Al/Hg reduction

icecool · Insistent Chemist

Can people post there method on how they do an reduction using Al/Hg.
Like how to make the Al pieces, how much Al for how much P2NP.
How much GAA and how much solvent used in total in the reaction and how much Hg salt is used and just about the reaction how long reflux, what stirring method.
How big flask for how much P2NP, how long reflux, how long does it normally take for 20g of Al foil to dissolve and 10g P2NP etc, how much water is used...
These are two pics SWIM sent me of what his Al looks like it are 2 different types.
He guesses it is not good to use the Al as it looks like in these pictures, but he isn't sure.
On one pic it is put in the grinder for a long time like 15 second the other one 5 seconds.

Much thanks in advance.

bio · Working Bee

There is, IIRC, a procedure for PNP on the Rhodium archive.

The pics are good and somewhere in between the 2 is what you want about 10 sec.
Loosely fold the foil in half, strain out all the little pieces and the Al lasts much longer. Also use the Extra Heavy Duty foil if you can find it.

PM me if you don't get your answers.

Radiumhero · Sun Aug 28, 2005 4:36 pm

Well if u are not sure mak a mix try to get pure Al foil ( there are online stores )
and theres one more intresting thing swirh found some nice AL "foil" used
for isolating and stuff with a thickness of 0.1 - 0.8 mm wich is a damn lot ..
but the prices forit are rather high , on the other hand one could gain thick al
by buying food that comes on those thick al plates covered with plastic foil ..

bio · Working Bee

........on the other hand one could gain thick al
by buying food that comes on those thick al plates covered with plastic foil .........

Make sure you test these first because most of these do not work.

Buying "pure" Al as was suggested is really the only way to go considering the effort required to get to the reduction stage. Look on SM for a recent post I made on sources of good Al.

icecool · Insistent Chemist

What about making rings of Al I've heard of 1cm width strips and 4cm long and wrap it around your finger.
0,2-0,3mm thick Al; anyway is it better to stirr an Al/Hg reaction constantely (SWIM has the options overhead stirring and magnetic stirring).
SWIM also heard it is better to occasionally stirr....if so every 10minutes for 1 minute stirring is that enough?
SWIM is going to use EtOH for his next Al/Hg reaction found it for 5 liters for 17,94 euro hehe....

nubee · Master Archiver

in this reduction the hg is used to "clean" the alu surface, could you just dip in KOH or NaOH for a bit to do the same thing ???

also there is no such thing as pure aluminium foil it is an alloy, the white residue is silicon and the black is iron... there is more silicon in the tougher sheets as used for stove protectors.

proxy · Mon Sep 05, 2005 11:11 am

this is the stuff to use.... its available through a major australian welding supplier for around $25 ... Very Happy

icecool · Insistent Chemist

Some alu foil is 99% pure Al or even more.
You just need to search for it, and no you can't use KOH to clean the surface, at least not the purpose in the Al/Hg reduction.
The Hg also prevents a new surface of Al2O3 forming on the Al.

bio · Working Bee

.......in this reduction the hg is used to "clean" the alu surface, could you just dip in KOH or NaOH for a bit to do the same thing ???................

NaOH or KOH solution (very dilute) is often used to clean the Al surface which promotes better amalgamation with the HgCl2. This is usually not needed but if any grease traces they can be removed with hexane (white gas) or sanding for thicker Al.

Vogel has a procedure but I think the 10% lye is a misprint. Should be 1% or less, just try it and you will see

Even my ACS Al granuals have some traces of cutting oil I discovered.

Mercury metal or a mercury salt is needed to amalgamate by definition (amalgam).

icecool · Insistent Chemist

SWIM had a better reaction, and a 19% yield.
Always get's around 19% but the reaction was much nicer and steam distilled to yield ~3ml of freebase, but unpure, finally he got 2,1g of amphetamine sulfate.
Used ~0,5ml H2SO4 98%.
Started with 4,8g of P2NP and 9g of Al foil reduced in EtOH.

The point is, that he now folded the al 4 times normally he doesn't even fold it once.
So well 4 times so it was 0,3mm thick now, and then cut strips of 5cmx1cm.
And folded this around a pencil.
So there was also no need to stirr it constantely but only every 15min or so a swirl.

icecool · Insistent Chemist

SWIM had a better reaction, and a 19% yield.
Always get's around 19% but the reaction was much nicer and steam distilled to yield ~3ml of freebase, but unpure, finally he got 2,1g of amphetamine sulfate.
Used ~0,5ml H2SO4 98%.
Started with 4,8g of P2NP and 9g of Al foil reduced in EtOH.

proxy · Thu Sep 15, 2005 7:55 am

i recall reading not long ago (but i cant find nemore) someone advising to do a practice reduction before the real thing, i think they mentioned the words methoxy and ethoxy, and maybe methanol ...

otherwise is there some material that could be practice reduced al/hg to practice technique and materials ???

bio · Working Bee

Al Methoxide or Ethoxide prep will give the hang of it although not a reduction..

At least you will prove the Al quality and method of amalgamation etc. before wasting valuable intermediates.

To make the methoxide use 20ml+ MeOH per gram Al. When it all dissolves you know it worked. Reaction must be anhydrous, means dry,dry, dry, otherwise it won't start or just reacts with the water.

Vogel has the procedure using IPA. Maybe you read my posts on the SM forum where
this was suggested.

Stinging_Nettle · Thu Sep 15, 2005 3:12 pm

Al amalgam is not hard to do. The method Shulgin uses in the MDMA section is a good template with two corrections.

(I) He uses alot of HgCl which is not really necessary.
(II) NaOH washes are not required unless you are using old pie tins as your Al source.

There is no magical way to do these reactions other than I think it is possible for the product to get trapped in all the gakk post reaction during the work-up.

bio · Working Bee

Shulgins method is not really very good IMHO. Runs too cold, not long enough
with too much aluminum.

Having done it several times years ago the yields do not compare to
newer methods!