Could you review my DMT extraction technique?

[blue.magic]

Here is my current extraction technique. I have marked is each step by white color and each question by yellow color.

Could you please help me resolve the questions and/or provide some notes based on your experience?

I know the technique is a bit overkill but my intent is not a quick extraction, rather to make a highly pure quality product for my beloved friends.

Here is the technique:

Prepare filtered water

Freeze/thaw soaked MHRB several times to pulverize
Is this necessary for powdered MHRB?

Adjust water pH to 4 using using medium-strength organic acid like phosphoric
Strong acids like hydrochloric may react with some of the plant material and create by-products, it is also more sensitive to dillution (pH will drop quicker). Do not use weak acid either as this may not pull enough alkaloids.
Is it true? Or the type of acid used does not really matter?

Soak MHRB in 1/3rd of the water heated to 55° C (131° F) for an hour
Cooking clogs MHRB making it un-filterable in later steps and even separation was impossible for me when cooking because it clogged the separatory funnel.
May long cooking (e.g. 6 hours) unclog MHRB again? I saw this in cacti but the cooking was very long, over 8 hours.

Filter MHRB using cloth filter, replace water

Repeat previous two steps two more times
Maybe one long cooking is better than three shorter soaks?

Defat with DCM
The reason I do defatting now is to avoid clogging when reducing the amount of water by cooking later. Another reason is that the DCM will have to be cooked away anyway.
Some people found that DCM removes more impurities than naphtha so I do at least two DCM pulls to remove polar impurities (the second pull is already pretty clear).

Reduce the water by cooking.
I found no clogging happens now (was the fats responsible?) - the cooking is mild and slow until I get more manageable amount of water, like half a litre or so.
The cooking also removes the dichlormethane (DCM).

Add zinc, let the water cool to room temp. for few hours while sttirring
Zinc converts DMT-n-oxide to DMT early on, so I don't have to convert it later, which would add unnecessary steps.
I found on this forum that 1-2 grams of zinc per litre is enough, other people say one should add 'excess' amount of zinc, never saying how much that is.
Should I add zinc at all? Should I add it later only if an oily residue appears?

Add 100ml lye water
Should I add just enough to get pH 12-12.5? Or should I add excess to 'break down' the plant material? However, there is not much plant material left at this point and I could not add lye earlies as the fats were present... Maybe the best order would be: add lye, defat, separate, cook, add zinc.

Decant through paper filter
I have a huge Buchner funnel and a vacuum bottle. I believe this step will remove any traces of plant material as well as the majority of zinc dust, undissolved lye and impurities in it. The filtrate will be also easier to work with.

Heat, pull with hot naphtha
I do several pulls (5-6) using small amounts of solvent naphtha in a separatory funnel. Slightly shaking each time.

Wash with sodium carbonate solution, filter
I voted for Washing Tek to clean up the naphtha of water-soluble impurities (e.g. lye!) before I put it in the freezer.
Sodium carbonate solution is slightly salted with NaCl.

Partly evaporate and cool the naphpta to room temp.
This saturates the solution improving freeze precipitation efficiency.

Freeze precipitate

Pour off naphtha, dry and scrape the crystals

Purify using heptane and activated charcoal
The reason for using heptane now is that it is more selective than naphtha. However, using it first would lower the yield. Just like it is better to use coarse sieve, then a fine one, I use naphtha first, then heptane.
I add a minimum amount of heptane, remove the colored oily layer - I found there is only a minuscule amount and it immediately sticks to the bottom of the beaker, so decanting is easy.
I follow this purification method, basically boiling the heptane with charcoal for a while, then filtering the charcoal.

Evaporate or recrystallize
Instead of freezing, the solution will is cooled slowly to obtain larger (i.e. purer) crystals.
My dream is to have a rotavap device to be able to evaporate and recycle the solvent, then scrape it or redissolve in tiny amount of hot eco-friendly solvent, then evaporate in pyrex dish, then scrape the pure white powder comfortably.

Maybe recrystallizing is better than evaporation because freebase crystals are more resistant to air (as air cannot enter into the crystals) then the powder?

Dry thoroughly
I would use a vacuum dessicator filled with silica gel. This should remove any traces of solvent, the DMT can dry peacefully in a vacuum, not attacked by oxygen and airborne impurities while drying.

Store
Transfer the DMT to a small vial (less air inside), close it tightly, wrap in a tin foil and store in a fridge or freezer.
And alternative may be to vacuum seal DMT in a foil if long term storage is intended, then put this in a bottle with a drying agent inside.

 

[syberdelic]

Is this necessary for powdered MHRB?

No, freezing is not necessary. It MIGHT speed up the process a little, but you stated that there is no rush.

Is it true? Or the type of acid used does not really matter?

I don't know the specifics, but there are some acids that work better than others. I have experience with HCl and acetic acid (vinegar). If you aren't in a hurry, I would recommend vinegar. It takes longer, but seems to have produced a cleaner product, is fairly easy to obtain, and is safe to work with. If you can get glacial acetic acid, you can use much less volume. I would recommend diluting to 25%. My last extraction used 5 gallons of 5% to extract from 1kg of MHRB.

May long cooking (e.g. 6 hours) unclog MHRB again? I saw this in cacti but the cooking was very long, over 8 hours.

If you aren't in a rush, there is no need to cook the MHRB. Heating it will only result in a slightly faster extraction into acidic solution and as you said, more difficult filtration. The stuff is hard enough to filter as is. The above scenario using vinegar was a 1 gallon soak for 3 days, repeated 4 more times for the 5 gallon total and then boiling it down to a reasonable volume.

Maybe one long cooking is better than three shorter soaks?

This is incorrect. One soak will never come close to full extraction from any plant material. With multiple soaks, you will pull successively less from the plant material with every soak, but say for instance that each soak pulls 50%. by soak #3, you will be at 87.5%. This is an under estimate, but with a single longer and heated soak in the same scenario, you would not get more than around 60%. In reality, the 3 soaks should pull at least 95% with a strong acid. Weaker acids like acetic or the phosphoric you mentioned will require longer soak times and more soaks.

Should I add zinc at all? Should I add it later only if an oily residue appears?

I don't have any experience using zinc, but I would assume that you would want to do this after evaporating the naphtha but before recrystalizing. If you mix the zinc with a base, I'm not sure how this would react.

Should I add just enough to get pH 12-12.5? Or should I add excess to 'break down' the plant material? However, there is not much plant material left at this point and I could not add lye earlies as the fats were present... Maybe the best order would be: add lye, defat, separate, cook, add zinc.

There is really no need to take the pH any higher than 12. I'm not sure exactly at what point it happens, but if you get the pH too high, it will tear apart the DMT molecules. I would recommend using sodium carbonate which can be made from baking soda. Put tin foil on a cookie sheet. Put a thin layer of baking soda on the foil (2-3mm). Bake at 400F for a few hours. You can test it by putting a tiny amount on your tongue. It should have a little bite to it, easily differentiated from baking soda. If you don't think it's quite there, simply place it back in the oven. This way, you can add solid sodium carbonate to solution which is a definite no-no with lye. You simply can't add too much. The pKa is high enough to freebase DMT, but not high enough to damage the molecule. The saturation pH for sodium carbonate is 11.37. I will slowly add it to my acidic solution to allow it time to neutralize the acid, keep adding until I reach around 11.3, and then add in a healthy amount more so that I'm certain that the pH will stay over 11 as it continues to react.

You want to do the defating while the solution is acidic. At this phase, the DMT salts are insoluble in non-polar solvents but the fats are very soluble. Many claim that this is unnecessary with MHRB, but I find that a single defating makes the subsequent steps like filtration easier and produces a cleaner product. My defating solvent of choice is xylene, but beware that almost all plastics will either dissolve or degrade with contact to xylene. Other non-polar solvents work, but I find xylene both readily available and a very effective defating solvent.

Maybe recrystallizing is better than evaporation because freebase crystals are more resistant to air (as air cannot enter into the crystals) then the powder?

This is true. I will usually get pure white and sometimes fairly large crystals with re-x. After pouring off the naphtha, while the residual naphtha is evaporating, the outside of the crystals will turn a little yellow and sometimes with a little orange hue. I assume that this is oxidation. After it's dry, I can crack a crystal in two and the inside is pure white, but if I leave it exposed long enough it will yellow a little as well.

The other benefit of re-x is that while DMT is mostly insoluble in sub 0C naphtha, most of the impurities that dissolve in naphtha or heptane, will stay soluble and are discarded when you pour off the cold solvent.

Good luck with your extraction!

 

[blue.magic]

Thanks for the elaborate answer. This is very helpful and I will apply your advice to my next extraction run.

No, freezing is not necessary. It MIGHT speed up the process a little, but you stated that there is no rush.

Okay. I will do a side-by-side experiment once to test how much the freezing helps.
Mine MHRB is powder-ish, a very well shredded dusty material, but still contains some root fibres.

This is incorrect. One soak will never come close to full extraction from any plant material.

I understand. I was weighting several scenarios:

- 1 long cook
- multiple short cookings
- multiple short (1-2 hour) hot soaks
- multiple short soaks, then two or so long soaks w/o heating

Based on your advice, I will try the last one. I guess the hot soaks will take most alkaloids out, then the longer soaks will get the 98-99th percentile.

I am drinking re-steeping loose leaf tea so I am intimately familiar with how the strength decreases with successive infusions

In reality, the 3 soaks should pull at least 95% with a strong acid. Weaker acids like acetic or the phosphoric you mentioned will require longer soak times and more soaks.

I have lab-grade phosphoric (85%) and hydrochloric (35%).

I don't like the hydrochloric of course for the caustic fumes and reactivity.

I like phosphoric for a couple of reasons:

- more viscous, reducing the risk of splashes
- not a weak acid, nor strong one - only few drops reduce pH very quickly, yet it does not ionize completely, no danger of reacting with plant material
- reduces soaking time (I am patient but not that patient )
- easy to obtain as pH- liquid for growers

Thanks for suggesting acetic, it's good to know it works for you.

The pKa is high enough to freebase DMT, but not high enough to damage the molecule. The saturation pH for sodium carbonate is 11.37.

Wonderful! This sounds too good to be true as I can finally avoid lye I was converting sodium bicarbonate in a frying pan earlier so I am familiar with it.

If you mix the zinc with a base, I'm not sure how this would react.

I agree - zincates may form, probably harmless but better safe than sorry. I would add more steps later than contaminating plant material with zinc.
Also I just realized the DMT N-oxide can be collected and then converted all at once rather than doing this for every extraction.
Finally, it is more eco-friendly as MHRB and zinc can disposed separately (compost MHRB, landfill/recycle zinc).

Aluminium should perform even better than zinc as a reducing agent, but I don't think it worths the health risks.

My defating solvent of choice is xylene, but beware that almost all plastics will either dissolve or degrade with contact to xylene.

I cannot work outdoors to get enough ventilation so I avoid xylene as a safety measure. I store the used DCM in a metal can with pressure seal (for later recycling perhaps).

...

I forgot mentioning the salting step, i.e. adding saline solution before basifying to improve ionic strength as described in Cyb's 'MAX ION' tek.

Okay back to work. Thanks for having patience with a newbie, will post my results later.

 

[syberdelic]

I find that adding salt (NaCl) is only necessary for resolving emulsions. I have had some extractions that require zero salt and some that require large amounts. I'm not exactly sure why this is, but assume there is some kind of surfactant in the plant material that varies. Salt will not allow more ions in solution, but rather make the solution more polar so that it separates from the non-polar easier after agitation.

 

[downwardsfromzero]

Maybe the best order would be: add lye, defat, separate, cook, add zinc.

Definitely not. You must defat the (cooked) acid solution, otherwise you are just pulling the actives, do you see? Then, while it's still acidic, you might as well chuck in the zinc. That's another place where you might want to split the extraction to compare results - one part with zinc, the other without. Next, add the salt if you're going to use it, then add base.

Or, just follow Cyb's Max Ion tek. No need to re-invent the wheel.

Also I just realized the DMT N-oxide can be collected and then converted all at once rather than doing this for every extraction.

That really depends on how many extractions you end up doing, and how much oxide there is in the plant material.