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Hennig Brand
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Some of the old mercury I have found is quite heavily contaminated. It appears to have a dark greyish crusty/filmy layer in some cases, and some has
redish/brown layer on outside. I guess the redish stuff is mercury oxide. There also seems to be some other "dirt" in some of the samples. I think it
was quicksilver, who on another thread talked about using a big syringe and some cotton wool to filter mercury. This would probably get rid of most of
the contaminants. How hard, and how safe would it be to improvise a mercury distillation experiment? I know I have seen it in an old article
somewhere, like in a how to article about extracting gold and later retrieving the mercury by distillation. If its contaminated mostly with mercury
oxides though, it would make little difference in a MF synthesis, would it? Anyway I am now the proud owner of 10+ pounds of mercury, 90% of which
looks good and pure%.
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ammonium isocyanate
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10 pounds!? How on earth will you dispose of that? After all, you can't keep
it forever, and there will be mercury-based waste from anything you do with it.
For that matter, how do plan on storing all that? I know somebody in my town spilled 1/2 pound of mercury recently (in this case, they used it for
Al/Hg reduction for methamphetamine production) and it took the hazmat team days to clean up (I know they kinda over-do this stuff alot of the time,
but still!).
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Hennig Brand
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Well maybe I should have done a little more preparation before I aquired the material, but I am sure it can be stored safely. If anyone has some
advice on storing mercury I would surely love to hear it. I have already transported it for more than 100 miles and had no problems. Right now I have
it stored in a remote location, in a camp at least 1/2 mile from any residences. I only stored it there because I am the only one who goes there, and
it is locked. I didn' t want to keep it at home because I felt a spill would have more severe consequences. Also with all the people doing things
around home, container breakage and a spill was a very real danger, even around the outbuildings. I only brought a couple ounces to the house, and it
is in a couple small thick glass bottles with strong leak proof tops, and these are both in a flat bottomed (leak proof) metal container with paper
towel packed loosely around and underneath them.
My primary interest so far is of course MF, but it does have many other uses in chemistry. I was interested in building a weather station for awhile,
and that could take a lot of mercury. I would also love to find some gold somewhere, and when I do the mercury will definately come in handy.
Never heard of that way of making methamphetamine, and I assure you that making it is not my intent at all! Don' t think you thought I was, but I
wanted to clarify anyway.
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ammonium isocyanate
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Yeah don't worry I didn't think that was your intent but that was just the only example of a mercury spill in my city I know of.
Wouldn't we all love to find some gold. I actually do recreational gold panning and have always considered using mercury for the recovery. I even
built my own sluice for getting gold from riverbeds. I have a small pile of concentrate that I plan on extracting with aqua regia. I'll have to see
how much I get.
Anyway, good to know you're keeping it away from people. Wish I had somewhere to squirrel away my more dangerous reagents (or the ones that I would
get if I did have such a place).
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watson.fawkes
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Quote: Originally posted by Hennig Brand  | | How hard, and how safe would it be to improvise a mercury distillation experiment? I know I have seen it in an old article somewhere, like in a how to
article about extracting gold and later retrieving the mercury by distillation. |
I've thought though how to
do this. It's not particularly difficult, although it requires skills and equipment different from most chemistry gear. Essentially, you make a still
with all iron-based materials, such as cast iron, steel, and stainless steel. You can use ordinary black iron pipe for most all the components. You
need a boiling chamber, a condenser, and a collection flask, just like any other still. That's the simple part.
Since you're dealing with Hg and presumably care about your health and environmental contamination, that means you need a completely sealed still when
it's in operation. Completely sealed is non-trivial. The threads in ordinary commercial pipe are not gas-tight and will make spiral leaks (along the
thread root), so you'll need to seal them. You can't really braze the threads up, because mercury amalgamates will all the materials in common pipe
brazing alloys (copper and silver primarily). So you'll be welding. Pipe welding is not basic welding, because you're after a complete seal, which
does not tolerate pinholes, and not just mechanical strength, which does. There is special pipe with high-precision threads that will seal completely
by mere tightening, if you can find it and want to pay for it.
Assuming you make a batch still, you need to be able to open it up and reseal it. Basically, that means flanges. I'd build the gear in the three parts
I mentioned above. The boiling and collection containers should be the only place where bulk mercury resides when the still is cold. All the rest of
the piping, including the condenser, should be the third piece. You'll need a way to hold the flasks stable while you're demounting the condenser. The
flasks will need metal gaskets, which you can cut out of ordinary sheet metal, but you'll want to anneal them dead-soft before assembly and replace
them each time the system is resealed.
You'll want to pressure test the assembly, which leads to a whole new set of issues. One way is to pressure test it with a test flange, twice, once
from each end. Another is to put in a valve. In either case, you'll want to figure out what your still pressure is and test it to that limit plus a
safety margin. In my case, I was thinking about distilling under vacuum, down at say 0.1 Torr (the easy lower limit of a rotary vane pump), to
minimize heat and vapor pressure. Pressure testing under vacuum requires a second, separate test, because vacuum failures are different from pressure
failures. The test itself consists of attaching a gauge, putting it under pressure or vacuum, detaching the pump, and leaving the system alone for a
day. The test passes if the gauge doesn't move.
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Hennig Brand
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That sounds very professional. I am pretty sure that what I read about was much more basic and probably poison hazardous. It was written in an earlier
time when we weren' t as poison or environmentaly conscious, I guess. I never really thought of a completely sealed still, but I guess steel can take
a great deal of pressure. My perceptions could be off a bit as well, and I have never looked up the pressures involved.
I am not a proffessional welder, but I have welded quite a few times as an amateur. I found that stainless steel was super easy to weld and get a
perfect seal(at least for alcohol and water). I have made several different stills in the last 6-8 years with stainless, mostly for alcohol though. I
used a DC arc welder, with stainless rods.
Thanks for the well thought out description and info Watson.Fawkes.
Ammonium Isocyanate, if you live in the city, or any heavily populated area it can be a little tricky. I guess it wouldn' t be even responsible, in
many cases. A small locked garden shed in a remote location could work quite well. I have seen these small type buildings go for very little,
especially if used. Some of the baby barns and such can be put up and taken down in pieces. Even the ones that aren' t really designed to be taken
apart, often can be if one doesn' t mind a little work, then transported and put back together on site. I am moving to the city in less than a month
to go to school, and I think that I will have to leave most of my toys at home here.
[Edited on 12-8-2009 by Hennig Brand]
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woelen
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Another way to clean up metcury is to drip it through dilute (5% or so) HNO3. A tall column, filled with the dilute HNO3 needs to be prepared. A few
centimeters wide and one meter height. Then you very slowly pour the mercury in the acid. While it is falling through the acid, most crap dissolves
and all the mercury collects at the bottom. Any remaining crap stays on top. In this way you easily can process more than 1 kilo of metal per batch.
The nitric acid can be reused and only needs to be replaced after several batches. It should not be used for any other chemistry experiments after
this use.
This dilute nitric acid trick is used to also remove soluble impurities. Less noble metal, dissolved in the mercury, dissolve in the dilute acid,
while the mercury itself only is attacked very slowly.
If you don't want to use such a tall column, then you probably also can use e.g. 500 ml of 5% HNO3 and add 10 ml or so of mercury and shake for a
while. Then collect the metal and replace with a another batch of metal. In this way, you also can clean the metal, but it is more work. The shaking
is more risky though. The glass container must be really thick-walled, otherwise the splashing of the dense metal may break the glass container.
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barbs09
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I have about 10 kg of cinnabar bearing sinter from Puhipuhi, NZ that JohnWW mentioned. As John said it is mainly silca with ~~<5% HgS?? I was
considering pounding it to powder using a dolly-pot and extracting the Hg with dilute nitric acid. This would probably be a fair amount of work
however considering the hardness of the rock. Anyone else out there with experience in obtaining the metal from silicified ore?
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watson.fawkes
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I've been reading up on mercury safety, which led me to the CRC Handbook of Laboratory Safety, which contains a section on mercury safety. Large
sections of this section are cribbed from the web set of Mercury Safety Products, Ltd., especially their page on mercury toxicity. There's interesting information on that page, but there's no references to medical literature. This is the caveat; I'm not sure
just how reliable the following is.
The claim is that Hg is not a cumulative toxin. | Quote: | Mechanisms of Mercury Toxicity
When you work in an environment contaminated with mercury, you quickly absorb the toxic metal. For example, dentists are exposed to mercury vapour and
to mercury-rich amalgam dust; this is the 'fall-out' of aerosols generated during removal of amalgam restorations. Skin exposure to native mercury
used to be common in dentistry when amalgams were mixed by hand in a chamois leather, but this practice has almost ceased.
On occupational exposure to mercury, absorption is mainly via the lungs; mercury vapour is absorbed to an extent of between 90 and 100% by this route.
Dust and droplets on the skin and in the gut are absorbed to a minor extent (about 15%) but doses to these regions are often high.
Some biotransformation of inorganic mercury to short-chain alkyl (methyl and ethyl) forms occurs in micro-organisms in the mouth and in the gut;
absorption of these organic forms is relatively efficient (80 to 100%); these are the same chemicals which wreaked so much human devastation in
Minemata. Distribution of absorbed mercury throughout the body readily occurs via the blood and mercury partitions reversibly into all organs,
including the brain and nerve tissue, which have a higher affinity for the organic forms.
Whilst the half-life of mercury in the blood has been estimated as about 3 days, mercury in body tissues clears slowly, with a half-life of about 90
days. So cessation of exposure will not therefore have immediately beneficial results, in the event of mercury poisoning - benefits of ceasing
exposure will only be seen after about a year - four half-lives.
Both inorganic and organic mercury compounds have an avid affinity for thiol (-SH) chemical groups and this is the property which renders them toxic.
Most proteins, and all enzymes, contain these thiol groups; this explains both the binding of mercury to all body tissues and many of the biological
effects. Most mercury compounds are potent but unspecific enzyme inhibitors, affecting membrane permeability and hence nerve conduction and tissue
respiration. In this respect, the biochemical effects of mercury resemble those of black widow spider venom. |
So it "partitions reversibly" and clears tissue with a half-life of three months. While not permanent, chronic exposure would lead
to some steady-state level that would look like permanent take-up.
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watson.fawkes
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As I have read, this is the
usual first purification step before distillation.
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JohnWW
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| Quote: Originally posted by JohnWW | | Mercury does not form an amalgam with iron; I have an old cast-iron bottle that came from a disused mercury mine at Puhipuhi, New Zealand, that was
used to store and transport mercury distilled from cinnabar which occurred in an old hydrothermal siliceous sinter deposit. But it fairly readily
forms amalgams with the likes of zinc, magnesium, copper, silver, gold, lead, tin, bismuth, and aluminium. |
Barbs09, here is a photo, attached, of my old cast-iron mercury bottle from the mercury mine at Puhipuhi, which is about 30 miles north of my place.
It is 350 mm tall, weighs a few kg, and the opening has a screw thread inside it. I got it at an antique auction in Whangarei. BTW I also possess
about 1 kg of mercury.
I understand that the mine had become almost uneconomic before the War, but because of the wartime demand for mercury (for use in switches,
thermometers, and as mercuric fulminate explosive) the mine was revived, but closed down soon after 1945.
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Ketone
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| Quote: Originally posted by hodges |
Right now, on United Nuclear's site, I see this:
| Quote: |
Special Note: The price of Mercury metal has risen tenfold in the past few months. Due to rapid price fluctuations our quantities on hand are limited.
1 ounce vial: $30.00
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This is the first I had heard of the price of mercury rising so much - has anyone else heard about this? In that case, mercury could be a good
investment . I have a pound of it which I paid I think $25 for a few years ago.
If an ounce is really worth $30, then my investment is now worth over $400! That certainly beats silver and gold.
Hodges
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Yeah, I've heard of the price of mercury rapidly rising too.. (though not by how much) It's likely it has to do with the fact that Hg production today
is pretty small (atleast compared to what it used to be) and demand is rapidly rising as many countries are banning real lightbulbs in favor of those
crappy mercury-using CFL's "low-energy bulbs" as they're sometimes called.
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Ketone
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| Quote: Originally posted by Formatik | Mercury even reacts with solid sulfur flakes, which are used in mercury spill kits to absorb mercury vapors (spill kits also use activated
charcoal and powdered zinc)
I've tried this and got nothing. No reaction with zinc dust. None with sulfur flower either. The zinc dust I even mixed around with the Hg
occasionally and let it sit with the mercury for several days and mixing. |
I don't know about the S, can't see why they should react at room temperature..
(to make HgS that is, but they might clump together though, as thick liquids like Hg should do with alot of powdery materials of all kinds)
But the Zn probably doesn't react cause it has an oxide-layer.. You'd often have that same problem when trying to react Hg with Al too.
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JohnWW
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That recent steep Hg price rise cannot be due to any jump in use of fluorescent light bulbs and LCD TVs and screens containing them, because they have
been around for many years now, and are set to be superseded by even more efficient LED bulbs and screens. Besides, the use of Hg amalgams for dental
fillings is just about extinct, being now banned in several countries, and about to be prohibited in many others. The traditional use of Hg compounds
as dyes or pigments, e.g. on hats (hatters no longer go mad) and as vermilion, has long been superseded by organic and other substitutes. Hg has also
long been superseded by cyanide for extraction of Au and Ag in mining. There are also several non-chemical applications of Hg for which Ga, or
eutectic alloys of Ga, can easily substitute, like high-temperature thermometers, Ga being a much more common metal recovered mostly in the refining
of bauxite for alumina.
It must be due to speculators, with more money than sense, trying to "corner the market", by creating a public perception of shortage. But it will
turn, before long, into a case of "fools and money are soon parted", in view of what happened around 1980 (when large quantities of Ag were still
being used for black-and-white photography, now confined to radiography), when the Hunt Oil brothers tried to "corner" the Ag market, causing the
price of Ag to soar astronomically for a few months, before collapsing when the Hunts ran out of money and got their fingers burnt.
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watson.fawkes
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I'm not sure I believe that there's been a drastic surge
in the price of Hg overall. Maybe United Nuclear has seen a jump from their supplier. See http://www.minormetals.com/index.aspx?mode=hg for some recent (spotty) price activity.
More interesting is the "salient mercury statistics", which indicates an overall trend in loss mercury consumption and production. It's pretty clear from these figures
that some significant industrial uses are being phased out.
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psychokinetic
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[rquote][
Barbs09, here is a photo, attached, of my old cast-iron mercury bottle from the mercury mine at Puhipuhi, which is about 30 .][/rquote]
I'm suprised to hear we even have/had a Hg mine here in New Zealand. *heads off to find out more*
“If Edison had a needle to find in a haystack, he would proceed at once with the diligence of the bee to examine straw after straw until he found
the object of his search.
I was a sorry witness of such doings, knowing that a little theory and calculation would have saved him ninety per cent of his labor.”
-Tesla
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blogfast25
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| Quote: Originally posted by Joyce21 | Mercury is ONLY safe when you handle it correctly. Don't be foolish, don't try to soak your friend's head in it. So handle it correctly.
Regards
Joyce
____
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No but it's interesting to see how even a solid lead object floats on it...
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S.C. Wack
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This week's NYMEX: $550 a flask, down from $640 2 weeks ago. Of course delivery of a single flask if you could get one would be considerably more, but
not what UN is asking.
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zed
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When I was a boy, I had friends that brought containers of Mercury to school with them. They had lots of it, had no fear of it, and they got lots of
exposure. Their family owned a small Mercury mine.
By way of warning, they seemed to be about the dullest boys in our school.
Their child pleasing trick? Putting a little Mercury, onto a fellow students Silver dime.
Shazzam! The Mercury would quickly mirror-ize the dime, amalgamating itself to the dime's surface.
Were it not for the currently high price of Silver..... A brush with fine, Silver wire bristles, would be an excellent means of recovering spilt
Mercury. Silver sucks it right up. Silver plated bristles would probably work just as well.
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agorot
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I want to get some mercury to try to build my own Castner-Kellner cell for several reasons, but mostly because I can  ...if I get the mercury for it. I have 100g I bought from a website a little while
back for $6, but they have stopped selling it. I would really like to find another source. There are cinnabar deposits less than 200 miles away from
me, but I'm not sure I'm ready to try to separate it from the sulfur. Does anyone have a cheap supplier that they know of?
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Skyjumper
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Yeah, electricians, and heater repair people may have them from old switches and such. Befriend them and ask them to hold onto the switches.
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manimal
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I read that one of the past treatments for syphilis involved inhaling mercury vapor, or "fumigating". Essentially, they would hotbox the patient,
sticking his head over a pan of mercury and lighting a fire underneath. He would breathe deeply, the boiling mercury clearing the sinuses and causing
intense sweating that was thought to expel harmful pathogens.
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entropy51
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But organic arsenic was much more effective in those days before penicillin.
Hg was more commonly administered as an ointment applied to the chancres.
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manimal
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I think they used all three routes: ingestion of calomel tablets, inhalation of vapor and application as a salve. Arsenic came a little later as an
"improvement" to the mercury. A saying went "one night with Venus leads to a lifetime on mercury".
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manimal
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| Quote: Originally posted by watson.fawkes | I've thought though how to do this. It's not particularly difficult, although it requires skills and equipment different from most chemistry gear.
Essentially, you make a still with all iron-based materials, such as cast iron, steel, and stainless steel. You can use ordinary black iron pipe for
most all the components. You need a boiling chamber, a condenser, and a collection flask, just like any other still. That's the simple part.
Since you're dealing with Hg and presumably care about your health and environmental contamination, that means you need a completely sealed still when
it's in operation. Completely sealed is non-trivial. The threads in ordinary commercial pipe are not gas-tight and will make spiral leaks (along the
thread root), so you'll need to seal them. You can't really braze the threads up, because mercury amalgamates will all the materials in common pipe
brazing alloys (copper and silver primarily). So you'll be welding. Pipe welding is not basic welding, because you're after a complete seal, which
does not tolerate pinholes, and not just mechanical strength, which does. There is special pipe with high-precision threads that will seal completely
by mere tightening, if you can find it and want to pay for it. |
The ordinary black stock can usually be tightened gas tight without brazing using a couple of large pipe wrenches, con huevos.
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