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Preparation of mercury nitrate with subsequent use in Al/Hg. Video.

HIGGS BOSSON

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In some syntheses, such as aluminum amalgam, mercury nitrate is used to reduce phenylnitropropenes and phenylnitrostyrenes, which is limited in circulation in some countries. If mercury nitrate is difficult to buy, then it can be prepared by yourself. This will require only a mercury thermometer and concentrated nitric acid. The video then shows the synthesis of mercury nitrate from the described components, followed by use in aluminum amalgam to reduce 1-phenyl-2-nitropropene to amphetamine.
Video description:
0:06-0:40 - extraction of mercury from the thermometer 0:45-1:45 - loading of nitric acid.
1:45-2:00 - reaction of nitric acid and mercury, followed by
mercury nitrate two valence. The reaction proceeds with the release of NO2 gas and water.
2:15-4:00 - amalgamation of aluminum (12 g of household foil) using a prepared solution of mercury nitrate.
4:10-5:55 - reduce of 1-phenyl-2-nitropropene (a solution of 10 g P2nP in acetic acid and alcohol was used).
 
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billy

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so the final solution shown in the video has , al still in it are we simply takiing the al out and using the rest of the solution as are nitrate ???
 

DocX

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Great stuff, thanks! So after reacting the mercury, how would one go about isolating the mercury salt from the solution if you wanted to save it for later? Boiling off the nitric acid?
 

Marvin "Popcorn" Sutton

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If dry mercury nitrate is needed, the mercury nitrate solution must be cooled until crystals fall out, filtered, and dried.
 
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Marvin "Popcorn" Sutton

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so the final solution shown in the video has , al still in it are we simply takiing the al out and using the rest of the solution as are nitrate ???
Reuse of mercury nitrate solution in water is not possible. Mercury nitrate is hydrolyzed .
 

uselessdragon

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Is nitric acid a readily available substance for purchase? Or is it more easily acquired via darkweb resources?
 

HIGGS BOSSON

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Is nitric acid a readily available substance for purchase? Or is it more easily acquired via darkweb resources?
Nitric acid is not a precursor and is fairly easy to buy.
 

DocX

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I guess it depends on where you are. In the EU, nitric acid is a listed chemical and cant be bought without an end user license. Neither can you buy sulphuric acid. But you can make nitric acid if you first manage to get sulphuric acid, quite easily.
 

DocX

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Here is the legislation in your country. I cant find nitric acid there, but sulphuric acid is listed as a Class B precursor. Along with things like acetone, MEK, toluene and ether.
https://laws-lois.justice.gc.ca/eng/acts/C-38.8/ (clearnet)
 

Montecristo

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any other acids i can use? nitric is another restricted chem here
 

DocX

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You need the nitric acid to nitrate mercury. If you can't get it, make it. If nitric acid is restricted then sulphuric acid is probably restricted too, but there's always ways. Get sulphuric acid from car batteries, boil it down and then distill it. You'll find hundreds of videos on Youtube on how to do this. Once you have concentrated sulphuric acid you can make nitric acid- you'll find about as many videos on this on Youtube too.
If you do proper research you can sometimes find nitric acid in lower concentrations in products not labelled "nitric acid". I found it in PH adjustment liquids for home growing kits, for example (although that has been changed to phosphoric acid now).
OR you could try making a nitrating mixture using ammonium nitrate and sulphuric acid. You'll find videos on this on ... well, I think you should get it by now. Otherwise, just give it up. Then this is not for you. You will have to dig up information by yourself too, noone will be able to spoonfeed you every single detail.
 
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DocX

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I have a question though: what would happen i you react the mercury nitrate with aluminium powder? Too violent? I have some fine german dark alu powder from my pyro days ...
 

Morpheus

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I can't watch the video :(

Any clever solutions for stirring? overhead is preferable. Electric drill mounted high up, pp paddle with a looong shaft n tight hole? really tight on the shaft to prevent distil escape? with condenser of course...or is a nice loooong pp hose sufficient? Talkin bout mdma al/hg without nitro. Is a overhead stirrer stainless steal with high corrosion resistance ok? I guess not. Most reaction vessels I see it looks liek they have some stainless steal parts, like the stirrer. 25-50L could be nice...but do they work. Just doing a synth rendering in my brain to see if its anything I should read more into. I would like some good ideas for diy large reaction vessels...or is it better to just buy a glass one premade?
 
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Loooow

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any other acids i can use? nitric is another restricted chem here
Synthesize nitric acid yourself!

Synthesis: 80g potassium nitrate in a round bottom flask together with 250ml 98% sulfuric acid.
Connect the distillation bridge and let everything boil.
The distillate will be your
high quality HNO3! (You should dilute it a little bit with distilled water, because it will be
water, because the distillate is azeotropic HNO3, which, despite its highest possible concentration
which, despite its highest possible concentration, apparently reacts more slowly than somewhat diluted
HNO3.)
 

billy

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Synthesize nitric acid yourself!

Synthesis: 80g potassium nitrate in a round bottom flask together with 250ml 98% sulfuric acid.
Connect the distillation bridge and let everything boil.
The distillate will be your
high quality HNO3! (You should dilute it a little bit with distilled water, because it will be
water, because the distillate is azeotropic HNO3, which, despite its highest possible concentration
which, despite its highest possible concentration, apparently reacts more slowly than somewhat diluted
HNO3.)
sorry why would this be neccersary , if we already had sulfuric acid would it not be easier just to use this.
 

G.Patton

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Synthesize nitric acid yourself!

Synthesis: 80g potassium nitrate in a round bottom flask together with 250ml 98% sulfuric acid.
Connect the distillation bridge and let everything boil.
The distillate will be your
high quality HNO3! (You should dilute it a little bit with distilled water, because it will be
water, because the distillate is azeotropic HNO3, which, despite its highest possible concentration
which, despite its highest possible concentration, apparently reacts more slowly than somewhat diluted
HNO3.)

Nitric acid syntheses

 

G.Patton

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sorry why would this be neccersary , if we already had sulfuric acid would it not be easier just to use this.
Mercury sulphate (HgSO4) is extremely dangerous and hard to handle substance.
 

Loooow

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I have a question though: what would happen i you react the mercury nitrate with aluminium powder? Too violent? I have some fine german dark alu powder from my pyro days ...
 

Loooow

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Better not do that.... I'm not a chemist but I'm sure that's not a good idea!!!!
 
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