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plante1999
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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]
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garage chemist
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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.
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plante1999
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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!
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garage chemist
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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]
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plante1999
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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?
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Endimion17
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garage chemist
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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.
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plante1999
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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" />
<!-- bfesser_edit_tag -->[<a href="u2u.php?action=send&username=bfesser">bfesser</a>: reduced
image size(s)]
[Edited on 2.8.13 by bfesser]
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garage chemist
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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.
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Endimion17
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Please don't encourage him to distill mercury. You have no idea how dangerous that is.
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plante1999
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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]
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garage chemist
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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.
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blogfast25
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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.
<!-- 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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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>.
<!-- 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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garage chemist
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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.
<!-- 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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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]
<!-- 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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barbs09
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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
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bfesser
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Just a thought, but it may be easier and safer to just find a local source.
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plante1999
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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]
<!-- bfesser_edit_tag -->[<a href="u2u.php?action=send&username=bfesser">bfesser</a>: removed
unnecessary quote; subscript; rxn. eqn. cleanup]
[Edited on 3.8.13 by bfesser]
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plante1999
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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.
<!-- bfesser_edit_tag -->[<a href="u2u.php?action=send&username=bfesser">bfesser</a>: reduced
image size(s)]
[Edited on 2.8.13 by bfesser]
I never asked for this.
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Endimion17
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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.
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.
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plante1999
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The word synthesis is Edited. Thanks for remmenbering me that!
[Edited on 12-2-2012 by plante1999]
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garage chemist
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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.
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Endimion17
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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]
<!-- bfesser_edit_tag -->[<a href="u2u.php?action=send&username=bfesser">bfesser</a>: removed
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[Edited on 2.8.13 by bfesser]
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plante1999
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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]
<!-- bfesser_edit_tag -->[<a href="u2u.php?action=send&username=bfesser">bfesser</a>: removed
unnecessary quote; rxn. eqn. cleanup]
[Edited on 3.8.13 by bfesser]
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