I am seeking some information on the cleansing of mercury.

[Mkury]

I have approximately 28cc of mercury (~450g), which is contaminated with about 2 or 3 grams of lead.

The issue is that I am using the mercury to restore atmospheric measuring gauges - and the lead oxides etc. leave grey stains inside the glass tubes, where as very clean mercury doesn't.

I mean I can ram some cotton wool into a syringe and filter it like that.... but 28cc of mercury is very hard to get hold of... and I use it extremely sparingly, for atmospheric testing instruments... and I am reluctant to lose even a fraction of the metal in the filtering medium.

Since mercury has a boiling point of ~360*C (or ~260*C under vacuum) and lead has a boiling point of 1750*C - I could tripple distill the mercury and leave the lead and lead oxides behind.

BUT because this issue is actually quite rare in terms of cleaning the mercury..... I was wondering if there is a way to clean out the lead oxides using a flux, rather than distilling the mercury.

I figure that I could just clean out the oxides first and if that ran through the glass tubes without staining them, the small amount of dissolved lead, might not be an issue.

AND sometimes, trying the easiest things first is usually a grand idea..... You know "my computer does not work" - "Have you tried plugging it in?"

Maybe a teaspoon of zinc chloride soddering flux over some slightly warmed up mercury might be just the thing, rather than setting up a still to boil off the mercury...

The idea of Rosin - as used in tin-lead sodder, comes to mind, as does "killed spirits" or zinc chloride etc...

OR some kind of an acidic or alkaline wash - using common store bought materials - such as hydrochloric acid or sodium hydroxide - in a heavy dilution solution.

I am in a fairly remote area of Australia - and most chemicals are hard to get, and or hard to get freighted**, or they are restricted to licensed people... or only available in large drums of 20 or 200 liters plus... and it can get to be very very expensive all around - when at best I might only need a teaspoon full of it / them.


** When trucks catch fire or crash, the fire dept / emergency services want to know what is on board, so all loads, beyond tyres and tins of beans, have to be registered. e.g. drums of really toxic insecticide concentrates catching fire - or spilling etc... well this hazchem business is fair enough but it can add double or tripple to the cost of the freight - i.e. car batteries - contain acid... so you get registration, insurance and all the ****, so your $300 lead acid battery now has $400 of administration costs on top of it...

I only want a teaspoon of flux of some description to pull out the lead oxide...

Does anyone have any experience or can cite a reliable source or method to clean lead oxide out of mercury?


Potential solutions:

http://www.sciencemadness.org/talk/viewthread.php?tid=62600
(fluxing off lead oxide during a cast) - As for fluxes for lead the simplest is paraffin wax. It seems to work primarily by adhering to the oxides which reduces the wetting action of the metal. Simply add a pea-size chunk to the metal and stir, you will end up with loose dross that can easily be skimmed off the surface.


Very dilute HNO3 works like a charm. Use somewhere between 5% and 10% concentration, not higher. At such low concentrations, HNO3 is not that strongly oxidizing. Because HNO3 is a strong acid, it acts much more rapidly than acetic acid. HCl and H2SO4 also are strong acids, but their lead salts are (nearly) insoluble, so they do not work well.
The problem with the acetic acid solution is that you'll be removing
the lead oxide but at the same time you'll be producing lead
acetate, which is basically replacing one whiteish cover with
another one.

https://www.tackleunderground.com/community/topic/22401-removing-lead-oxidation/
The best acid for this purpose is dilute HClO4, which is not oxidizing at all, while at the same time it is a strong acid having a freely soluble lead salt. But not many people will have HClO4, the next best option is more common.


~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~
Thoughts so far:

Acetic acid - 5% house hold vinegar will convert the lead oxide into lead acetate, but it will also convert mercury into mercury acetate....

Me thinks that a dab of bees wax will work well as an oxide flux, as the bees wax has a very low melting point, it's basically non reactive, and when the mercury and lead oxide contamination is stirred up and exposed to the bees wax, and the dross is skimmed off, then the material can be frozen in a deep freeze, and the bees wax will be a hard skin and the mercury can be drained away from it and then the mercury can be recleaned with with acetone / spray painting solvent to lift out any wax / oily contaminants..

I think this is worth a try.

Bees wax has a melting point <65*C and parafin wax has a melting point starting at 37*C...

Or perhaps the bees wax or parafin wax can be warmed up and dissolved in a solvent and added cold, to the contaminated mercury...

 

[goldshark]

From what I can gather, Hydrochloric acid may be your best best. It dissolves Lead in finely divided particles, and isn't supposed to react with Mercury. I have a retort, my go to cleaner, so never gave it much thought . A retort is extremely easy to build, if you have a welder and pipe. Maybe not in the bush though. If you could get to a lab, dissolution in nitric, then reprecipitate, would yield clean Mercury. I don't know the history of your Mercury, but if the "crud" is only on the outside, it could also be contaminated from the pyrite group, particularly Arsenopyrite. Old prospectors tip was to make a solution of sodium Hydroxide, place in leak proof container, then agitate well. I hope this helps. Wood ash may be the bush fix.

 

[Mkury]

From what I can gather, Hydrochloric acid may be your best best. It dissolves Lead in finely divided particles, and isn't supposed to react with Mercury. I have a retort, my go to cleaner, so never gave it much thought . A retort is extremely easy to build, if you have a welder and pipe. Maybe not in the bush though. If you could get to a lab, dissolution in nitric, then reprecipitate, would yield clean Mercury. I don't know the history of your Mercury, but if the "crud" is only on the outside, it could also be contaminated from the pyrite group, particularly Arsenopyrite. Old prospectors tip was to make a solution of sodium Hydroxide, place in leak proof container, then agitate well. I hope this helps. Wood ash may be the bush fix.

Yeah well the first stage is to simply remove the lead oxide (fluxing with wax = low temperatures = easy and safe) and then suck the mercury through some glass tubing to see if it stains the glass.... and if it's good to go, I will use that. BUT if the dissolved clean lead mixed in with the mercury leaves a film inside the glass, then it's to the still that it goes....

I am not truly truly stuck.... it's just thanks to the evil government regulating everything so that no one can manufacture any DIY explosives and engage in home brew blasting of their own mining operation or the evil government, and to stop people poisoning themselves, each other or sending themselves into orbit in pieces... AS WELL AS - people getting hold of things that they are not familiar with and not having the training to use and or store and or the proper processes - or they setup criminal labs for making crystal meth etc....


I mean that teenagers who lack experience, are doing drugs like alcohol etc., and adding speeding and monsterously fast cars - were just killing themselves AND OTHER PEOPLE in huge numbers - so all of that got banned.....


And all the kiddies who survived themselves are mean old *******s opposing 130 Kmh speed limits on the interstate freeways in Australia.....


Remember Guy Fawks night in Australia - remember how kids would have a spark land in a pocket full of fire crackers and the kid would get a HUGE hole blown in their leg or blinded in one eye from a wayward skyrocket and all sorts of dramas...

Well rather than do a school training session for all the kids to go to on how to use fireworks safely and how to have fun with them, they just outright banned them totally.... except for really lame crap like sparklers...


I mean people think common over the shelf vitamins are just hunky dory and if one is good so two must be better etc., and lots of people go down with liver failure etc., from gutsing Vitamins A and D and E, while it says on the packet take only as directed and if symptoms persist see a medical professional - and vitamins may only be of assistance IF dietary intake is inadequate.... But people are still killing themselves with vitamin supplements....


I mean if you want to get a lot of things from an industrial or scientific chemical supplies, you either have to be licensed to buy it and handle it.... which is kind of fair enough.... or your placed on a terrorist watch list... or your reported as a potential illicit drug manufacturer..... OR you can only get it in 200 liter drums...

OR if you can only get it in small amounts - in analytical grades, your going to pay astronomical amounts for "spectrum analyser purity" grades....

It just gets up my arse at how insane it has become to so simple things with small amounts of "chemicals" for legitimate purposes.


Unless it's over the counter chemicals from the supermarket or the hardware store - it's generally such a head ache and super high prices to get and or transport.... especially for small quantities.


Like for instance - there is a very old type of photography process called Daguerreotype - which is based upon mercury... and as mercury has NO grain in it, unlike celluloid film, the images taken with it, are precise to the atomic level of clarity. These images are so beautiful... but try setting up a photographic studio that uses mercury based images - even if you only want to knock out a dozen photos...


Your immediately into an absolute nightmare of regulation, rules, OH and S, requirements for all sorts of things and a multitude fo compliance and inspections and certifications etc..


https://www.skinnerinc.com/news/blo...beautiful-storied-pictures-early-photography/

I just want to clean perhaps 1/4 of a gram of lead oxides out of the mercury and be done with it...

There are more lead oxides on a wheel weight, and more mercury in a loose tooth in a car wreck, than in the mix.

There are a LOT of idiots in the beaurocracy too.....

"Oh my god, your using lead pencils - and what are you doing to minimise risk and exposure and disposal of the shavings??"

 

[Southfork]

Did you try fine sand water and a gold pan? Shake it down like panning gold then tip the pan the mercury will come out clean maybe. Squeeze through a filter to finish.

 

[Mkury]

From what I can gather, Hydrochloric acid may be your best best. It dissolves Lead in finely divided particles, and isn't supposed to react with Mercury. I have a retort, my go to cleaner, so never gave it much thought . A retort is extremely easy to build, if you have a welder and pipe. Maybe not in the bush though. If you could get to a lab, dissolution in nitric, then reprecipitate, would yield clean Mercury. I don't know the history of your Mercury, but if the "crud" is only on the outside, it could also be contaminated from the pyrite group, particularly Arsenopyrite. Old prospectors tip was to make a solution of sodium Hydroxide, place in leak proof container, then agitate well. I hope this helps. Wood ash may be the bush fix.

There are published papers from a long time ago, on making super pure mercury - but it involves many exotic chemicals, reactions and steps - and I have them.... but there is "clean enough" mercury, and then there is super precision atomically clean mercury.

I just want "clean enough" grade mercury, to run the mercury though fine glass tubes, without staining the glass tubes up with grey lead oxide...

At best I will FIRST try fluxing with bees wax, because I can use a small bottle, low heat, and a thorough shaking for several minutes and then inverting the bottle, freezing it so the wax hardens as a crust on the top of the mercury and the mercury can be poured out...

And then seeing how that goes up the tube....

AND then resort to a straight distilation of the mercury if the fluxing does not work well enough....


~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~

This is from a PDF from an ancient book, with a citation from another text in 1927....

THE PREPARATION OF VERY CLEAN MERCURY
DUANE ROLLER, UNIVERSITY OF OKLAHOMA
ANY PROCESS which proves adequate for the purifying of a metal used as
the active substance in a photoelectric cell can also be employed with con-
siderable confidence in other fields of experimentation where extraordinary
purity is desired. This follows from the fact that the highest obtainable
degree of purity is the most essential requirement in the investigation of
the photoelectric properties of a substance.
In preparing mercury for photoelectric purposes the mercury not only
must be freed from foreign metals and other substances, but it must be
protected during the process of distillation from contamination. Especially
must contamination with organic substances be avoid-
ed. Stopcock grease, which is a mixture of rubber
and vaseline, and certain other organic substances
produce pronounced changes in the photoelectric be-
havior of mercury, as has been shown by W. B. Hales
and F. L. Poole in unpublished work, and by the
author (Phys. Rev. 32, 323, 1928). The removal of
occluded gases from the mercury is also important,
for it is well known that absorbed and adsorbed gases
often produce marked changes in photoelectric proper-
ties.
The following technique for cleaning mercury for
photoelectric purposes has been used by the author
with success:
(1) Remove grease by washing the mercury thor-
oughly with a 10 percent solution of potassium hy-
droxide.
(2) Shake or mix the mercury for several hours
with an equal volume of 3-normal nitric acid, thus
removing most of the metallic contamination.
(3) Wash the mercury with distilled water, dry by
heating it to about llOoe. in a porcelain dish, and
filter by forcing it with compressed air through
chamois skin, or by passing it through a pinhole in
the apex of a glazed paper funnel.
. 1 Ce trif I '
( 4) Distill the mercury several times by the method
Fig..
n uga mlxer. of Hulett and Minchin (Phys. Rev. 21, 388, 1905); in
this method, air is bubbled through the mercury in the still during distilla-
tion, thus oxidizing volatile foreign metals.
(5) Pass the mercury through a filter consisting of a glass tube with
one end drawn to a capillary opening; repeat this process until all traces
of oxide have disappeared from the surface of the mercury.
(6) If it is desired to remove occluded gases, as is necessary in photo-
dectric work, distill the mercury repeatedly in the highest obtainable vacu-
um. The still used in this process should form an integral part of the
apparatus in which the mercury finally is to be used. This method of re-TIIE ACADEMY OF SCIENCE
139
moving occluded gases from mercury was first used by Kazda (Phys.
Ftev. 26, 643, 1925).
The: washing processes described in steps (1), (2), and ( 3), above,
are best accomplished with a centrifugal mixer (Fig. 1). This device can
be made easily and it is more effective than the "fall" tube commonly
employed in cleaning mercury, or than the ordinary mechanical stirrer;
Bray (Am. Chem. Soc. J. 49, 2572, 1927) used a centrifugal mixer in
preparing mercury, but does not describe it. This mixer is much more
efficient than the ordinary stirrer and undoubtedly can be put to many
uses besides the present one, particularly in the laboratory of the organic
chemist. The vertical shaft of the mixer consists of a 30 cm length of
7 mm glass tubing. The upper end of the shaft is sealed shut and to the
lower end is sealed a 10 em length of similar tubing, shaped as in Fig.
1, and drawn out at each end to an opening approximately 2 mm in di-
3meter. This tube contains a third opening in its lower center, opposite
the point where it is sealed to the shaft. The upper end of the shaft is
fitted with a piece of short glass tubing of slightly larger diameter than
the shaft, this being held in place by two perforated corks which fit the
shaft tightly. It is necessary to lubricate the part of the shaft between
the two corks with a small amount of vaseline or graphite.
A clamp is attached to the larger tube, between the corks, and the
mixer is supported vertically in a battery jar containing the mercury and
washing liquid. The liquid should cover the openings in the ends of the
mixer and the shaft should be so adjusted that air and mercury alternately
enter the center opening during rotation. It is essential that the mixer be
operated at high speed, preferably by means of a small motor attached ttl
the shaft with rubber tubing or with a belt.
The still used in step (4) of the mercury cleaning process should be
constructed in the manner described by Hulett and Minchin, except that
all joints made with rubber tubing or stoppers should be replaced by ground
glass joints. Experience also shows that a receiving bottle for the distillate,
connected to the condensing tube by a ground glass joint, is much more
ronvenient and also less fragile than the usual tube of barometric height.
Since phosphorus pentoxide is often used as a drying agent in apparatw
containing mercury, it might be well to say here that the phosphorus and
lower oxides, often present in impure phosphorus pentoxide, are likely to
soil mercury. Phosphorus pentoxide can be purified sufficiendy for this
purpose by heating it thoroughly in a current of dry air.

 

[Mkury]

Did you try fine sand water and a gold pan? Shake it down like panning gold then tip the pan the mercury will come out clean maybe. Squeeze through a filter to finish.

Yeah I'll go with this because with using BEES WAX, it's a soft piable wax when at room temperature....


Sciencemadness Discussion Board - Removing lead oxide from lead ingots. - Powered by XMB 1.9.11
(fluxing off lead oxide during a cast) - As for fluxes for lead the simplest is paraffin wax. It seems to work primarily by adhering to the oxides which reduces the wetting action of the metal. Simply add a pea-size chunk to the metal and stir, you will end up with loose dross that can easily be skimmed off the surface.

I can melt the beeswax over the warm mercury (~70*C) and shake the **** out of the bottle, and then with all the oxide entrained in the wax, I can invert the bottle, and let it cool to solidify the wax, and maybe throw it in a refrigerator or deep freeze to harden the wax right up, and then pour out the mercury. IF if comes out NICE and CLEAN, and does not stain the inside of the glass tubes, it's good to go.


BUT if the remaining dissolved lead, greys up the inside of the glass, it's to the distillation process it goes.

 

[Southfork]

I like doing things simple and easy not to complicate. Squeezing it through a chamois cloth several times will do the trick,

 

[goldshark]

Still wondering how you determined the contamination is from Pbo?

 

[Mkury]

There is the other method, to bubble air through the mercury to oxidise all the lead, and then just use moltern beeswax wax to soak up the lead oxides - Like I am not insanely paranoid about mercury.... but it's not good for you and some forms / compounds are extremely toxic - even in tiny doses....

If the people who handle it and purify it go to considerable lengths to not produce fumes, and to not breath them in, and to not be handling it, or any of it's compounds and to minimise the risk of any spills and to contain any spills, then if that is good enough for them, then it's good enough for me.


So straight mercury is ONE thing, and mercurial compounds are another thing..... AND it's generally a bad idea to delve into areas when one lacks the expertise and equipment to undertake "grand plans" to chemically modify mercury and to create by products that can be extremely toxic in almost infitesimally small amounts - by fume or by contact.


So cleaning with bees wax and then a straight distillation if necessary is safe - if done properly. This is within my technical skillset.


Mercury and making really toxic compunds either accidentally or deliberately, is not an area I wish to go into unless it is with a good reason, and comes with the proper training and the proper places to do it in....


And the lack of familiarity with anything other than basic cleaning and uses of mercury - is not an area I will be going into.

It's easy enough to get it very wrong and the consequences are quite serious.




Dimethylmercury.

https://en.wikipedia.org/wiki/Dimethylmercury
Dimethylmercury ((CH3)2Hg), also known as Mercury dimethanide, is an extremely toxic organomercury compound. A highly volatile, reactive, flammable, and colorless liquid, dimethylmercury is one of the strongest known neurotoxins, with a quantity of less than 0.1 mL capable of inducing severe mercury poisoning resulting in death, and is easily absorbed through the skin. Dimethylmercury is capable of permeating many materials, including plastic and rubber compounds. It has been described as having a slightly sweet odor, although those who have reported its smell were exposed to toxic amounts.[2]

Synthesis, structure, and reactions​

The compound was one of the earliest organometallics reported, reflecting its considerable stability. The compound was first prepared by George Buckton in 1857 by a reaction of methylmercury iodide with potassium cyanide:[3]

2 CH3HgI + 2 KCN → Hg(CH3)2 + 2 KI + (CN)2 + Hg
Later, Frankland discovered that it could be synthesized by treating sodium amalgam with methyl halides:

Hg + 2 Na + 2 CH3I → Hg(CH3)2 + 2 NaI
It can also be obtained by alkylation of mercuric chloride with methyllithium:

HgCl2 + 2 LiCH3 → Hg(CH3)2 + 2 LiCl
The molecule adopts a linear structure with Hg–C bond lengths of 2.083 Å.[4]

Safety​

Dimethylmercury is extremely toxic and dangerous to handle. Absorption of doses as low as 0.1 mL can result in severe mercury poisoning.[2] The risks are enhanced because of the compound's high vapor pressure.[2] Medicinal chemist Derek Lowe called it "deadly and hideous" in a 2013 article.[11]

Permeation tests showed that several types of disposable latex or polyvinyl chloride gloves (typically, about 0.1 mm thick), commonly used in most laboratories and clinical settings, had high and maximal rates of permeation by dimethylmercury within 15 seconds.[12] The American Occupational Safety and Health Administration advises handling dimethylmercury with highly resistant laminated gloves with an additional pair of abrasion-resistant gloves worn over the laminate pair, and also recommends using a face shield and working in a fume hood.[2][13]

Dimethylmercury is metabolized after several days to methylmercury.[12] Methylmercury crosses the blood–brain barrier easily, probably owing to formation of a complex with cysteine.[13] It is not quickly eliminated from the organism, and therefore has a tendency to bioaccumulate. The symptoms of poisoning may be delayed by months, resulting in cases in which a diagnosis is ultimately discovered, but only at a point in which it is too late or almost too late for an effective treatment regimen to be successful.[13] Methylmercury poisoning is also known as Minamata disease.






A Scientist Spilled 2 Drops Organic Mercury On Her (gloved) Hand. This Is What Happened To Her Brain.

 

[Mkury]

Still wondering how you determined the contamination is from Pbo?

Oh it's not plumbum, it's lead - that is the contaminant.

Well it's like this, when you convert lead to mercury, through neutron bombardment of the nucleus, of the isotopes at around 32 million electron volts, this causes alpha decay of the nucleus and the transition from lead into mercury.

While a conversion rate of greater than 99.9% is possible, it's very hard to get all the lead to convert into mercury, thus the lead remains in solution and it forms an adhesive and floating oxide from contact with the air.

The oxide sticks to the glass and the mercury simply rolls over it.

 

[FrugalRefiner]

My spidey sense is tingling.

Are you telling us you created this mercury through neutron bombardment of lead?

Dave

 

[Mkury]

My spidey sense is tingling.

Are you telling us you created this mercury through neutron bombardment of lead?

Dave

No, goldshark asked me how did I know the contamination was plumbum, I told him it wasn't plumbum, it was lead.

It's not the conversion of lead into mercury by neutron bombardment of the nucleus, it's knocking out protons, from the nucleus, to create alpha particle decay....

Me doing this?

Do I sound like the kind of guy who has access to a top secret, near gigavolt particle accelerator, and nuclear research facility, under the Maralinga Nuclear Bomb testing sites?

Not a chance.

 

[Mkury]

You might find this helpful for protection against pychotronic mind control devices.

I know I have.

https://zapatopi.net/afdb/

 

[goldshark]

Your original post stated Pbo, now you state Pb. Which is it, and how did you determine what it is? Please answer the question, without all the cut and paste mumbo jumbo. What statement are you trying to make? The Goldsnark in me says maybe something went wrong with an experiment, and you may have ingested some of the Mercury. Do you need some professional help?

 

[Mkury]

You like to sticky nose and your arrogant enough to think I owe you an answer.
Most sticky noses are arrogant pricks and you don't seem to qualify as an exception to the rule.
Your lack of graces and good manners is your problem.
Live with it.

 

[FrugalRefiner]

Mkury, you're a hair away from being banned. We don't address each other like that here. If you do it again, you will be gone.

Dave

 

[goldshark]

Hey Mkury, sorry we got off on the wrong foot. Now that you have definitely identified it as Lead, you already seem to have found the solution for purifying it, good. I never called your Pb or Pbo Plumbum, I only asked if you knew for sure what contaminant it was, and how you knew what it was. Pretty simple and straight forward question. Everybody knows there are 2 types of Plumbum, Plumbum Nigrum, and Plumbum Candidum. If I had said it, I would have referred to the specific one.

 

[Yggdrasil]

Oh it's not plumbum, it's lead - that is the contaminant.

Well it's like this, when you convert lead to mercury, through neutron bombardment of the nucleus, of the isotopes at around 32 million electron volts, this causes alpha decay of the nucleus and the transition from lead into mercury.

While a conversion rate of greater than 99.9% is possible, it's very hard to get all the lead to convert into mercury, thus the lead remains in solution and it forms an adhesive and floating oxide from contact with the air.

The oxide sticks to the glass and the mercury simply rolls over it.

Get your names straight, you are basically saying: "its not Lead it is Lead"
Plumbum is the Latin name for Lead and what gives the Pb notation in the Periodic table.

 

[Yggdrasil]

Hey Mkury, sorry we got off on the wrong foot. Now that you have definitely identified it as Lead, you already seem to have found the solution for purifying it, good. I never called your Pb or Pbo Plumbum, I only asked if you knew for sure what contaminant it was, and how you knew what it was. Pretty simple and straight forward question. Everybody knows there are 2 types of Plumbum, Plumbum Nigrum, and Plumbum Candidum. If I had said it, I would have referred to the specific one.

Well in this modern world we have Lead (Plumbum Nigrum) and Tin (Plumbum Candidum) and only one of them is used for PbO

 

[goldshark]

Well in this modern world we have Lead (Plumbum Nigrum) and Tin (Plumbum Candidum) and only one of them is used for PbO

The point is, all I ever asked is, "Are you sure it is Lead or Lead oxide as the contaminant"? Then the conversation went ballistic. A simple yes or no would have sufficed.