Is there a way to reduce without evaporation?

[downwardsfromzero]

By ethanol you are talking about drinking alcohol

This was with 90% alcohol from the pharmacy and experiments were carried out with dilutions by adding 20% alcohol, also from the pharmacy.

Here's the thread about the original differential solubility experiment.

Also worth mentioning that vodka is a lot more expensive than acetone

Not if you live in Germany. (I'm talking about OTC acetone and the cheapest supermarket vodka. Then they're roughly the same price:
https://www.obi.de/verduenner-abbei...on-reinigungsmittel-transparent-1-l/p/1721455 €6.99/L
RACHMANINOFF Wodka 3-fach destilliert 37,5% Vol | LIDL €7.19/L

Of course, the acetone is ca. 99%, whereas the vodka is only ca. 37% ABV, so the price per liter of absolute alcohol would be €19.17 or so.)

 

[fathomlessness]

Super interesting!

So:
- convert baking soda to sodium carbonate
- base bark with sodium carbonate and dry
- pull with 50% ethanol (add 10% water to 40% vodka)
- freezing ethanol at around -20 C, filter precipitated base residue away
- separate bottom dark layer from top clear layer
- save top layer for re-use
- evap bottom layer to obtain "dirty" dmt freebase yield
- dissolve yield in minimum amount of carbonated water, filter solids away
- evaporate solution to obtain "clean" dmt freebase yield

Right?

I don't really see why you would dry the basified bark when you're just going to be adding water again in the form of 50% ethanol 50% water. If you had 50ml of water in there already, then you put 45ml of 95% ethanol in, it would effectively be the same would it not? Then you wouldn't have to worry about the time it takes to dry bark or phyllodes and could go straight to freeze and separate.

 

[downwardsfromzero]

I think you may find your answer in this thread:

Extracting DMT with ethanol, vinegar and sodium carbonate -endlessness 06/2012

Here's the link, fixed.

 

[fathomlessness]

I think you may find your answer in this thread:

Extracting DMT with ethanol, vinegar and sodium carbonate -endlessness 06/2012

Here's the link, fixed.

Sorry, i think I meant to link this thread instead: Solubility of DMT freebase in aqueous ethanol - some observations

Pls feel free to chime in on the question I asked above yours if you like.

 

[downwardsfromzero]

Super interesting!

So:
- convert baking soda to sodium carbonate
- base bark with sodium carbonate and dry
- pull with 50% ethanol (add 10% water to 40% vodka) < this bit is wrong, as discussed above!
- freezing ethanol at around -20 C, filter precipitated base residue away
- separate bottom dark layer from top clear layer
- save top layer for re-use
- evap bottom layer to obtain "dirty" dmt freebase yield
- dissolve yield in minimum amount of carbonated water, filter solids away
- evaporate solution to obtain "clean" dmt freebase yield

Right?

I don't really see why you would dry the basified bark when you're just going to be adding water again in the form of 50% ethanol 50% water. If you had 50ml of water in there already, then you put 45ml of 95% ethanol in, it would effectively be the same would it not? Then you wouldn't have to worry about the time it takes to dry bark or phyllodes and could go straight to freeze and separate.

Pls feel free to chime in on the question I asked above yours if you like.

Indeed I shall... One reason to dry the basified bark is that any water present would dilute the ethanol by an unmeasured amount. Sodium carbonate forms a number of different hydrates depending on the conditions so not all the water would remain available. Water is/can also be formed in the neutralisation of ammonium/amine salts by a carbonate:
2 R3NH+ + CO3-- = 2 R3N + CO2 + H2O

On a small scale this might not appear significant; best would be to do a comparison on a split sample where one half is dried as some_one suggests and the other half is processed using your no-drying variation.

 

[Woolmer]

I mean add enough acetone to the acidic solution to take the ratio to around 60:40% acetone:water. At that point, the sol'n shouldn't freeze, but the solubility of solute in solution is poor enough that precipitation occurs.

Would the acetate crash out as oil or crystals?