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G.Patton

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Introduction

Here you can find detailed information about aluminum amalgam, it's producing manuals from mercury nitrate or mercury chloride. There is a mercury nitrate synthesis manual with video instructions. Mercury chloride synthesis isn't described by reason that it's produce from mercury nitrate. Aluminum amalgam is one of a number of metal amalgams that is not described here for the reason that only aluminum amalgam is mainly used in synthetic routes of illicit drug production.

What is Amalgam

An amalgam is an alloy of mercury with another metal. It may be a liquid, a soft paste or a solid, depending upon the proportion of mercury. These alloys are formed through metallic bonding, with the electrostatic attractive force of the conduction electrons working to bind all the positively charged metal ions together into a crystal lattice structure. Almost all metals can form amalgams with mercury, the notable exceptions being iron, platinum, tungsten, and tantalum. Silver-mercury amalgams are important in dentistry, and gold-mercury amalgam is used in the extraction of gold from ore. Dentistry has used alloys of mercury with metals such as silver, copper, indium, tin and zinc.
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Aluminum can form an amalgam through a reaction with mercury. Aluminum amalgam may be prepared by either grinding aluminum pellets or wire in mercury, or by allowing aluminum wire or foil to react with a solution of mercuric chloride/mercuric sulfate. This amalgam is used as a reagent to reduce compounds, such as the reduction of nitro compounds to amines. The aluminum is the ultimate electron donor, and the mercury serves to mediate the electron transfer. The reaction itself and the waste from it contain mercury, so special safety precautions and disposal methods are needed. As an environmentally friendlier alternative, hydrides or other reducing agents can often be used to accomplish the same synthetic result. Another environmentally friendly alternative is an alloy of aluminum and gallium, which similarly renders the aluminum more reactive by preventing it from forming an oxide layer.

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Aluminum in air is ordinarily protected by a molecule-thin layer of its own oxide. This aluminum oxide layer serves as a protective barrier to the underlying aluminum itself and prevents chemical reactions with the metal. Mercury coming into contact with it does no harm. However, if any elemental aluminum is exposed (even by a recent scratch), the mercury may combine with it to form the amalgam. This process can continue well beyond the immediately exposed metal surface, potentially reacting with a large part of the bulk aluminum before it finally ends.

The presence of water in the solution is reportedly necessary; the electron rich amalgam will oxidize aluminum and reduce H+ from water, creating aluminum hydroxide (Al(OH)3) and hydrogen gas (H2). The electrons from the aluminum reduce mercuric Hg2+ ion to metallic mercury. The metallic mercury can then form an amalgam with the exposed aluminum metal. The amalgamated aluminum then is oxidized by water, converting the aluminum to aluminum hydroxide and releasing free metallic mercury. The generated mercury then cycles through these last two steps until the aluminum metal supply is exhausted.
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Preparation methods

Al/Hg amalgam from HgCl2 in MeOH solution
Set up a two-liter flat-bottom three-neck flask, and plugged one of the necks. Arrange a reflux condenser in the center hole. The apparatus was placed on stirrer/hotplate. Cut Reynolds Heavy Duty aluminum foil into about 1" squares, to make a total of 27.5g.
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5g of foil in 1" squares and 5g of foil and foil after 8-10 seconds of grinding in a Braun coffee grinder

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Closeup of foil balls and 27.5g foil in a 2000 mL flat-bottom flask

Put 5g batches into a small Braun coffee grinder and ground the foil for 8-10 seconds. The foil doesn't really get "ground", but it gets all balled up into little globs. This works amazingly well. It may sound weird to put your foil in a coffee grinder, but this is without question a breakthrough in the preparation of aluminum for the Al/Hg. Next, 400 mg of HgCl2 was dissolved in 750 mL of lab grade MeOH. When the MeOH was ready (all HgCl2 dissolved), it was also dumped in the flask and the condenser was put in place. It was stirred for 5-10 seconds every minute or so. In less than 10 minutes, faint bubbling was visible, the solution was gray, and the aluminum was distinctly less shiny. Some pieces had started to float. When the amalgam is ready, gas evolution stops.
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Amalgamation complete

Dry Al/Hg amalgam from Hg(NO3)2

We take 14 g of aluminum foil and tear it with our hands into pieces of 2x2, 3x3 cm in size. Be sure to tear, not cut, to increase the surface area. Place into a 3-necked round-bottomed flask and fill the foil completely with water.
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Now we are preparing the mercury salt. We take a mercury thermometer from the pharmacy, wrap it in paper, break it at the bottom tip. Pour all the mercury (~1-2 g) into a glass, where then add 4 mL of nitric acid (70%). Do not forget that mercury vapors are hazardous to health! To initiate the reaction, the glass had to be heated to about 50 degrees, stirring occasionally. All the mercury dissolved about for 30 minutes, and an orange gas, nitrogen oxide (IV), was released from the glass. The reaction equation is as follows:
Pipette 2 mL of the solution and place it in a round-bottom flask with foil. After about 5 minutes, the foil lost its shine, became dull, and a small layer of gray sludge (aluminum hydroxide) collected at the bottom of the flask. After 10-15 minutes, the reaction stops, this can be seen by the cessation of gas evolution.
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We drain the liquid and rinse the foil with water 3 times.
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Acetic essence is often used to produce hydrogen, but I "start" the reaction to produce hydrogen with water. Less acidic medium, which means less alkali must be added later. Many people ask the question: "How to remove this water?" There is no need to remove water anywhere, it reacts with aluminum and hydrogen is obtained: 2Al + 6H2O ---> 2Al (OH)3 + 3H2

How to use it

Al amalgam (Al/Hg) is widely used in reduction organic reactions of nitro-compounds to amines. Reduction reaction is a one-pot exothermic reaction with Al/Hg with organic unsaturated compound. Aluminium, water and mercury release hydrogen gas (H2) in reaction mixture and saturate organic compounds. You can meet Al/Hg reduction in most popular reactions such as Synthesis of amphetamine from P2NP via Al/Hg (video), Complete MDMA synthesis from sassafras oil, Synthesis and extraction of d-amphetamine (Nabenhower, 1942) and so on.
 
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ACAB

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According to wikipedia, for the production of mercury(II) nitrate, hot and concentrated nitric acid is needed, or does that make no difference?
The reaction with hot nitric acid looks at least more violent, a lot of gas is produced and that did not take 10 minutes.

With the mercury(II) nitrate and the aluminiun, is there a ratio to follow? Or how can you determine the correct amount so that you get proper amalgam.

Is it a mistake to have a nitric acid solution with about 50mg of mercury(II) nitrate dissolved in 0.1ml of solution? Because I read that you should use an acidic solution to prevent precipitation of hydrolysis products.
Or what other possibilities are there?
 

G.Patton

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Hi
According to wikipedia, for the production of mercury(II) nitrate, hot and concentrated nitric acid is needed, or does that make no difference?
answer:
To initiate the reaction, the glass had to be heated to about 50 degrees, stirring occasionally.

With the mercury(II) nitrate and the aluminiun, is there a ratio to follow? Or how can you determine the correct amount so that you get proper amalgam.
Approximate ratio is from 1:1300 up to 1:650 (mercury(II)nitrate to Al in moles).
Is it a mistake to have a nitric acid solution with about 50mg of mercury(II) nitrate dissolved in 0.1ml of solution? Because I read that you should use an acidic solution to prevent precipitation of hydrolysis products.
Or what other possibilities are there?
This acid is activate Al foil surface to start reaction with Hg. A lot of acid will spoil reduction product. It's not necessary to use.
to prevent precipitation of hydrolysis products
what hydrolysis products do you mean?
 

ACAB

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Hi

answer:
ok, so it makes no difference whether you add hot nitric acid to the mercury or cold and then heat it. Probably the second method is more gentle.

Approximate ratio is from 1:1300 up to 1:650 (mercury(II)nitrate to Al in moles).
This is a relatively large range, with 50g Al this would be an amount from 0.4g to 0.9g. But now I know why increasing the feed did not give much more yield, way too little salt to form the amalgam. Thanks a lot!

Is it better to give more mercury(II) nitrate or only as much as necessary? I always assumed that the amalgamation is a chain reaction, which only needs a push to react completely.
This acid is activate Al foil surface to start reaction with Hg. A lot of acid will spoil reduction product. It's not necessary to use.
What does a lot of acid mean? Acidic solution means I have a little more acid than reacted in the solution.
I dissolved 21g of mercury in 70ml of 60%HNO3, that should give a concentration of 0.1ml of acidic solution to about 50mg of mercury(II) nitrate and I would have put in about 50ml of HNO3 too much.
That would be about 1ml (0,5g salt) acid solution for 50g Al. Is this already too much acid?
what hydrolysis products do you mean?
I think this means monohydrate, octahydrate and hemihydrate.
 

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Is it better to give more mercury(II) nitrate or only as much as necessary?
Necessary amount would be better, excess of Hg salt will make more Hg-contain waste.
What does a lot of acid mean? Acidic solution means I have a little more acid than reacted in the solution.
I dissolved 21g of mercury in 70ml of 60%HNO3, that should give a concentration of 0.1ml of acidic solution to about 50mg of mercury(II) nitrate and I would have put in about 50ml of HNO3 too much.
That would be about 1ml (0,5g salt) acid solution for 50g Al. Is this already too much acid?
I mean excess of acid, your quantitative is ok.
I think this means monohydrate, octahydrate and hemihydrate.
I think an excess of acid can slow down Hg and Al(OH)3 formation reaction in accordance with Le Chatelier's principle
 

ACAB

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I mean excess of acid, your quantitative is ok.
I think an excess of acid can slow down Hg and Al(OH)3 formation reaction in accordance with Le Chatelier's principle
Ok, I see so I don't have to worry about the hydrolysis products but rather that the excess nitric acid is messing with my amalgamation.

I proceeded very theoretically according to the principle I want 50mg per 0.1ml solution and took this formula and calculated the rest:
3HG + 8HNO3 --> 3HG(NO3)²+...+....
601.77g+504.08g -->1027.86g +...+...
2.93g+2.45g -->5g +...+...
5g mercury(II) nitrate + 10ml HNO3 = concentration 0.05g/0.1ml
70ml HNO3 therefore require 21g mercury.
Of the 70ml HNO3, 17.15g=12.55ml should then have reacted and the remainder (57ml) would be the acidic solution.

What would be the best way to save my prepared solution?
-Can I distill off the nitric acid? What would be left, the pure mercury salt? But with the small quantity, however, this would certainly be too costly.

-Or should I rather add mercury and heat the whole thing to get a higher concentration of mercury salt and less acid?
 

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3HG + 8HNO3 --> 3HG(NO3)²+...+....
601.77g+504.08g -->1027.86g +...+...
2.93g+2.45g -->5g +...+...
You made wrong reaction and, hence, amounts of reagents. Look at my topic above, there is correct reaction.
What would be the best way to save my prepared solution?
Seal it airtight and put it in the fridge
-Can I distill off the nitric acid? What would be left, the pure mercury salt? But with the small quantity, however, this would certainly be too costly.

-Or should I rather add mercury and heat the whole thing to get a higher concentration of mercury salt and less acid?
You don't need to do these procedures, man. If you want to solve Hg in HNO3, you need to heat it. You can use reflux condenser to avoid evaporation of acid.
 
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ACAB

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You made wrong reaction and, hence, amounts of reagents. Look at my topic above, there is correct reaction.
But sir, the reaction
HG + 2HNO3 --> HG(NO3)² + NO2 + H2O
from your post cannot be correct,
HG + 2HNO3 --> HG(NO3)²+ H2 would be the correct one if so, but it should probably be ->
HG + 4HNO3 --> HG(NO3)² + 2NO2 + 2H2O , otherwise the molecule number on both sides is not correct, you would be missing one nitrogen and three oxygen. Do you agree with me on this? In any case, nitrogen dioxide (NO2) is formed, I agree with you 100%, I could smell it.
My reaction with nitric oxide (NO)
3HG + 8HNO3 -->3HG(NO3)² + 2NO + 4H2O
would also be correct, from the molecule numbers, but nitric oxide is odorless, so that can't be right, my fault.

No idea why I can find so many reactions for HG + HNO3 and which one is the right one.
Seal it airtight and put it in the fridge
I thought my solution was not right, too acidic, at least that's how I understood you, and I thought of two ways to "rescue" my solution, distill or concentrate. But...
You don't need to do these procedures, man.
Doesn't seem necessary after all, as you just wrote.

I will then use the new reaction if you agree with me for calculation in the future to determine the correct amount of mercury salt.
 

G.Patton

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But sir, the reaction
HG + 2HNO3 --> HG(NO3)² + NO2 + H2O
from your post cannot be correct,
HG + 2HNO3 --> HG(NO3)²+ H2 would be the correct one if so, but it should probably be ->
HG + 4HNO3 --> HG(NO3)² + 2NO2 + 2H2O , otherwise the molecule number on both sides is not correct, you would be missing one nitrogen and three oxygen. Do you agree with me on this?
Yes, you are right! This is exactly right. Thanks for your notification. NO2 is correct product, brown gas.
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I thought my solution was not right, too acidic, at least that's how I understood you, and I thought of two ways to "rescue" my solution, distill or concentrate. But...
Ohh, sorry for misunderstanding. You can evaporate acid, but use well-ventilated place and use mask with gloves!
 
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diogenes

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Hi Patton, I tried putting my foil in the coffee grinder (in my utmost desperation) but was not sure whether it would work, so I left the small balls aside, but then I read your post above and it instilled new hope in me. My question is, can it be used with the normal amalgamation method as well or only with MeOH. It would be a life saver as ripping up all this foil is a killer. Thanks
 

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How do I know when the little balls (made by the coffee grinder) are amalgamated and ready to go. What signs should I look out for?

Also, do I understand well that the reaction needs more foil when using the coffee grinder method? If yes, what is the proportion in your experience?
 

G.Patton

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How do I know when the little balls (made by the coffee grinder) are amalgamated and ready to go. What signs should I look out for?
Color and bubbles. When bubbling is finished, it's ready to go
Also, do I understand well that the reaction needs more foil when using the coffee grinder method? If yes, what is the proportion in your experience?
you have to count it by mass, the cutting and mixing in mixer used for increasing square of surface
 
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diogenes

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Thank you Patton, will try it and will use the same weight of foil (although it appears much less like this and one hour shorter the time it takes :) ).
 

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I wonder if one can use aluminum powder instead of foil or chunks? Something like german dark powder (200 mesh- 2 microns). If you mix that with mercury nitrate, what would be the result?
 

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I wonder if one can use aluminum powder instead of foil or chunks? Something like german dark powder (200 mesh- 2 microns). If you mix that with mercury nitrate, what would be the result?
I have read that it is not so good because you can not get good amalgam from powder, it reacts too quickly, I have never tried it myself, but foil is always used.
 

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Ok, interesting. Where did you read that, I'd love to read it too! I expect the reaction to be downright violent, as reactions usually are with alu powder, but why should the reaction time affect the final product?
I have read that it is not so good because you can not get good amalgam from powder, it reacts too quickly, I have never tried it myself, but foil is always used.
 

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Ok, interesting. Where did you read that, I'd love to read it too! I expect the reaction to be downright violent, as reactions usually are with alu powder, but why should the reaction time affect the final product?
Sorry i cant provide a link, i think it was in an old forum. We are certainly not the only two who think the larger the surface that can react then better, but in this case it is probably not, because practically all cooks always work with foil. Why exactly I can not say, sorry. Perhaps an expert here could answer why no powder but foil is used here.

The reaction may also proceed too fast. For example, a controlled reaction that runs evenly over a long period of time can be much more complete in the conversion of substances than a short violent one.
 

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Ah, ok, I get it. I was just thinking of the reaction to produce the aluminum amalgam. But then there's the reduction of P2NP ... That's where the powdered amalgam might be too quick to work.
 

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for the thermometer thechnic, we need nitric acid only 70% ? (not ok for 60/65/69.5%... not the same price)
 
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