Is there a way to reduce without evaporation?

[fathomlessness]

If only DMT extractions were as easy as harmalas where you can salt the harmalas out and then decant the water in order to redissolve and base..

I understand this subject hasn't a quick and easy viable solution, so I just want to make a thread to get some input on thinking about the ways in which we might be able to avoid the evaporation stage.

All I can think of is leaving the solution in a wide tray outside in summer to evaporate, this could attract mould and insects though, not to mention the skin of oils that builds up on the surface which would prevent evaporation. Is there any chemical additive in industrial practices that will make water evaporate twice as fast at room temperature?

 

[benzyme]

either salt or free base... you can freeze precipitate, and decant the mother liquor.
eventually you have to evaporate trace solvent

 

[fathomlessness]

either salt or free base... you can freeze precipitate, and decant the mother liquor.
eventually you have to evaporate trace solvent

To my understand you can not salt DMT out of an acidic solution. Freebasing the solution would require more non-polar solvent which is costly.

 

[benzyme]

either salt or free base... you can freeze precipitate, and decant the mother liquor.
eventually you have to evaporate trace solvent

To my understand you can not salt DMT out of an acidic solution. Freebasing the solution would require more non-polar solvent which is costly.

no, but you can crash it out in acetone by freeze precipitation.

 

[Jagube]

either salt or free base... you can freeze precipitate, and decant the mother liquor.
eventually you have to evaporate trace solvent

By solvent do you mean water?

And when you say freeze precipitate, do you mean something like this:

1. Put the jar with the acidic or basic soup in the freezer.
2. Let it freeze throughout.
3. Take it out of the freezer and let it thaw just a little bit, so the non-water fraction doesn't stick to the ice.
3. Remove the ice and discard it.
4. Evaporate the liquid water.

?

 

[doubledog]

I also wonder what keeps dmt freebase in water solution after base is added as it should be not soluble in water.

 

[benzyme]

either salt or free base... you can freeze precipitate, and decant the mother liquor.
eventually you have to evaporate trace solvent

By solvent do you mean water?

And when you say freeze precipitate, do you mean something like this:

1. Put the jar with the acidic or basic soup in the freezer.
2. Let it freeze throughout.
3. Take it out of the freezer and let it thaw just a little bit, so the non-water fraction doesn't stick to the ice.
3. Remove the ice and discard it.
4. Evaporate the liquid water.

?

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.

 

[some one]

Now that's interesting benzyme. You say both salt and FB work?

If so we could do bark water pulls, evap solution down, add aceton, freeze pricipiate, collect DMT-tannate + misc compounds?

As for FB (doing the same as above but after adding the base) the remaining base will also precipitate so you'd need to clean the final yield with NPS.

 

[Jagube]

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.

Cool, never heard of this before. Presumably IPA would work the same, but the ratio would be different?

Is the decrease in solubility selective, as in favoring DMT over other things?
Could this be as good as to provide a (crude-ish) extraction path that avoids pulls, or is its usability limited to being an alternative to evaporation?

 

[some one]

lol Jagube. Sync.

Does it only apply to acetone with water? If ethanol also freeze pricips freebase dmt then this won't work:

When I find the time I will experiment with getting zero sodium carbonate residue in ethanol. By hope the following procedure works:

- convert baking soda to sodium carbonate
- base bark with sodium carbonate and dry
- pull with 96% ethanol
- freezing ethanol at around -15 C, filter precipitated base residue away
- distillate ethanol down to 10% volume, save returned ethanol for re-use
- evaporate remaining ethanol to obtain "dirty" dmt freebase yield
- dissolve yield in carbonated water, filter any solids away
- evaporate solution to obtain "clean" dmt freebase yield

Back to acetone with water:

Imaging obtaining DMT in its natural salt form using this tek.
Then dissolving it in water and nebulizing.
Now that's high tech..

 

[Samvidbuho]

doubledog, I too have been wondering recently what keeps DMT Freebase in basic solution. I'm doing some solubility tests now, but I'm sure it has to do with the degree of basicity of the water - I've noticed that very high pH water holds on to freebase extremely well, and if the solution is diluted to bring the pH down then more freebase will precipitate out. I think the solubility of freebase in water increases considerably with increasingly high pH levels But yeah it's interesting, because with its low aqueous solubility this wouldn't be expected..

 

[downwardsfromzero]

lol Jagube. Sync.

Does it only apply to acetone with water? If ethanol also freeze pricips freebase dmt then this won't work:

When I find the time I will experiment with getting zero sodium carbonate residue in ethanol. By hope the following procedure works:

- convert baking soda to sodium carbonate
- base bark with sodium carbonate and dry
- pull with 96% ethanol
- freezing ethanol at around -15 C, filter precipitated base residue away
- distillate ethanol down to 10% volume, save returned ethanol for re-use
- evaporate remaining ethanol to obtain "dirty" dmt freebase yield
- dissolve yield in carbonated water, filter any solids away
- evaporate solution to obtain "clean" dmt freebase yield

[...]

Can't remember where else I posted about this, but it's worth repeating here:
DMT freebase is exceedingly soluble in ethanol. DMT freebase when dissolved in 50% aqueous ethanol separates into two phases (both liquid) at about -18°C. (It's possible that this is the eutectic mixture.) The dark yellow lower layer is ethanolic DMT, the colourless upper layer is aqueous ethanol with virtually no DMT. The upper layer can be removed with a pipette. This could be a viable way of reducing liquid volume in the case of ethanolic solutions of freebase.

 

[some one]

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?

 

[Jagube]

Can't remember where else I posted about this, but it's worth repeating here:
DMT freebase is exceedingly soluble in ethanol. DMT freebase when dissolved in 50% aqueous ethanol separates into two phases (both liquid) at about -18°C. (It's possible that this is the eutectic mixture.) The dark yellow lower layer is ethanolic DMT, the colourless upper layer is aqueous ethanol with virtually no DMT. The upper layer can be removed with a pipette. This could be a viable way of reducing liquid volume in the case of ethanolic solutions of freebase.

How? Is the ethanolic DMT layer significantly smaller in volume?
Does this apply to fb only or salts too?
What about the other stuff, the plant gunk - will it precipitate, go in the top layer or the bottom one?

And again, can IPA be used?

- pull with 50% ethanol (add 10% water to 40% vodka)

If you add water to 40% vodka, the result will be less than 40% ethanol.

- freezing ethanol at around -20 C, filter precipitated base residue away

I don't think it will freeze, but I take it you meant "cool ethanol to -20C".

 

[some one]

Brain fart, had 40% water in my head, but the 40% is reference to the alcohol content of course. Yes, meant cool to -20 C indeed.

Good questions, looking forwards to the answers as well.

 

[fathomlessness]

either salt or free base... you can freeze precipitate, and decant the mother liquor.
eventually you have to evaporate trace solvent

To my understand you can not salt DMT out of an acidic solution. Freebasing the solution would require more non-polar solvent which is costly.

no, but you can crash it out in acetone by freeze precipitation.

Thanks. I'll link your thread here by the way:

https://www.dmt-nexus.me/forum/default.aspx?g=posts&m=1033964 - Benzyme 12/2019

In this thread benzyme seperates dmt laden acetone/water mixture with sodium hydroxide and epsom salt.

It is to my understanding that I could essentially dry a solution of bark mixture with sodium carbonate dissolved. Once dry, use acetone to collect the alkaloids. Once collected with acetone, mix with 40% water. Then add NaOH and epsom salt (MgSO4). Then decant the acetone and evaporate to yield product.

This would thereby conclude the thread as it offers a way to use little water and no boil off evaporation.

 

[fathomlessness]

lol Jagube. Sync.

Does it only apply to acetone with water? If ethanol also freeze pricips freebase dmt then this won't work:

When I find the time I will experiment with getting zero sodium carbonate residue in ethanol. By hope the following procedure works:

- convert baking soda to sodium carbonate
- base bark with sodium carbonate and dry
- pull with 96% ethanol
- freezing ethanol at around -15 C, filter precipitated base residue away
- distillate ethanol down to 10% volume, save returned ethanol for re-use
- evaporate remaining ethanol to obtain "dirty" dmt freebase yield
- dissolve yield in carbonated water, filter any solids away
- evaporate solution to obtain "clean" dmt freebase yield

[...]

Can't remember where else I posted about this, but it's worth repeating here:
DMT freebase is exceedingly soluble in ethanol. DMT freebase when dissolved in 50% aqueous ethanol separates into two phases (both liquid) at about -18°C. (It's possible that this is the eutectic mixture.) The dark yellow lower layer is ethanolic DMT, the colourless upper layer is aqueous ethanol with virtually no DMT. The upper layer can be removed with a pipette. This could be a viable way of reducing liquid volume in the case of ethanolic solutions of freebase.

By ethanol you are talking about drinking alcohol (vodka). Why couldn't denatured alcohol be used? (also called methylated spirit in Australia, New Zealand, South Africa, and the United Kingdom).

Also worth mentioning that vodka is a lot more expensive than acetone (ie 60/40 tek hypothesis above from benzyme).

 

[fathomlessness]

You say both salt and FB work?

either salt or free base...

I don't understand how salt would work. DMT salts like DMT-fumarate are insoluble in acetone afaik.

If so we could do bark water pulls, evap solution down, add aceton, freeze pricipiate, collect DMT-tannate + misc compounds?

or rather add a small amount of sodium carb water to bark and dry it. Then add acetone. Which was what the thread was trying to do "find a way to reduce without evaporation". That would be far less time consuming than doing 3 boils and reducing.

As for FB (doing the same as above but after adding the base) the remaining base will also precipitate so you'd need to clean the final yield with NPS.

Might need more than a naphtha wash. maybe another mini A/B or backsalt. I imagine it would be filthy with tannins and microparticles of bark.

 

[fathomlessness]

Can't remember where else I posted about this, but it's worth repeating here:
DMT freebase is exceedingly soluble in ethanol. DMT freebase when dissolved in 50% aqueous ethanol separates into two phases (both liquid) at about -18°C. (It's possible that this is the eutectic mixture.) The dark yellow lower layer is ethanolic DMT, the colourless upper layer is aqueous ethanol with virtually no DMT. The upper layer can be removed with a pipette. This could be a viable way of reducing liquid volume in the case of ethanolic solutions of freebase.

How?

I think you may find your answer in this thread:


Solubility of DMT freebase in aqueous ethanol - some observations
Extracting DMT with ethanol, vinegar and sodium carbonate -endlessness 06/2012

 

[doubledog]

Maybe it could be possible to partially freeze the acidic solution and separate the ice. It should lead to a more concentrated soup, and alks hopefully stay in nonfreezed fraction.