Aluminium amalgam (Al/Hg) summary

[IM BATMAN]

Mercury isn't bounded (connected) with amph free base. When you make extraction from amalgam solution, Mercury remain in water (which than be discarded).

yes..thats what i thought , but, in the classic al/hg amalgam synth routes in rhodium etc...the never do it, in fact add the ketone/mma directly without a single rinse....

 

[IM BATMAN]

The following observation: 15 minutes after adding water to the aluminum foil and the mercury salt, I have a dark gray water solution with many small bubbles that form a foam. After I pour off the water, I hear the aluminum crackling and white smoke rising, a lot of white smoke.

Was I too early to drain the water, or too late?

trust me , too late .... ive done 2 failed amalgams, like the one you are relating , if you use grinded balls , the surface has been scratched a lot and the reaction starts much more faster... as ive seen in less than 5 minutes its ok, even before..... if you wait 30 secs more than you should do, trust me dont add any valuable stuff (precursors etc) because you are willing to loss...
i dont like the grinded balls method, it goes very fast and the best amalgam reaction should spend 6 hours or so... if too quick, the yield will be much lower than if slow reaction...
i prefer the squares , but before to put in the flask you can squeeze all them manually ( in several times, all that fits in your hands each time) to form irregular semi-balls , then it will not stick and cause the loss of reaction foil settled in the bottom... that way are more easy to float, but not ultra expose the AL foil ..... learned by the worst way haha

i had 2 scary attempts , high temp raised too quick and tons of h2 gas all over the place, and...mercury?

 

[IM BATMAN]

In your place I would simply test with a small load if you have gallium available and report the result here.
Gallium forms an amalgam with aluminum just like mercury and produces hydrogen, but there are also some differences at the electron level that make mercury impossible to replace with gallium completly.

what form of gallium is needed? salts or elemental?

 

[ACAB]

trust me , too late .... ive done 2 failed amalgams, like the one you are relating , if you use grinded balls , the surface has been scratched a lot and the reaction starts much more faster... as ive seen in less than 5 minutes its ok, even before..... if you wait 30 secs more than you should do, trust me dont add any valuable stuff (precursors etc) because you are willing to loss...
i dont like the grinded balls method, it goes very fast and the best amalgam reaction should spend 6 hours or so... if too quick, the yield will be much lower than if slow reaction...
i prefer the squares , but before to put in the flask you can squeeze all them manually ( in several times, all that fits in your hands each time) to form irregular semi-balls , then it will not stick and cause the loss of reaction foil settled in the bottom... that way are more easy to float, but not ultra expose the AL foil ..... learned by the worst way haha

i had 2 scary attempts , high temp raised too quick and tons of h2 gas all over the place, and...mercury?

Yes, I now also know, was a misunderstanding, as soon as the soup turns gray and bubbles form it is time, no longer wait. I use a shredder to get small snippets and press them together with my hands, so also a very large surface.
What do you think should take 6 hours? The reduction from the P2NP or the amalgamation?

what form of gallium is needed? salts or elemental?

In the examples elementary is used.

 

[IM BATMAN]

Yes, I now also know, was a misunderstanding, as soon as the soup turns gray and bubbles form it is time, no longer wait. I use a shredder to get small snippets and press them together with my hands, so also a very large surface.
What do you think should take 6 hours? The reduction from the P2NP or the amalgamation?

In the examples elementary is used.

thats the key , dark grey and aluminum squares/balls start to rise up , then proceed inmediatelly.... and personally i always rinse it, 2 times is enough ..the amalgam will continue without problems, and without almost all the mercury.

the 6 hours , thats an old info, i prefeer to let it overnight, but the 6 hours is a minimum of time, if AL foil is dissolved, if not i left close to 12 hours, otherwise low yields for sure. im not doing for amph, so i dont use P2NP , so i assume its for the full amalgam proccess .

 

[ACAB]

and personally i always rinse it, 2 times is enough ..the amalgam will continue without problems, and without almost all the mercury.

I always wonder what you have with your mercury, the amount is very small and would disappear completely from the product after the release of the freebase. As far as I have heard, it has other reasons and that is that the mercury salt (partially dissolved in nitric acid) interferes with the subsequent reaction. Because even if you have rinsed out the mercury, you still have the dirt on your cheek and have to dispose of it.

the 6 hours , thats an old info, i prefeer to let it overnight, but the 6 hours is a minimum of time, if AL foil is dissolved, if not i left close to 12 hours, otherwise low yields for sure. im not doing for amph, so i dont use P2NP , so i assume its for the full amalgam proccess .

The reaction is the same, no matter which amine you reduce, I can only imagine that it is more difficult to reduce P2NP and therefore you need more extreme conditions which makes a slow reaction impossible. The reaction with P2NP has to be exothermic in any case, but also not too hot. I don't know if it makes sense to heat the reaction mass further to maintain the conditions that the reaction continues to run. Unfortunately, there is too little information about what now affects how and how an optimal path should be in all details.

What also surprises me is that no one names the by-products that are formed, nowhere does it say how they can be prevented, or what is formed there and where in the first place. Either such a thing has never been researched or one is silent about it.

 

[IM BATMAN]

I always wonder what you have with your mercury, the amount is very small and would disappear completely from the product after the release of the freebase. As far as I have heard, it has other reasons and that is that the mercury salt (partially dissolved in nitric acid) interferes with the subsequent reaction. Because even if you have rinsed out the mercury, you still have the dirt on your cheek and have to dispose of it.

The reaction is the same, no matter which amine you reduce, I can only imagine that it is more difficult to reduce P2NP and therefore you need more extreme conditions which makes a slow reaction impossible. The reaction with P2NP has to be exothermic in any case, but also not too hot. I don't know if it makes sense to heat the reaction mass further to maintain the conditions that the reaction continues to run. Unfortunately, there is too little information about what now affects how and how an optimal path should be in all details.

What also surprises me is that no one names the by-products that are formed, nowhere does it say how they can be prevented, or what is formed there and where in the first place. Either such a thing has never been researched or one is silent about it.

well , i tested the amalgam with and without rinses, and the result is the same in yields.... then, i prefeer to rinse to eliminate at least a part of it, in the mdma production, there are many routes, but if you decide to make alkali-acid extractions , the HG should just get out , anyway, if the yield are the same...why not try to eliminate at the very first step? maybe in the final result is not important, but if you can be less expossed to HG while reach those steps i think worth the 3 minutes in rinses step.

as for the p2np , in fact i think is not neccesary at all that the AL foil is completely "melted"(my english haha) , it seems you can discard a lot of unreacted foil without yield loss, but in MDMA if you dont wait till the AL foil is completely reacted you will have a big loss on yield.

as for the temperature, i think should be apply to keep the correct reaction temperature, even when the exotermic reaction finished, when done it the bubbling etc keeps running and less time to wait...
if we left it by its owns , the reaction will continue till all is reacted, but it can delay more than 12 hours, normally left it overnight.

as the amalgam is an equilibrium difficult to control al 100% we have to keep watching, ideally in those 6 hours should finish the reaction, without external temp, but it depends on a decission of maybe seconds? just wait to see dark gray... wait till foil floats? when it happens how much will wait till rinse , or add the precursors?
maybe one day ill be able to do always the same, but this day has not reached yet haha

sorry for my SpainGlish

 

[mixxxman]

man, to be honest , you should have a bit more of patience, and maybe dont think the people are stupid just because are asking something thah you know easily....

anyway, you replied something very different in this thread about when start to add the ketone and methylamine after amalgam started, ive correctly asked about the best moment to add those, and as diogenes said for example, and you were agreed, the best moment is when the first 3 signs appears instead to wait too much...
thats what im asking for, i know how to do amphetamines.

i can understand those questions are boring for you, then i would recommend you to not reply to it.
i know deeply a lot of things in a lot of fields and if i really want to help, ill do kindly , because someone have the same doubt you had time ago.
dont take as an ofense, just saying.

as for the non english people trying to talk, be patient sir, there are much more people in the world talking spanish than english, and when a tourist or someone come to my country and at least try to talk spanish im always happy , kind and patient.
the other day i had to reformulate a question just because you think we all have to speak perfectly english..and every single person that readed it , for sure understood it.

totally agree bro..
humility is the key of the knowledge...
and yes, i had the same problem, when i made my amalgam...
cause i wanted to rinse it to much.. but the problem the h2o react with the al.hg...
some people leave it... and they say : don't care, with the A/B extraction no problem...
but i am a bit scared too, to have a bit of mercury in my organic solvent or what ever...
i am very paranoiac with the mercury salt !

thank you for your message and never give up, i wish this place can be a beautiful sharing area and a chemical family