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A/B extraction with D-limonene?

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awalmartbag

awalmartbag

Rising Star
Hey everyone

I'd like to try classic A/B Lextek for my first extraction attempt, using limonene instead of naphtha as a NPS, so I don't have to worry as much about contaminants if I screw up.
Will this work? Limonene's vapor pressure is a lot lower than naphtha's (0.01 atm @ 50C). Will limonene residue after freeze precipitation evaporate on a reasonable timescale? To what temperature can I heat freebase DMT without risking it decomposing or evaporating (Wikipedia isn't clear on it) to speed this along? Is freeze precipitation even feasible with limonene?

The limonene idea comes from Amor fati's Nontoxic tek. The reason I'm not just following that is that it's more complicated and gives the salt, not freebase, as a final product.

Many thanks in advance
 
BioBoostedSpirit said:
Hey there!!!

I might be wrong but I think you can't freeze precipitate with d limonene. Some folks were talking about it..


Best regards
Click to expand...

That's too bad. Thank you for the info though. Do you think I can heat the limonene to evaporate it instead, leaving the DMT behind?
I found two very different boiling points for DMT: 80C (pubchem - seems unrealistically low) and 305C (chemsrc.com - more what you'd expect). Limonene's is <200C, so this seems like it should be doable. I don't know to what degree making a limonene/DMT solution affects these properties though...
 
Limonene is unsuitable for freeze precipitation. Rather than evaporating, pull the alkaloid into acidified water (e.g. 1% white vinegar), evaporate, mix resin with moist sodium carbonate, dry then pull with acetone or isopropanol. Evaporate to recover active goo.
 
downwardsfromzero said:
Limonene is unsuitable for freeze precipitation. Rather than evaporating, pull the alkaloid into acidified water (e.g. 1% white vinegar), evaporate, mix resin with moist sodium carbonate, dry then pull with acetone or isopropanol. Evaporate to recover active goo.
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What if I pull it into acidified water, discard NPS, then basify the water so the DMT becomes insoluble freebase - will it precipitate out? Then filter and wash to get rid of any clinging acetate/hydroxide/sodium.
 
awalmartbag said:
What if I pull it into acidified water, discard NPS, then basify the water so the DMT becomes insoluble freebase - will it precipitate out? Then filter and wash to get rid of any clinging acetate/hydroxide/sodium.
Click to expand...
I doubt you could precipitate DMT freebase from water. But someone else would be a better authority.
Edit: Ignore this!

What I know you can do is a vinegar, lime, limonene, vinegar, lime, heptane, freeze precipitate process. I've done it before and it works fine. The only non-food safe step is the heptane, but you only use a small volume and it evaporates clean. If you are being super careful you can do a final cleanup step with ethanol to ensure no heptane is caught in the DMT xtals.

Check out Q21Q1's vinegar/lime tek. Once you get the DMT acetate jimjam, you base with lime, pull with heptane, then freeze. If you want to go this route I will give you more details on going from DMT acetate jimjam to DMT freebase xtals. This is what I did to convert my acetate jimjam to freebase. It was worth the effort.

Of course it is easier to skip the limonene, vinegar, lime, heptane process and just pull directly with heptane. 8)
 
shroombee said:
awalmartbag said:
What if I pull it into acidified water, discard NPS, then basify the water so the DMT becomes insoluble freebase - will it precipitate out? Then filter and wash to get rid of any clinging acetate/hydroxide/sodium.
Click to expand...

I doubt you could precipitate DMT freebase from water. But someone else would be a better authority.
Click to expand...

Yes, DMT fb precipitates from water very well, you just need to filter it out and wash with fresh water.
Just do not use too much water for pulls from NPS and also dry NPS before pulling with acidic water.
 
doubledog said:
Yes, DMT fb precipitates from water very well, you just need to filter it out and wash with fresh water.
Just do not use too much water for pulls from NPS and also dry NPS before pulling with acidic water.
Click to expand...
So would this work:

- Dry limonene. Using magnesium sulfate? Calcium chloride?
- Pull with vinegar, keeping volume low relative to NPS. 25 ml vinegar to 300 ml limonene? Do we need multiple pulls?
- Add lime. 2 grams?
- DMT freebase should precipitate?
- Filter through a coffee filter and wash with fresh water;
- Evaporate and scrape DMT from coffee filter;
 
I never use limonene, as I prefer xylene or toluene, but CaCl would be probably good drying agent for limo. For toluene, NaOH is fine.

Then pull using titration to weak acidic to avoid excess acid or just pull with diluted vinegar, keep volume low (ratio 25ml to 300 ml of solvent is ok).

Multiple pulls are not needed, but really good mixing of both liquid phases is a must (limonene seems to be quite difficult to mix with water properly).

Add base (you need something soluble in water, something like KOH, do not know whether lime is ok for this step).

Dmt fb precipitates in form of nice white crystals. Actually it is precipitate, not crystalized material, but it looks great :)

I think it's good to store it for a while in fridge, then filter it.
Funnel with cotton ball in the neck is good, coffee filter should be also fine.
Wash collected product with little bit of cold fresh water while it is still in the filter.
 
Thanks a ton to both of you. I'll give this method a shot as soon as my wrist heals, and maybe do some experimentation with different solvents.

One thing I don't understand: why are we drying the NPS if we're adding water in the next step? If there are pockets of water in NPS that will keep the DMT trapped, won't they just reform when vinegar is added and the solution agitated?

shroombee, I'll try the vinegar/lime tek you linked too and see how the final products compare. My reason for not using heptane in every NPS step is that it costs 10x as much as limonene - and that's just lab grade, not even food!
 
Water in NPS could contain some base from initial alkaline soup. This base will be salted out to acidic water as a salt (depends on the base and acid used, in case of NaOH and vinegar it would be sodium acetate).
This means impurity.
Very important rule in extractions is to not allow unwanted stuff to transfer to another step, if possible.
Probably not a big issue when dmt fb is precipitated from acidic water (assuming this impurity will not precipitate), but needed in case of mescaline extraction.
 
doubledog said:
Then pull using titration to weak acidic to avoid excess acid or just pull with diluted vinegar
Click to expand...
Meaning titrate to pH 6.5 or pull with 1% acetic acid?

doubledog said:
Add base (you need something soluble in water, something like KOH, do not know whether lime is ok for this step).
Click to expand...
I used lime to base DMT acetate jimjam before pulling with heptane. The jimjam came from the q21q21 tek where I salted limonene with vinegar and then reduced the vinegar to 5 ml of dark red tincture. The lime worked well for pulling with heptane. We'll see whether it would work for precipitating DMT freebase.

awalmartbag said:
shroombee, I'll try the vinegar/lime tek you linked too and see how the final products compare. My reason for not using heptane in every NPS step is that it costs 10x as much as limonene - and that's just lab grade, not even food!
Click to expand...
Wow - my ACS heptane and food grade limonene are about the same price, around $65 USD.

Note the vinegar/lime tek yields full spectrum DMT acetate jimjam which is sort of harsh to smoke and apparently not highly regarded. And I've read that acetate vaporization by-products are not healthy. But I originally tried this tek because it appeared easy and is food safe for my first DMT extraction. Going forward I would pull directly with heptane (not limonene) or maybe try precipitating going from limonene/weak acid.

BTW, please review this and edit your post. Pending deliveries of dried plant material is included in the category of "no discussion". Thanks! :)
 
shroombee said:
doubledog said:
Then pull using titration to weak acidic to avoid excess acid or just pull with diluted vinegar
Click to expand...
Meaning titrate to pH 6.5 or pull with 1% acetic acid?
Click to expand...
Does not really matter, it will be based anyway, so pull with diluted vinegar (1-2%) is totally fine, water just need to be acidic after salting out to be sure dmt is in there.
 
Sorry about that! Post edited.

In that case, I better skip the jimjam and try to get pure DMT by precipitation. Thanks for letting me know about the acetate.

I don't think we have to worry too much about drying NPS. Sodium/potassium/calcium acetate are all quite water-soluble, so they should not precipitate along with the DMT.
 
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