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Extracting DMT with ethanol, vinegar and sodium carbonate Options
 
some one
#261 Posted : 11/18/2019 12:49:48 AM

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skoobysnax, true. For pharma you'd want a dmt-salt.

Regarding freebase creation for smoking, call me a purist, but I don't like the idea of some base left in spice, let alone calcium /sodium salts. I also prefer not to evaporate non food grade solvents like lab grade IPA down to obtain yield.
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some one
#262 Posted : 12/18/2019 1:47:51 PM

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Update:
I read through this entire topic again and really like Eaglepath's post.
I combined his/her procedure with other knowledge /input and came up with the following plan:

1. Obtain base
Sodium Carbonate "SC" or Calcium Hydroxide "CH". Go for food grade. SC can be made by heating easily obtainable baking soda. CH is preferred for its low solubility. If the CH is less than 100% pure it can contain Calcium Carbonate.

2. Obtain alcohol
Food grade 96% grain ethanol, or >99% lab grade Isopropyl Alcohol (IPA). Optional: choose one of the following drying agents: Calcium Oxide, Sodium Sulphate, or Calcium sulphate to dry your alcohol with.

3. Extract
- cook bark 3x, preferably in (distilled) water (don't use vinegar etc.)
- discard plant matter and evaporate solution down to a low volume
- add base after cooling and evaporate dry (optional: use a vacuum desiccator)
- pull based mix with alcohol
- optional: cool the alcohol to -15c to -17c, filter precipitated base away
- optional: distillate the alcohol down to 10% volume prior evaporation
- evaporate the alcohol containing the actives
- the yield is (less pure) DMT

Alternative:
Instead of cooking and discarding plant matter, do a STB on the bark with minimal water, then evaporate dry and pull the plant mix with alcohol. This saves cooking time, but a larger amount of alcohol is required to pull. Can be expensive if grain ethanol is used and not distilled.

4. Clean up (optional)
- dissolve yield in carbonated water, filter away solids and evaporate dry
- pull with alcohol, filter away solids and evaporate dry
- the yield is (more pure) DMT

Notes:
No vinegar or other acids are used, as these form calcium /sodium salts when combined with bases, contaminating final yield. Carbonated water has a low pH and everything in it fully evaporates prior basing (no acids reacting with bases forming salts). If you choose to use acid, choose citric or fumaric over acetic. Said to give a cleaner result.

As endlessness suggested and doubledog reports success with, the final yield can be washed with a minimum amount of water to dissolve and get rid of base and salt residues. In this case the use of acids prior basing, or the use of SC as base leaving residue in final yield can be counteracted.

Ethanol probably cannot be dried with Anhydrous MgSO4. It can be dried with Calcium Oxide. This can be made DIY: Buy Calcium Carbonate (chalk), convert into Calcium Oxide using a oxy-propane blowpipe. Optional: convert Calcium Oxide into CH by slowly(!) adding water (danger: very intense exothermic reaction).

Further research:
Maybe a sufficiently small amount of alcohol can be used to pull the based mix (with no plant material), saving costs without needing to distillate the alcohol for reuse.

Maybe you can simply use (wet) 96% ethanol to pull moist CH/SC base mix (either boiled down actives or plant mix) by placing the pulled alcohol in the freezer, precipitating all base residue.

Maybe freezing dry alcohol is not required if CH is used as base and the based mix is fully dried prior pulling.

Maybe the initial yield is clean enough and no clean-up procedure is needed.

Conclusion:
Still some research to be done, but the goal is to use all food grade products to obtain pure freebase DMT with zero base and zero salt residues. Thank you endlessness for all the inspiration! I will experiment and report results.
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downwardsfromzero
#263 Posted : 12/28/2019 1:53:56 AM

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Nice outline, here's my thoughts and commentary:
Firstly, lets clarify a few cations Wink
some one wrote:
Update:
[...]If the CH is less than 100% pure it can contain SC.
No, it will contain calcium carbonate. Mixing 'CH' with 'SC' and water produces crude sodium hydroxide and a suspension of calcium carbonate, however.

Quote:
1. Obtain base
buy Calcium Carbonate (chalk), convert into Sodium Oxide using a oxy-propane blowpipe. Save some and convert some into CH by carefully adding water (intense exothermic reaction).
Calcium oxide.

Quote:
2. Obtain alcohol
Food grade 96% grain ethanol, or >99% lab grade Isopropyl Alcohol (IPA). Optional: choose one of the following drying agents: Sodium Oxide, Anhydrous MgSO4, Sodium Sulphate, or Calcium sulphate to dry your alcohol with.
Again, Calcium oxide.

Technical aspects:
Quote:
- optional: cool the alcohol to -15c to -17c, filter precipitated base away
I strongly suspect DMT will not precipitate from 96% ethanol at that temperature, and certainly not as crystals if it does separate. It separates from 50% ethanol as a highly concentrated oil containing an estimated 50% ethanol (the remainder being DMT and a trace of water) at -18°C. This suggests to me it will remain in solution at that temperature. 400mg of DMT easily liquefies with a single drop of 90% ethanol at room temperature and does not resolidify at -18°C.

Quote:
No vinegar or other acids are used, as these form calcium /sodium salts when combined with bases, contaminating final yield. Carbonated water has a low pH and everything in it fully evaporates prior basing (no acids reacting with bases forming salts).
There will be plant acids present in the source material used. This still means there will be salts produced - but of course, they will be there in smaller amounts.

Quote:
Further research:
Maybe a sufficiently small amount of alcohol can be used to pull the based mix (with no plant material), saving costs without needing to distillate the alcohol for reuse.
At some point one encounters the problem that most of the solvent remains physically absorbed by the dry material.

Quote:
Maybe you can simply use (wet) 96% ethanol to pull moist CH/SC base mix (either boiled down actives or plant mix) by placing the pulled alcohol in the freezer, precipitating all base residue.
What I would suggest is dilution of the 96% ethanol extract with an equal volume - perhaps more - of distilled water, followed by freeze concentration, whereby practically all the alkaloid will precipitate as an oil which can then be swiftly removed with a Pasteur pipette. This should at least serve to reduce the volume of ethanol without having to use thermal or ventilation-based evaporation. It is fair to suspect it may be reliant on having a sufficiently concentrated initial solution.

Quote:
Maybe freezing dry alcohol is not required if CH is used as base and the based mix is fully dried prior pulling.
Dry (absolute) ethanol is very hygroscopic and not that easy for the hobbyist to obtain without actually purchasing it. Magnesium sulfate won't dry 96% ethanol, I'm pretty certain. Calcium oxide is again the key, although those lumps of rock might not be food grade. [EDIT: it seems this can also be achieved with straw, sawdust or cornmeal - so I've rather overstated the difficulty level here.]


SAFETY NOTE

PLEASE NOTE THAT THE FOLLOWING PROCEDURE IS LIKELY TO BE DANGEROUS!
Hydration of calcium oxide can cause it to reach a temperature of 300°C, which is capable of igniting some combustible materials!
An only partially tangential thought here is that using normal vodka to slake (hydrate) your calcium oxide would be a potential short-cut to making high proof ethanol simultaneously with calcium hydroxide, although it would be wise to use distillation apparatus for this process as the heat of hydration would certainly evaporate a lot of the ethanol.

56g of CaO would be hydrated by 18g of water found in 18*(100/(100-37.5)) = 28.8ml of 37.5% ABV vodka. Density of CaO is 3.3g/cm3 so that's about 17ml of CaO solid. Ca(OH)2 has a density of 2.211 g/cm3 so the resulting 74g has a volume of about 33.5ml.

The heat of hydration of CaO is -63.7kJ/mol; the specific heat capacity of of EtOH is 2.5kJ/kg/K and its specific latent heat of vaporisation is 85J/kg. Subtracting 18ml of water leaves us with 10.8ml of EtOH. This equates to 10.8*0.789=8.52g of EtOH; heating this amount by 60K requires 2.5*8.52*60=1.28kJ and evaporating it requires (85/1000)*8.52=0.724J (not kJ!) That leaves a generous 63.4kJ to heat up the ethanol vapour and the calcium hydroxide. (I haven't checked the spec. heat cap. of EtOH vapour, but its density is roughly 0.724kg/m3 at s.t.p., so we'd get a good 12l of vapour produced.) We might not get to see much of that ethanol Big grin

Moral of the story: adding (too much) CaO to (too much) vodka too quickly might cause an explosion. You have been warned!

(Using CaO to dehydrate already high proof ethanol is a different story but it pays to examine the thermodynamics for the ABV you are intending to use.)
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some one
#264 Posted : 12/28/2019 5:03:14 PM

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Hi downwardsfromzero,

Silly of me to mix up sodium/calcium multiple times. I've corrected my post above. Note for the readers: CH and SC are not official abbreviations.

Quote:
I strongly suspect DMT will not precipitate from 96% ethanol at that temperature, and certainly not as crystals if it does separate. It separates from 50% ethanol as a highly concentrated oil containing an estimated 50% ethanol (the remainder being DMT and a trace of water) at -18°C. This suggests to me it will remain in solution at that temperature. 400mg of DMT easily liquefies with a single drop of 90% ethanol at room temperature and does not resolidify at -18°C.

The freezer step is to precipitate and separate base residue. The DMT stays dissolved, obtained by evaporation in the next step. The freezer step to precip base might not be necessary with CH, but could be done at least once just in case.

Quote:
There will be plant acids present in the source material used. This still means there will be salts produced - but of course, they will be there in smaller amounts.

That's a very good point. I guess the only way to get rid of these salts is to do a water wash on the final yield as endlessness mentioned.

Quote:
At some point one encounters the problem that most of the solvent remains physically absorbed by the dry material.

If you boil and discard the plant material and reduce the solution to a dry powder, the solvent absorbing plant matter is a much smaller volume. Of course boiling and reducing takes much more work /time vs basing and pulling straight from the plant material.

Quote:
What I would suggest is dilution of the 96% ethanol extract with an equal volume - perhaps more - of distilled water, followed by freeze concentration, whereby practically all the alkaloid will precipitate as an oil which can then be swiftly removed with a Pasteur pipette. This should at least serve to reduce the volume of ethanol without having to use thermal or ventilation-based evaporation. It is fair to suspect it may be reliant on having a sufficiently concentrated initial solution.

This is really interesting!

Quote:
Dry (absolute) ethanol is very hygroscopic and not that easy for the hobbyist to obtain without actually purchasing it. Magnesium sulfate won't dry 96% ethanol, I'm pretty certain. Calcium oxide is again the key, although those lumps of rock might not be food grade. [EDIT: it seems this can also be achieved with straw, sawdust or cornmeal - so I've rather overstated the difficulty level here.]

Good to know Magnesium sulfate won't work - edited. The food grade thing (heavy metals etc) can be an issue for this project. Will check out the straw, sawdust or cornmeal options. If the freezer step works to precip base, then drying the ethanol might not be needed.

Thanks for elaborating regarding the safety note regarding converting Calcium Oxide to CH with water. I added an extra warning to my post just in case.
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downwardsfromzero
#265 Posted : 1/12/2020 6:24:20 PM

Comical egg spurt; Senile mumbler

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Quote:
I guess the only way to get rid of these salts is to do a water wash on the final yield as endlessness mentioned.
Some calcium salts with organic anions are poorly soluble to practically insoluble. Among these would be calcium oxalate and calcium fumarate. Others will be quite appreciably soluble - it would be wise to look these up but calcium malate and calcium citrate will sometimes be fairly soluble depending on the cation:anion ratio.

Sodium salts are almost always fairly soluble.
Ora, lege, lege, lege, relege et labora

“To be GOVERNED is to be watched, inspected, spied upon, directed, law-driven, numbered, regulated, enrolled, indoctrinated, preached at, controlled, checked, estimated, valued, censured, commanded, by creatures who have neither the right nor the wisdom nor the virtue to do so. To be GOVERNED is to be at every operation, at every transaction noted, registered, counted, taxed, stamped, measured, numbered, assessed, licensed, authorized, admonished, prevented, forbidden, reformed, corrected, punished. It is, under pretext of public utility, and in the name of the general interest, to be place under contribution, drilled, fleeced, exploited, monopolized, extorted from, squeezed, hoaxed, robbed; then, at the slightest resistance, the first word of complaint, to be repressed, fined, vilified, harassed, hunted down, abused, clubbed, disarmed, bound, choked, imprisoned, judged, condemned, shot, deported, sacrificed, sold, betrayed; and to crown all, mocked, ridiculed, derided, outraged, dishonored. That is government; that is its justice; that is its morality."
― Pierre-Joseph Proudhon
 
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