mercury in a regular glass reagent bottle. It's a rule to keep small amounts in bottles with thick glass walls, or in plastic bottles. Otherwise, the bottom can fall off.

And in the end, there's a ton of methanol in an open bowl, evaporating in the room. A real treat.

Now, if this isn't fucking stupid, I don't know what is.
Mercury is distilled in steel distillation systems.
Cinnabar is roasted in such systems, too.

I mean, come on, these are laboratory basics and common sense.
I didn't learn my chemistry from Youtube, but from books and practice and thinking "I might be wrong, let's see what smarter and older educated people think by checking in laboratory manuals".

Learning shit from Youtube introduces a lot more chance to learn something wrong, and Internet is not selective. Errors spread around.

[Edited on 13-2-2012 by Endimion17]

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plante1999 - 12-2-2012 at 16:54

I totally approuve this. This is why if someday I distill my mercury I will do it in steel welded pipe so there will be no leak and the steel is not suposed to break.

Edit: I will probably try this reaction:

4 CaCO<sub>3</sub> + 4 HgS --> 4 CO<sub>2</sub> + 3 CaS + CaSO<sub>4</sub> + 4 Hg

Calcium carbonate is easier to get than Iron powder...
This is a varient of a process that I saw in many documents.

[Edited on 13-2-2012 by plante1999]

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mr.crow - 13-2-2012 at 10:22

He MELTED the fuse in his hotplate

No suckback trap

Mercury crud everywhere

He even has a Darwin logo on his website *facepalm* Darwin Award!

vmelkon - 15-2-2012 at 11:38

Isn't it bad to have teflon at the joints? I've heard teflon expand quicker than borosilicate and could cause a break.

Also, I'm quite shocked at the amount of mercury those guys have. They say they are doing a job for someone so i guess a company gave it to them so that they would distille it and return it back.

Endimion17 - 15-2-2012 at 16:55

It's teflon tape, it's ok. It's pretty much the only right thing they did.
I doubt it was a company. Probably someone's private batch. A company would've done it professionally. There's simply too much of it.
I can literally imagine my anxiety while carrying that large reagent bottle, waiting for the bottom to fall off and bathe me like Terminator. Man, they're out of their minds.

plante1999 - 1-10-2012 at 04:06

I have bought another 100g of finely powdered cinnabar and I will make more mercury using different process such as air roasting, calcium carbonate reaction etc. Yield will be calculated and Air roasting process will be documented in my short book that should be online soon named:

Lab scale industrial process
For lab synthesis 2012

Plante1999

I will keep you informed!

Eddygp - 2-10-2012 at 13:00

I would love to be able to distil mercury. However, my equipment is a bit rudimentary and it may be dangerous.

neptunium - 8-12-2012 at 19:02

yesterday i boilled some cinnabar and conc nitric acide (just to see if i could ..)
and some water.
i got a little bit of fizzing ( thinking it was H<sub>2</sub>S bubbling up) but then after cooling i obtained this yellowish oily residue and a faint smell of sulfur
(not rotten eggs !)
but still not reaction from the cinnabar...

i thought maybe...HgS + 2 HNO<sub>3</sub> = H<sub>2</sub>S(g) + Hg(NO<sub>3</sub>;)<sub>2</sub>
since one of the product leaves the reaction shouldnt the reaction take place?
any help/thoughts?

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plante1999 - 9-12-2012 at 04:09

Generally, when sulphides are dissolved in nitric acid, it yield a nitrate salt and sulphur. You would be better to extract liquid mercury from the cinnabar, purify it, and then react it with the nitric acid.

neptunium - 9-12-2012 at 04:13

well yes that was exactly what i was aiming for! but it didnt happen!

plante1999 - 9-12-2012 at 05:31

I guess the yellow thing is sulphur, no? What is your desired product, and how much cinnabar do you have?

neptunium - 9-12-2012 at 05:35

if it is indeed sulphur then the reaction is painfully slow even at boilling point and needs constant re addition of acid/water..
i have about 50 g of cinnabar only about 1-2 grams were involved in this .
how did i arrived at S8?

my goal is to produce Hg with wet chemistry i dont want to roast the thing ....(too many kids live down wind)

neptunium - 24-12-2012 at 16:11

as previously mentioned, i was looking for a way to isolate mercury without roasting .

a wet chemical way was suggested elegantly by Plante1999.

72g of NaOH were added to 9.6 g of finely powdered sulfur and 200 ml of boiling water.

mercury I.jpg - 49kB

the solution remained yellow for a while and then turned deep orang/redish

mercury II.jpg - 50kB

after cooling 48.8g of cinnabar were added


strong stiring is apply when adding aluminum powder (or foil)

not too much just a little at the time ...or this will happen

mercury III.jpg - 62kB

when no more cinnabar is visible, i obtained a slushy metallic goo of aluminum and mercury alloy

mercury IV.jpg - 37kB

a dilute solution of KMnO<sub>4</sub> brings the bright color of metal back
after several cleaning [HNO<sub>3</sub>] is added cleaned and HCl finish the job.

mercury V.jpg - 44kB

when no more bubbling is apparent, i had 37g of clean mercury metal.


i arrived at a 75.5% of what i put in which is pretty good for a sloppy chemist like me!

mercury VI.jpg - 44kB

this reaction was thought of by Plante1999 and sudgested as a mean to obtain mercury from cinnabar through a wet process

this reaction is very eficient and deserve attention although not practical on an industrial scale because of the amount of waste chemicals being produce but on a lab scale is fast cheap and generate good purity mercury.

thanks to plante1999 for the idea


oh and merry chrismas to all...


[Edited on 25-12-2012 by neptunium]

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neptunium - 26-12-2012 at 15:56

i must add that the mercury had to be THROUGHLY rinsed with water to eliminate all remaining traces of acid
otherwise it will form crystals and loose its shine..

neptunium - 29-12-2012 at 15:54

ran the experiment again and combined the total Hg...

over 80g of mercury metal! and pretty shiny and pure!



mercury T2.jpg - 37kB

garage chemist - 30-12-2012 at 11:26

That's a very interesting method neptunium. Good to see that there is also a viable wet chemical method to prepare mercury from HgS.
What you're doing is forming a solution with thiomercurate anions and then reducing this with aluminium.
The purity of the mercury thus obtained should be checked, as many of the possible alloying elements in aluminium foil could stay with the mercury.

plante1999 - 30-12-2012 at 11:33

Well, I thought/ tried this process few month ago based on something pretty vague I read somewhere. When I saw that neptunium was in need of an wet method, because he didn't wanted to make mercury vapor. I told him my process in an U2U and some emails. I didn't posted it because it lacked of pictures, and some may have said that it was non working because they could not see picture of it.

There is not only the presence of element in the aluminium foil, but also in the ore itself, that generally contain gold, lead and arsenic. However the purifying process I recommended (which avoid distillation) should remove most metal which are less noble than mercury, leaving mostly the Ag and the Au in it. No test was done for the purity tough. (At least in my case).

elementcollector1 - 30-12-2012 at 12:30

Where do you buy powdered cinnabar?

plante1999 - 30-12-2012 at 17:29

On ebay there is a china supplier. Is name is Gaofudev.

I had very good service with him, but he is quite costly.

[Edited on 31-12-2012 by plante1999]

neptunium - 30-12-2012 at 17:57

yes thats the one i had the cinnabar from...i purified the mercury alloy with a dilute solution of KMnO<sub>4</sub> and then HCl conc.
it bubbles for as long as Al is present (about 30 to 45 min) and then rinse it with water and strong agitation for about 1 hour..

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S.C. Wack - 30-12-2012 at 18:50

You should check the composition of foil before saying this purification treatment will fix it. I think the treatment has to be done right (lots of shaking) in order to remove most contaminants (I've posted this), but it might not work here in any case.

Brauer recommends glass for distilling mercury (interesting method), and so do the Biltzes: Heat a mixture of 23 g. cinnabar and somewhat more than the calculated amount of iron filings in a small retort of difficultly fusible glass. The mercury distils into a small flask which serves as receiver. Yield, 16 to 18 g.

I keep my mercury in glass and used to have a big glass flask of it...just saying I didn't have a problem with the video, except they needed a shorter path and better insulation...if they didn't use water in the condenser someone would probably say they should have...though I wonder why it ended so soon...and whether they know how toxic mercury vapor is.

[Edited on 31-12-2012 by S.C. Wack]

neptunium - 31-12-2012 at 05:21

Quote: Originally posted by S.C. Wack  
You should check the composition of foil before saying this purification treatment will fix it.


Plante1999 uses foil i used pure very fine aluminum powder 500mesh. maybe i forgot to clarify that detail

plante1999 - 31-12-2012 at 05:29

In fact at the beginning I used foil, but the reaction was too violent, so I used 1/8 Al sheet pieces later on.

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PHILOU Zrealone - 6-1-2013 at 06:09

Quote: Originally posted by plante1999  
Edit: I will probably try this reaction:

4 CaCO<sub>3</sub> + 4 HgS --> 4 CO<sub>2</sub> + 3 CaS + CaSO<sub>4</sub> + 4Hg

Calcium carbonate is easier to get than Iron powder...
This is a varient of a process that I saw in many documents.


The following must be equal:
4 CaO + 4 HgS --> 3 CaS + CaSO<sub>4</sub> + 4 Hg
4 Ca(OH)<sub>2</sub> + 4 HgS --> 3 CaS + CaSO<sub>4</sub> + 4 H<sub>2</sub>O + 4 Hg

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Mercury Purification [lit.]

bfesser - 2-8-2013 at 12:40

Quote: Originally posted by blogfast25  
You can purify mercury to some extent by keeping it under dilute nitric acid, I seem to recall a lab procedure consisting of dripping contaminated Hg through a column of SG = 1.1 HNO<sub>3</sub>. The contaminant metals mostly dissolve in the nitric, leaving behind purified mercury.
I was a little bored, so I transcribed a few pages from a book in my personal library:
Quote:
<em><strong>Appendix 8</strong></em>

<div align="right"><em><strong>Purification and Decontamination of Mercury</strong></em></div>

&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;Dirty mercury contains dissolved metals, as well as organic materials, grease, oxides, and just plain dirt, which are usually found on top and in pockets trapped under the surface.
&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;The three steps in the purification process are: filtration, to remove grease, dirt, and some dissolved metal; oxidation, to remove base metals; and distillation, to remove noble metals.
&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;First, pass the mercury through a pinhole in a cone or funnel of filter paper or through glass wool to remove dirt and some dissolved metal. The heavy mercury falls through the pinhole, while dirt, oxide, and grease will stick to the paper and remain behind. As the mercury falls through the pinhole the surface layer in which metallic impurities are concentrated will contract. The impurities will concentrate further in the contracting surface and lower the surface tension so that the impure surface mercury does not pass through the pinhole. Each passage of mercury through a pinhole is equivalent to partial extraction. A dozen or so repeated filtrations will purify mercury sufficiently for most purposes. However, it is usually better to filter once or twice and then to remove most active metals by oxidation.
<table><tr><td>&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;This is done by forcing air through the mercury. The simplest apparatus is shown in Diagram I. Put a layer of 10&ndash;20% nitric acid over the dirty mercury and pull air through by an aspirator or vacuum line. The air will oxidize the base metal such as zinc, lead, etc., while stirring the mercury. The oxides will float to the top of the mercury and dissolve in the acid solution. The nitric acid will also oxidize any base metal at the mercury surface. The bubble rate should be fast enough to stir the mercury without splashing it into the side arm. The glass wool plug is present to protect the aspirator or vacuum line from acid droplets. Usually 8 hours of oxidation at the rate of two to three air bubbles per second will clean about 10 pounds of mercury.
&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;After the oxidation wash the mercury with distilled water. Then pass it through a pinhole in a filter paper to remove the last traces of oxides. For most purposes the mercury will now be sufficiently clean. For example, the gold, platinum, or silver still present will not affect routine density measurements or interfere with use in mercury contacts or seals.
&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;When very pure mercury is require, as in a polarography and in surface tension measurements, after the oxidation vacuum distill the mercury at 25&ndash;30 mm pressure. Use an all-Pyrex apparatus with a glass shield and distill in a hood in case the apparatus breaks.</td><td>diagram_I.jpg - 63kB</td></tr></table>

<strong>REMOVAL OF SPILLED MERCURY</strong>

&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;Spilled mercury on desk tops and in cracks in the floor is an <em>extremely dangerous health hazard.</em> Mercury vapor is poisonous, and if inhales attacks the nails, hair, teeth, brain, and kidneys. To avoid spillage, work with mercury over wide-mouth safety jars or pots. Place apparatus on trays so that if a container breaks and the mercury spills it will be caught. To remove or deactivate spilled mercury, use sequestering agents, chemicals which lower the vapor pressure of the mercury and convert it into a form that can be swept up. (Mercury splashes into droplets to small to be seen and too fluid to be swept up.)
&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;Cover the contaminated areas with either sulfur or some other sequestering agent, such as an organic sulfur compound. Sulfur, over an extended period of time, cuts down the vapor pressure by combining with the mercury to form solid mercury sulfide, which may be swept up. Organic sequestering agents do not contain free sulfur but hydrolyze to form H<sub>2</sub>S, which then reacts with the mercury. Dissolve the sequestering agent in water and wash the floors and desks with the solution. Vacate the room for a period of time to avoid the hydrogen sulfide, which is an even more deadly poison than the mercury. After the room is ventilated, sweep up the mercury sulfide.

&ndash; <em>Laboratory Course in Physical Chemistry.</em> Salzberg, Morrow, & Cohen. Second Printing, Academic Press, 1966. (<a href="http://books.google.com/books/about/Laboratory_course_in_physical_chemistry.html?id=jsc0AAAAMAAJ" target="_blank">Google Books</a> <img src="../scipics/_ext.png" />;)


[Edited on 3.8.13 by bfesser]

plante1999 - 2-8-2013 at 17:53

Thanks bfesser for the handy references. It will help keep member safe.

Very glad the thread is toped.

By the way, I didn't updated much this thread, but I did proceed a lot of cinnabar since my last reported try.

The process I invented/tried:

-Wet sulphur increased solubility aluminium reduction. (Personally developed)

It was very messy, and pretty violent, but the yield is good and no mercury vapors are involved. Mercury is of OK purity. Costly.

- Sodium/calcium carbonate, and heating, at low temperature the yield is very high and the mercury is of high purity, but as temp increase, the carbonate/sulphur mixture decompose back to sulphur which spoil the mercury. By far the best process if a careful chemist do it.

- Iron filling, give Good mercury, pretty easilly but is a mess to clean, very good for a sloppy chemist.

- Air oxidation (Look in lab scale industrial process 1). By far the cheapest and nice(st) to look at, mercury fog rising from the red cinnabar and driping back is simply the most beautiful thing I saw in my whole life honestly. Deal with heavy apparatus and mercury vapors.

-Aluminium/Zinc
EXTREMELY dangerous, explode making a quite loud sound, with moderating agent or filling burn extremely fast like cellulose hexanitrate making a dark coating of suspected mercury sulphide due to hydrolysis of the poor metal sulphide. it is beleived that the mercury is trapped in the sulphide(s).

-Wet process using aqua regia. Extremely costly. Dissolve cinnabar in aqua regia, filter and precipitate with copper. Gives very good purity Hg but mess with strong mercury solution. Best process for the riches out there.

starman - 2-8-2013 at 18:04

Hi plante. I see this a quick summary of some of the methods discussed in the thread and you have implemented yourself,
I wonder of you would mind putting a few hard figures on your yields. Further how did you characterise purity?
Surely you would not state 'high purity' just because product looks nice and shiny?

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