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Extracting DMT with ethanol, vinegar and sodium carbonate

Migrated topic.
some one said:
I'm reading positive results in the last posts. Which means this method has developed into a working tek.

Can someone write an executive summery?

So everyone wanting to learn the best way to achieve good results needn't need to go over 12 pages of experimentation.

:d
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This could be a wiki entry by now but i think maybe the details are still being worked through. However following a q21q21 path up to basing, then drying completely and pulling with 99%IPA or 190 proof ethanol is fairly foolproof to get the goods. I love changa made with this path.
 
Could you elaborate which details exactly?

For 100gr MHRB:

As per q21q21:
- add 100ml 5% vinegar
- add 100ml hot water
- add 75gr Calcium Hydroxide (can we also use Sodium Carbonate?)
- add small amounts of water to achieve a moist consistency
- dry in oven

As per this topic:
- pull with 190 proof ethanol (how many pulls?)
- evaporate ethanol (ready to smoke or clean up needed?)

If we use >95% Calcium Hydroxide (can't find 100% food grade), could there be some unknown residues which could dissolve in the ethanol and end up in the yield? If we use Sodium Carbonate converted from 100% food-grade baking soda (easy to buy), won't some Sodium Carbonate dissolve in the ethanol and contaminate the final yield making it harsh to smoke?

- Calcium Hydroxide 'Ca(OH)2' (lime) - poorly soluble in water, not soluble in ethanol
- Sodium Carbonate 'Na2CO3' (washing soda) - soluble in water, poorly soluble in ethanol
- Sodium Bicarbonate 'NaHCO3' (baking soda) - should be changed to sodium carbonate by heating

Also, is this applicable?

* When you add excess sodium carbonate to an aqueous solution of DMT acetate, you're left with freebase DMT, sodium acetate, water, CO2 and unreacted sodium carbonate.

* After drying, it's fb DMT, sodium acetate and sodium carbonate.

* The IPA pull leaves behind the unreacted sodium carbonate. But sodium acetate is soluble in IPA, so your IPA contains both DMT and sodium acetate; in fact, for each DMT molecule there is one molecule of sodium acetate. So only ~70% of your product is DMT.

To get rid of the sodium acetate, you'd have to wash your DMT with water, in which sodium acetate is very soluble (which fb DMT is not).
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Source: DMT acetate to freebase conversion with pics - Advanced/Enhanced chemistry - Welcome to the DMT-Nexus
 
(can we also use Sodium Carbonate?) Yes

(how many pulls?) One is enough for me

(ready to smoke or clean up needed?) Its possible to smoke but a clean up is prefered.
 
Eaglepath said:
(can we also use Sodium Carbonate?) Yes

(how many pulls?) One is enough for me

(ready to smoke or clean up needed?) Its possible to smoke but a clean up is prefered.
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I do 3 pulls. iPA is cheap.
This is an opinion but Ms. Wages pickling Lime works great and is eay to obtain. I dont believe it is soluable in IPA (if sombody knows if this is true chime in). My cleanup is simply re-dissolving in 99% IPAan letting anything that doesnt dissolve settle and decant carefully through cotton in a funnel.
 
skoobysnax said:
Ms. Wages pickling Lime works great and is eay to obtain. I dont believe it is soluable in IPA (if sombody knows if this is true chime in).
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Calcium hydroxide is practically insoluble in IPA (although come to think of it I've never actually checked). Calcium acetate, however, forms gelatinous material with IPA or ethanol - which actually retails as fire gel.
 
downwardsfromzero said:
skoobysnax said:
Ms. Wages pickling Lime works great and is eay to obtain. I dont believe it is soluable in IPA (if sombody knows if this is true chime in).
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Calcium hydroxide is practically insoluble in IPA (although come to think of it I've never actually checked). Calcium acetate, however, forms gelatinous material with IPA or ethanol - which actually retails as fire gel.
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:shock: pulls I have done with everclear needed a. Bit more cleanup. Definitely the drier the solvent the better. I love the way this spice smells btw. Definitely more floral.
 
Thanks, from the input given:

To extract 100g MHRB:
- add 100ml 5% vinegar
- add 100ml hot water
- add 75g Calcium Hydroxide OR: 100g Sodium Carbonate (1:1 ratio to bark)
- add small amounts of water to achieve a moist consistency
- dry in oven
- pull 1x with 190 proof ethanol OR: pull 3x with IPA
- evaporate
- clean yield by pulling with IPA to discard undissolved solids

Seems that you guys use (less than 100% pure lab grade) IPA to get rid of base residue.

When basing with Sodium Carbonate and pulling with 96% ethanol, an IPA clean-up seems needed as some Sodium Carbonate will dissolve in the 4% water from the 96% ethanol. But the IPA also dissolves Calcium acetate, making the IPA clean up not good after using vinegar. Could you use an other acid such as lemons (citric acid) instead of vinegar which doesn't leave anything dissolved in the IPA?

I can only find 99% lab grade IPA. Problem with evaporating non food-grade solvents is the accumulation of potentially harmful substances in the final yield. If you use 400ml 99% IPA to pull 1000mg DMT, the IPA contains 4000mg impurities (@1%). Say 2,5% of all 1% IPA impurities stay in the yield, that's 100 mg impurities per 1000mg DMT, around 10%. Maybe toxic to smoke? Of course you should always perform a IPA evap test. But maybe the DMT + plant oils trap some IPA impurities? Like trapped Naphtha in an oily yield. Doesn't lab grade IPA defeat the purpose of performing a food grade tek? If the goal is to stay as food grade as possible, I'd chose to pull the bark with food grade ethanol and only clean the yield with an as small as possible volume of IPA if needed.

Could you dehydrate 96% ethanol to 100% using Anhydrous MgSO4 (made from food grade Magnesium Sulfate Heptahydrate)? Or Sodium Sulphate or Calcium sulphate? To not pull any base into the ethanol, skipping the needed IPA clean-up? Or will the ethanol directly re-hydrate upon contact with air during evaporation? If so, could you perform a closed valve distillation just above ethanols boiling point, letting pressurized ethanol vapor escape, but no air going in, leaving DMT behind? You'd start with an evap test by adding and removing desiccant in ethanol without DMT to see that no desiccant is left after evaporation.

I would always do a evap tests when adding base products to solvents. For example I found >95% food grade Calcium Hydroxide. But what if some of the 5% impurities dissolve in ethanol /IPA? They might be food grade, but not be good for smoking.
 
Could you dehydrate 96% ethanol to 100% using Anhydrous MgSO4
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It's not terribly effective. Calcium oxide would be a better bet, and you can make this by roasting calcium carbonate (chalk) with an oxy-propane blowpipe. You'll need sunglasses for this as it gets very bright (the original limelight)! While it's possible to obtain food-grade calcium carbonate as precipitated chalk for use in brewing, the heating process is much easier to perform on larger lumps of material, namely natural stone.

There is a small possibility of toxic mineral contamination from this but distillation (in a dry atmosphere) of the resulting absolute ethanol will clean things up sufficiently. Horticultural limestone should be low enough in heavy metals for this to be a non-issue and chalk tends to be pretty pure on the whole. It's possible to perform a few fairly simple chemical tests on a sample of the calcium carbonate mineral intended for use to ascertain its heavy metal content.

Once one has prepared calcium oxide, it is very easy to convert it to calcium hydroxide for the base stage of the extraction as well - hence its utility as a drying agent. Adding water to calcium oxide is potentially somewhat hazardous (but also quite entertaining) so anyone attempting such activities should be fully cognizant of the risks and avail themselves of appropriate personal protection equipment.

I found >95% food grade Calcium Hydroxide. But what if some of the 5% impurities dissolve in ethanol /IPA? They might be food grade, but not be good for smoking.
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The impurities are most likely to be calcium carbonate and the corresponding magnesium compounds. You could always pre-wash your lime with your solvent of choice before use.
 
Thanks! I enjoyed reading through your answer how to make Calcium oxide and perform the other steps, but for me personally this is a bit too much effort. You say Anhydrous MgSO4 is not so efficient, what does this mean? I don't mind using more if that does the job. And would Sodium Sulphate or Calcium sulphate work to dehydrate ethanol?

Just to be clear, if I can get ethanol fully dehydrated neither any Calcium Hydroxide nor Sodium Carbonate will dissolve in it, correct? If so I could pull with 96% (or 100%) ethanol and perform an clean-up on the initial yield with 100% ethanol (instead of IPA). Discard any solids from the 100% ethanol and distillate dry. Will the FB survive ethanol dist. temp?

Then there is the Sodium Acetate issue. Will using Calcium Hydroxide as a base instead of Sodium Carbonate solve this? If I do choose Sodium Carbonate, will using lemon instead of vinegar solve this? Or will Sodium Citrate form and cause the same issue? If so, any other food product acid to use instead?
 
Even 96% ethanol will only dissolve tiny amounts of calcium hydroxide. The main impurities carried over will be calcium or sodium salts of the relevant organic acids. One can search for this data online although having access to a copy of the CRC handbook is helpful as well.

DMT freebase is stable at 78.5°C but you would need very careful temperature control once down to the last few mL of solution. The heat coming through the glassware might be sufficient to vaporise some of the product - and anyhow, how would you get it out of the distillation flask?

Lemon juice is not that great an option as an acidificant, pure food grade citric acid is generally very easy to obtain. Sodium or calcium fumarate might prove to be very poorly soluble in the alcohols in question, making fumaric acid a possible option - but you'd need to check the data for this.
 
Considering calcium acetate is soluble in those solvents we've been talking about here, and all that was related earlier in the thread, I think maybe the easiest way is indeed to use sodium carbonate as a base and then simply wash the final freebased product with water to remove sodium carbonate excess and sodium acetate, leaving DMT behind, similar to what is described in Amor Fati's approach. I haven't tried out the wash with water, the only danger I see is that suspended DMT gets carried off with water, so one should prob be gentle with the water wash and/or filter and keep what stays on top of the filter.

Thoughts? Anybody can experiment a bit with this and let us know how it goes?
 
Even 96% ethanol will only dissolve tiny amounts of calcium hydroxide.
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Good to know.

DMT freebase is stable at 78.5°C but you would need very careful temperature control once down to the last few mL of solution. The heat coming through the glassware might be sufficient to vaporise some of the product - and anyhow, how would you get it out of the distillation flask?
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Distillation is for ethanol preservation (it's expensive). I'd distillate over a double boiler with water heated to 80-85 C. Wait for 90% volume reduction. Pour the 10% remaining solution from the flask and evaporate dry at room temp on a plate. This way you'd only loose around 10-12% ethanol instead of 100%.

Lemon juice is not that great an option as an acidificant, pure food grade citric acid is generally very easy to obtain. Sodium or calcium fumarate might prove to be very poorly soluble in the alcohols in question, making fumaric acid a possible option - but you'd need to check the data for this.
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It would take effort for me to check the data from theory (I'm not a chemist). But I could check by experimentation without DMT. Create acid solution. Add base. Evaporate. Add solvent. Descant solids. Evaporate solution. Check if any solids remain. If nothing does then good to go. I have Citric and Fumaric acid laying around. Can test with IPA. Pulling with 96% ethanol would dissolve any salt in the 4% water so a dehydrated IPA or dehydrated ethanol wash is always required.

Considering calcium acetate is soluble in those solvents we've been talking about here, and all that was related earlier in the thread, I think maybe the easiest way is indeed to use sodium carbonate as a base and then simply wash the final freebased product with water to remove sodium carbonate excess and sodium acetate, leaving DMT behind, similar to what is described in Amor Fati's approach. I haven't tried out the wash with water, the only danger I see is that suspended DMT gets carried off with water, so one should prob be gentle with the water wash and/or filter and keep what stays on top of the filter.
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I've done a water clean-up ones after converting DMT-fumerate to freebase with Sodium Carbonate in water. Evaporated the water and washes DMT with fresh water to get rid of base residue. Personally i found it a bit messy and suspected yield loss. But I guess if you get skilled at it one could do a better job than I did.

In my opinion it would be easiest to choose an (food grade type) acid which does not create an ethanol and IPA soluble salt.
Or could we even leave the acid stage out and go STB? With some more initial water and 1-2 days of waiting.
 
The first part of the extraction can def be done without an acid, just base the plant material and pull, but then if one would want to clean up, then an acid would be necessary to redissolve, filter, re-evap and basify. Many things could be tried, like vitamin c, citric acid (or maybe even just lemon).

A lot to test still :)
 
endlessness said:
... but then if one would want to clean up, then an acid would be necessary to redissolve, filter, re-evap and basify.
A lot to test still :)
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I use following sequence of steps for the final cleanup of my acidic saltings from toluene pulls. I think it could be used also in the type of extraction describe here, tried it once this way and it works:

Redissolve in acidic water (I use acidic saltings directly)
Basify
Filter out solids
Wash solids with water
Dissolve in IPA
Evaporate
Wash residue with water
 
Redissolve in acidic water (I use acidic saltings directly)
Basify
Filter out solids
Wash solids with water
Dissolve in IPA
Evaporate
Wash residue with water
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Glad to hear this worked. Two water washes. No yield loss? I personally don't like washing DMT with water, but that's just me.

The first part of the extraction can def be done without an acid, just base the plant material and pull, but then if one would want to clean up, then an acid would be necessary to redissolve, filter, re-evap and basify. Many things could be tried, like vitamin c, citric acid (or maybe even just lemon).
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Good to know STB can be used. The acid part of the clean-up extraction employs the insolubility of various matter in an acidic solution. The clean-up works by filtering out this matter, correct? If so then in theory we could dissolve the dirty yield in carbonated water, filter and discard the solids, evap solution to obtain clean freebase DMT. No basing and pulling required.

procedure:
- mix MHRB with excess sodium carbonate, add water to make a paste, spread it in a wide dish and let it dry
- 1-3x pulls with ethanol, filter the pulls, evaporate the ethanol
- redissolve dirty yield in carbonated water, filter and discard the solids
- evaporate the carbonated water solution to obtain clean freebase DMT

The only thing to make sure of is that no base from the first STB extraction dissolves in the pulling solvent. Using 96% ethanol and sodium carbonate, some base will dissolve in the solvent and stay in the yield. Then re-dissolve in the carbonated water and stay in the cleaned yield also. Downwardsfromzero mentions that hardly any calcium hydroxide dissolves in 96% ethanol, so food grade calcium hydroxide would be better. With Sodium Carbonate either 99.9% IPA or dehydrated ethanol should be used. Endlessness what's your take on using Anhydrous MgSO4, Sodium Sulphate or Calcium sulphate to dehydrate ethanol? Or will freezing the ethanol solution low enough precipitate out all Sodium Carbonate?

If this works we'd only need:
- baking soda (converted to sodium carbonate by heat in the oven)
- 96% alcohol
- sparkling water

All food grade 8)
 
Maybe some loss occurs from water washes, but is very small. When you wash with water (especially first time), there are still some residue of base within dmt fb and in filter itself and washing water becomes slightly basic from it. And of course, you should use very small volume of cold water for both washes to minimize losses.
 
some one said:
Nice one. Tiny water amounts is the key. Alright :)
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The only caveat is that my extactions seems more oily than crystalline. Are the amount of impurities really a problem? I haven't experienced any ill effects from the Changa made from this method. Might be a nice path for pharma
 
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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