Sciencemadness Discussion Board

Refining mercury from cinnabar

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plante1999 - 2-8-2013 at 18:22

No, mercury WILL leave residue in the flask when distilling. High purity leave little to no residue and OK purity leave quite a bit of it. My way to characteristic purity without heavy analysis work.

All processes give more than 70%, and moss of then give 90%+ When done carefully I usually get 96% or so yield with most of theses. Thermal process give higher yields unless it is the aqua regia one, which give the best yield and purity of all the processes.

[Edited on 3-8-2013 by plante1999]

[Edited on 3-8-2013 by plante1999]

testimento - 2-8-2013 at 19:32

Cool.

Can you make elemental mercury from grounded cinnabar in a steel reactor heated over 600C with air pumped into? This would be the easiest way to procceed, and I read that there will be formed SO2 and elemental mercury in vapor form, which will condense and accumulate in the collecting flask.

Is mercury compatible with plain steel, carbon steel and 300 series stainless?

plante1999 - 3-8-2013 at 02:53

All yes, buy did you even read lab scale industrial process? And no, it would definitly not be the "easiest" way to proceed, you should read my resume.

testimento - 3-8-2013 at 13:47

Cool, I've got to check that. I aint got no much glassware, just basic distillation, separation, refluxing and filtering apparatus, mut I prefer to make my own equipment. For mercury reactor I just need to take 4" steel tube, weld a bottom to it and make the flange neck and flange plate and weld the condenser and air inlet for it, and its ready. 600C is easily reaced with normal propane burner, an air injected carbon bed would be uneccessarily powerful and a coke bed could even melt the reactor. Please see the picture.

mercpot.png - 18kB

starman - 4-8-2013 at 17:45

Quote: Originally posted by plante1999  
No, mercury WILL leave residue in the flask when distilling. High purity leave little to no residue and OK purity leave quite a bit of it.


OK thanks plante. Basically BP determination on a single distillation. Very good yields possible.

subsecret - 17-10-2013 at 12:49

This is an example of an amateur gold refining retort, used for separating gold from the amalgam. I assume that it could be used to separate sulfur and mercury. Testimento's "cup" design is much better than the one in the video, as the heat only passes through one surface.

http://www.youtube.com/watch?v=ShgM07O1rqQ

The use of a water trap might serve to clean the mercury that condenses . . . the water would form an acidic environment in the presence of SO2, and would help to clean the mercury. In my opinion, a two-stage steel condenser is the way to go, with the first stage being air-cooled and the second stage being water-cooled to condense any remaining mercury.

The gold rush (personified here) used massive amounts of mercury to extract gold. The ore would be crushed and shaken along copper sheets coated in mercury. The amalgam would then be heated to drive off the mercury, (usually) condensing in a tub of water.

The Spanish used to send criminals to work in cinnabar mines. Mercury is no joking matter, be very careful.

[Edited on 17-10-2013 by Awesomeness]

[Edited on 17-10-2013 by Awesomeness]

plante1999 - 17-12-2013 at 09:44

I just managed to buy 2kg of cinnabar dirrectly from china with the money donated recently and the personnal funds I had, in a month or so it should be here, and I will be able to do the final work, pictures, all the processes description and purification.

I also managed to buy a cheap chinese 10g 0.001g scale, so calculation should be quite precise.

plante1999 - 25-12-2013 at 08:46

I experienced with a new cinnabar type, not the usual granular mineral, it was a fine dust. Many problem arrised from that, but I have a few general recommendation to make before I thoroughly analyse the inconvenient of fine cinnabar, and it advantages..

In the sulphur/sodium hydroxide/aluminium process, there is serious problem if you lack of hydroxide ions in solution. It appear that if there is not enough hydroxide ion per sulphide, the mercury precipitate back... As black sulphide. It appear that the acidic condition precipitate the dissolved mercury. I have more research onto that. Secondly, Nitric acid do leach cinnabar very effectively when copper is added to generate NOx that aggressively oxidize the sulphide. However, if you want liquid mercury, you should calculate some excess and use a stochiometry based onto the fact that copper is a reactant too, because copper dissolve preferably in nitric acid then reducing the mercury solution. In my experience, the excess is sort of hard to calculate due to the many side reactions happening. After 2 or three day, the copper started to amalgamate, meaning the nitric acid had been consumed. The mercury by this method is impressively pure.

Aggressive HNO3/NOx leach based on nitrite + nitric acid + cinnabar yielded on cooling a white crystalline solid which I have to believe is mercury II sulphate.

Here is a reaction I hypothesized based onto mys results, take note there is certainly other side reactions.

14HNO3 + 3HgS -> 3Hg(NO3)2 + 3H2SO4 + 8NO + 4H2O

10HNO3 + HgS -> Hg(NO3)2 + H2SO4 + 8NO2 + 4H2O

8HNO3 + 3Cu -> 3Cu(NO3)2 + 2NO + 4H2O

4HNO3 + Cu -> Cu(NO3)2 + 2NO2 + 2H2O

Cu(NO3)2 + H2SO4 -> CuSO4 + 2HNO3

Hg(NO3)2 + H2SO4 -> HgSO4 + 2HNO3

S.C. Wack - 25-12-2013 at 09:42

Quote: Originally posted by plante1999  
a white crystalline solid which I have to believe is mercury II sulphate.


Obviously some sort of verification should be done. The mercuric nitrate/sulfide complex of yesteryear isn't ruled out.

plante1999 - 26-12-2013 at 06:02

Yes, of course it should be analysed, although in such conditions I doubt any sulphide persist, really.

plante1999 - 26-12-2013 at 14:53

BE WARN BE WARN!!!

Aliexpress seller bian sell fake cinnabar. The cinnabar I worked on in the last few days was not in fact cinnabar, at least very very very far from pure. I should always rely to the classical mineralogical test!

The open tube showed it, it contain much much less then a 1% Hg, the remainder being white mineral ash that is not silica, and a red dye. Don't get scammed, I just got scammed really really hard, 150$ for nothing. Buy from gaofudev on ebay, he is a legit seller.

jharmon12 - 3-1-2014 at 18:23

Quick question about buying cinnabar from gaofudev on ebay. I looked at his listings and he has high quality stuff, but you can buy mercury by the pound online for $186.00, purified. I know I saw it less than a year ago for $150.00/lb on another site, but can't find it right now. This guy gaofudev charges so much for his cinnabar, if you are going to just retort mercury to get mercury, why not just buy it from online at a place like: http://www.sciencecompany.com/-P16860.aspx?utm_source=google... ?

I am trying to figure out the reasoning here. Maybe I am not looking at a cheap enough sample on ebay? Where is the cheapest place to get cinnabar chunks or powder???

Thanks,

Joel

jharmon12 - 3-1-2014 at 18:29

Found it on Amazon from GalliumSource:

http://www.amazon.com/GalliumSource-LLC-Liquid-Mercury-454g/...

Less than $100 and free shipping. How cheap can we get cinnabar to save money making mercury? $100/lb seems pretty cheap.

Joel

jharmon12 - 3-1-2014 at 18:35

What about a shotgun recoil reducer. 1 lb of mercury for $43.00: http://mpcsports.com/stockmodel78x516oz.aspx

Joel

plante1999 - 4-1-2014 at 15:22

"why not just buy it from online at a place like: http://www.sciencecompany.com/-P16860.aspx?utm_source=google... ?"

I don't live in the US...

I doubt the recoil contain mercury, and if so, probably less then a pound.

The point is to buy material which is not hazardous, proceed it, which is fun, and store it. Although it is nice to make it cheaply, it is not exactly the point.

khlor - 4-1-2014 at 20:01

Quote: Originally posted by plante1999  
<div align="center"><img src="../scipics/_warn.png" /> <em>Mercury and it's compounds are <a href="http://en.wikipedia.org/wiki/Mercury_poisoning" target="_blank">cumulative neurotoxins</a> <img src="../scipics/_wiki.png" /> and <a href="http://en.wikipedia.org/wiki/Mercury_cycle" target="_blank">persistent environmental pollutants</a> <img src="../scipics/_wiki.png" />! Proceed at your own risk & <u>dispose of wastes responsibly</u>.</em> <img src="../scipics/_warn.png" /></div><br /><hr width="80%" />
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!!!

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

[Edited on 11.10.13 by bfesser]


you don't exactaly need mercury to this. you could use a diaphragma cell, I tryed using paper filter(those you use to make coffee) and worked. sodium hydroxide in one side of the cell, well... at least to the sodium hydroxide.

[Edited on 5-1-2014 by khlor]

My mercury experiment

jharmon12 - 7-1-2014 at 18:25

Hello.

Well, I tried to extract mercury from an ore sample sent to me from South America with an unknown vermillion content. I used the chemical process laid out by Neptunium in the "Mercury from Cinnabar" thread. I think there is so much other rock in the ore that I cannot separate it from the mercury that is likely present.

I know that using extreme heat and airflow is an option when processing cinnabar, but I was trying to figure out how the chemical process works first.

I started with 40 Ml of water and added about 10 grams of sodium hydroxide and 3 grams of sulfur and allowed it to turn into an orange-red liquid with heat and continuous stirring.

I then added 10 grams of cinnabar (ore) to the mix after it cooled, and allowed it to mix with a magnetic stirrer until it cooled off.

I added aluminum, 20 mesh flakes, until the heat and gas liberation was mostly done. After cooling, I didn't have any permanganate as recommended by Neptunium, so I added potassium dichromate in solution, as my understanding from the original thread was that this could also be used.

I am frustrated. The problem I am having is that Neptunium's description is so cryptic on how he "cleaned" the aluminum/mercury alloy, that I am not sure on how to proceed. He wrote a couple of sentences on using permanganate to clean it up and then using nitric acid, then finally some hydrochloric acid. But I cannot make heads or tails of what the details of this process might be.

So far, I have a 100 mL watery solution of what looks like black filth with some K2Cr2O7 added to it.

I sent a message directly to Neptunium and Platte, who is also involved with mercury experiments, but they are not responding and I want to continue with this project.

I would appreciate any feedback on how to proceed to separate the mercury from the rock dust I currently have in solution.

Thanks for any help you might be able to offer...

Regards,

Joel

plante1999 - 7-1-2014 at 18:53

I'm not answering eh...


You will now know from now on what is not answering, and my username is plante by the way.

Mailinmypocket - 7-1-2014 at 19:08

Neptuniums post is not cryptic at all. To clean amalgam you first need to have amalgam. Do you have amalgam?

Give a better idea of what type of mineral you are using, with zero description is it difficult to suggest a method to separate the vermillion/mercury from other components. Perhaps a photo of it? Also, if the amount of mercury containing mineral is unknown, are you sure it contains any and if so the amount might be so small that the method you are using is simply impractical.

Just a note; sometimes giving people time to respond to your U2U messages is worth the wait. Patience... Saying they aren't responding quickly enough to your liking in the thread is a tad inappropriate.

jharmon12 - 8-1-2014 at 06:09

Hi Mailinmypocket.

This ore is coming from a mine that extracts cinnabar, orpiment, and realgar. It was sent by someone that is working the mine and has access to the ore. The ore clearly has dots of red crystals of what appears to be vermillion throughout its matrix.

I followed Neptunium's description up to the point of adding the aluminum and I added it until the heat and gas release was minimal. From what I understand from reading Neptunium's description, adding the aluminum powder should have created an amalgam of mercury and aluminum. So, what I have is whatever the non-mercury ore content was, plus an amalgam of mercury/aluminum. So, the trick is going to be separating the two.

I am not sure a picture would do any justice, as what I have is simply a black "sludge" that has sunk to the bottom of the beaker in the water/K2Cr2O7 solution.

The issue, I think, is that all the experiments listed in this thread so far involved a known quantity of mercury, such as the dental fillings by garage chemist...or a very good sample of vermillion that yielded almost 100%, by weight, of mercury, as illustrated by Neptunium and Plante (accidentally forgot your name spelling earlier...my bad). My experiment involves the use of ore with an unknown quantity of vermillion in it. Furthermore, the content of the rest of the ore is unknown. Perhaps it is granite? I do not know.

I have the option of getting 20 more lbs of this ore, as a granulated powder, for $13/lb, but don't want to commit to this until I test this sample first to see how much mercury I can "squeeze" out of it. If it appears that I can get a decent amount of mercury out of it (probably around 50% or more), I will consider it worth it to buy all 20 lbs and use that as my personal mercury source going forward. Otherwise, I will just get my mercury in 1 lb quantities from Amazon.

So, that gives you a picture of what I am trying to accomplish and what the end goal is. Thanks for the help so far.

Regards,

Joel

[Edited on 8-1-2014 by jharmon12]

[Edited on 8-1-2014 by jharmon12]

jsc - 28-5-2014 at 12:55

Quote: Originally posted by blogfast25  
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]


By "Castner cell" I am referring to the cells used in the Castner-Kellner process which uses mercury.

S.C. Wack - 28-5-2014 at 13:53

Those cells can be super easy to make if you have enough mercury and some use for chlorine in salt water.

The site is called sciencemadness.

http://www.youtube.com/watch?v=xiqmEibSY0I

careysub - 9-12-2014 at 21:36

I hope we are not about to lose the cinnabar thread due to spam being appended to the end.

(Will this save it?)

Bert - 9-12-2014 at 21:46

Quote: Originally posted by careysub  
(Will this save it?)


Not to worry...

plante1999 - 6-1-2015 at 07:52

Quote: Originally posted by tibow64  

I suspect that the fact that there seem to be no youtube vids demontrating this possibly provides an answer to your question, though!


This has to be the dumbest thing I have heard in a while. It is not because no one made a youtube video that no one tried it. Most things are posted on forum, or are not posted on the internet at all when it comes to home chemistry.

BTW, I already burned cinnabar in a quartz tube with air flow, it works very well to yield mercury.

[Edited on 6-1-2015 by plante1999]

Mailinmypocket - 6-1-2015 at 08:08

This is the closest that YouTube (aka chemistry school for some) was able to find:

http://youtu.be/znQh7m2mkiQ

fusso - 10-5-2018 at 12:37

Is cinnabar rly that expensive?!

Texium - 10-5-2018 at 12:45

Is it rly necessary to bump a lot of old threads that have been inactive for years with useless one liners that add nothing interesting to the discussion?




Answer: no

Johnny Windchimes - 8-10-2020 at 15:32

My turn....

I looked through the whole thread and didn't see this electro process mentioned, so here it is:

I have successfully done this several times. First with 50 grams of Cinnabar from eBay, all the way up to 2 kilograms (stuff is 8.1 g/cm3; dense!).

Get yourself a 2 amp / 20 volt DC power supply and you're off!

My recommendations:

-Use two platinum electrodes. Needs to be made of something that both wont dissolve in the electrolyte, nor amalgamate with the elemental Hg.

-PURE tungsten welding electrodes are also a great choice, as tungsten does not form amalgams either. I have not personally used tungsten but if I do this again I shall try them. Try automotive supply and welding shops.

-CAREFULLY powderize (as best you can) the cinnabar. This can make dust thats obviously super bad to breath and bad in general to spread around. Mortar and pestle make a HUGE cloud in my experience; I used a small coffee grinder but that makes even smaller airborne "smoke" almost size dust particles when its opened.....

-Once its (cinnabar powder) in the mix of NaOH and sulphide, give it LOTS of time to dissolve into solution. Lots of stirring. After it has (or as much has dissolved as is going to), filter it with a coffee filter and a funnel. If you don't, the junk left over (impurities in the cinnabar, etc) can amalgamate with the newly formed Hg metal, and it just makes for a cleaner prep.

-Use a secondary containment device. I put the entire electro setup into a nice and big ol' plastic bin in case any spills happened.


Enjoy, because it does work!




Attachment: US1718103 - Cinnabar electrolysis to Hg - Copy.pdf (213kB)
This file has been downloaded 425 times Stoichiometry Calculations for Hg Metal via Electrolysis of HgS (Cinnabar) - Copy.png - 60kB

[Edited on 8-10-2020 by Johnny Windchimes]

monolithic - 9-10-2020 at 13:48

Quote: Originally posted by Mailinmypocket  
This is the closest that YouTube (aka chemistry school for some) was able to find:

http://youtu.be/znQh7m2mkiQ


Very old post but can someone explain how this works? I'm just starting to read on this process but it seems it has to run at very high temperatures... but glass can't withstand 600C+?

Catslovechemistytoo - 8-9-2024 at 09:15

Quote: Originally posted by Johnny Windchimes  
My turn....
Get yourself a 2 amp / 20 volt DC power supply and you're off!

My recommendations:

-Use two platinum electrodes. Needs to be made of something that both wont dissolve in the electrolyte, nor amalgamate with the elemental Hg.

-PURE tungsten welding electrodes are also a great choice, as tungsten does not form amalgams either. I have not personally used tungsten but if I do this again I shall try them. Try automotive supply and welding shops.

Enjoy, because it does work!


Can titanium electrodes be used instead?

And where to get the Na2S? Can H2S just be bubbled through NaOH solution?

Or can we just dissolve sulfur in NaOH and then use this sulfides solution instead of pure Na2S?

[Edited on 8-9-2024 by Catslovechemistytoo]

[Edited on 8-9-2024 by Catslovechemistytoo]

Precipitates - 8-9-2024 at 19:00

Quote: Originally posted by Catslovechemistytoo  

Can titanium electrodes be used instead?



I'm not sure of the corrosion of titanium under these conditions - it's resistant at low temperatures, but starts to amalgamate at much higher temperatures. It's labelled as having just "good" compatibility:

Compatibility of Titanium and Mercury

Quote: Originally posted by Catslovechemistytoo  


And where to get the Na2S? Can H2S just be bubbled through NaOH solution?

Or can we just dissolve sulfur in NaOH and then use this sulfides solution instead of pure Na2S?


I would probably try the following patent's method to produce a NaOH and sodium sulphide solution:

Manufacture of sodium sulfide and sulfite

...as mentioned in this previous thread:

Sodium sulphite and sulphide from sulphur and NaOH

Be very careful working with mercury and its compounds - secondary containment is essential.

Catslovechemistytoo - 11-9-2024 at 02:38

Quote: Originally posted by Precipitates  

I'm not sure of the corrosion of titanium under these conditions - it's resistant at low temperatures, but starts to amalgamate at much higher temperatures. It's labelled as having just "good" compatibility:

Compatibility of Titanium and Mercury

Quote: Originally posted by Catslovechemistytoo  


And where to get the Na2S? Can H2S just be bubbled through NaOH solution?

Or can we just dissolve sulfur in NaOH and then use this sulfides solution instead of pure Na2S?


I would probably try the following patent's method to produce a NaOH and sodium sulphide solution:

Manufacture of sodium sulfide and sulfite

...as mentioned in this previous thread:

Sodium sulphite and sulphide from sulphur and NaOH

Be very careful working with mercury and its compounds - secondary containment is essential.


Okay, thank you for your answer. So Titanium should be fine at these temperatures. I think I'll just dissolve sulfur in NaOH solution and try dissolving HgS in it. As for electrolysis - how do I know when to stop it? My guess is that when H2 or whatever else starts evolving at cathode besides mercury then it's time to stop.
Can this be done inside of a plastic container(PP or HDPE)? I don't have large borosilicate beakers and doing this in regular glass is risky because it can crack.

Precipitates - 11-9-2024 at 17:57

When mercury stops being produced.

HDPE should be okay.
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