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Lex Coshi's DMT extraction v1 up for review

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Fable - I believe that we want to use a NP solvent that is selective for dmt, that's the whole point with an extraction such as this. Naphtha is chosen because at room temp it dissolves lots of dmt but way less at 0 deg C. Di-ethyl-ether and dichloromethane are other solvents used that are selective to dmt. But to see what else comes out I've wanted to try toluene instead of naphtha when basifying - would you get mixed 'red' spice with dmt + jungle-spice alkaloids..? A acid-base extraction will yeild 0.7 - 1.0% dmt depending of root bark quality. And, as far as leaving any dmt behind, just do a third and fourth pull with the NP-solvent, and evaporate all the naphtha from each pull to see if anything still comes out. You do get ALL the dmt out of the root by simply soaking the ground MHRB in Acid ovenight, and in 2 soaks there will be none left to get out of the bark. And when you basify the dmt will be 'running' for shelter in the naphtha - none will 'want' to stay in pH 11.5. SWIM finds that with using ratio of a 1-part-naphtha to 5-parts-basified-extract ( eg 100ml naphtha on 500 ml pH 11.5 extract), 100% of the dmt present comes out. Although there must be a limit to the solubility of dmt in naphtha, I'd say the chemical process is always working in our favour - "pulling" makes it seem like the dmt molecules are 'resisting' the NP-solvent, but at pH 11.5 they are more like 'pushing' their way into the naphtha. At room temp, taking note of the yeild in each NP-solvent-pull, SWIM gets no dmt from the third pull, it's all out in 2 pulls ! And her total yeild is usually 0.7 - 0.9% of the weight of MHRB used. And look what I found while trying to Google "dmt-solubility" ! http://lightsource.atwiki.com/page/molecules
 
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I understand the chemistry behind the extraction process and I do advocate the A/B extraction method as well as using the pKa to find the best pH to extract at without torturing the spice, it is more the solubility in shellite that is bothering me. I had an accident in the lab and left some spice heating on a large watch glass on a modified coffee mug heater, The watch glass cracked in half while I was off drinking a cup of tea and I had to recoup the spice off the broken glass. Room temperature shellite would not budge it, acetone dissolved it so quickly I almost missed what was happening. This lead me to think that if the solubility is low, how much is being left behind on the first pull? (I do my extractions hot to help drive the spice to the organic phase and I use leather gloves to hold the sep funnel) If I was to use toluene or xylene and get 95% of the spice in the organic phase at the first pull I would be happy to work on that and not worry about the 5% left behind. I am concerned that to get 95% across into shellite that I will need twice as much and that it will take 4 times as long to migrate to the organic phase. If I could be convinced that 95% of the spice was to migrate into the organic shellite phase then I wouldn't be concerned. I just think that a better yield could be obtained by using toluene then purifying the jungle spice, rather than running 2 to 3 extractions and combining the organic portions of shellite. I guess my concerns arise because I do not have access to high yielding material and I need to bulk up to say500g or 1lb to start with. Obviously this needs a lot of acidified water to add to it, and even after boiling down my 2liter sep funnel is starting to feel too small.
 
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Conshi - you mention to basify to "pH 14", right in the beginning of the .pdf article... Did you really mean this high of a pH (end-of-scale) instead of good ol' 11.5..? And please, since I may be making-it-up all wrong, let's all compare notes on "over acidifying" - from swim's experiences I have the impression that it is not a problem to acidify to pH = 1.8 What can happen with too much acid..? The H+ component of excess acid stays in solution, and enforces the dmt molecules to stay charged - it will not threaten the dmt molecule like excess OH- does at pH > 13.5. The excess salt (acetate or Cl-) could be an issue but it stays behind after the basifying and non-polar extraction.... So I liberally acidify, targetting pH = 2.0, soak overnight and use NO heat Swim uses strong acid-soaks (8 - 10 hrs at pH 1.8 - 2.2) to extract the dmt from ground MHRB, believeing that the acidity will breakdown cellulose and lignin in the wood of the bark, helping to further release dmt into solution. So a pH 2.0 works like the lye-stew pH of 13.5 - it digests the (powdered) MHRB And speaking of how much naphtha does it take to 'pull' all the dmt out of the basified aqueous, swim just noted NO dmt remained in the MHRB after 3 pulls with 100 ml NP-solvent to 500 ml basified sol'n. The fourth pull was empty. Swim has checked before and found < 1% of the yeild came out in the third pull with naphtha. So it seems that if you give it time and actively 'swill' and 'tumble' the naphtha layer for 30 minutes ( using 1:5 ratio NP:aqueous), let emulsions settle out ( 1 - 8 hours), then repeat just once, you'll get > 95% of the dmt that's in the basified aqueous layer. The third pull could be empty... From these very recent experinces, swim feels that this is a fairly reduced volume of NP solvent needed. Total naphtha used was 1.2 liters to get a 0.7% yeild of dmt from 200g MHRB - She could have stuck with just two NP-solvent pulls, reducing the NP volmue needed to 0.8 litres. She only did two acid soaks, and noted that nothing remained in the MHRB to be extracted during a third acid soak.
 
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good points there fable yeah for some reason acetone (and IPA, and ethanol and methanol apparently) dissolve dmt sooo easily, and shellite does indeed need some help. I find the key to a successful extraction is heat, room temp shellite doesn't do shit, people leaving their extractions to sit overnight so the lye can do its thing then pull the next day .. wonder why they didn't get anything? the shit needs to be HOT, i always make all liquids real hot first, then basify, then add shellite and etc... reheating is usually necessary (i usually do this by adding more lye but considering what El bong says perhaps a hot water bath or flameless stove would be a better option). but yeah, HOT, and the dmt goes in there happy El Ka Bong, i'll get trough your's one by one - i did mean pH 14, yes.. the reason i went so high is i've heard from numerous (reputable) extractors that dmt can easily survive lengthy high pH baths, and a well known major reason for failure (or poor results) is underbasification. Like mescaline (which is apparently bulletproof), dmt can apparently handle high and low pH situations with ease. Do you suspect otherwise? - noted your acidifying comment, i was thinking myself to change the ratio from 3:1 of water:vinegar to 2:1, this would have the pH around three (to lower the ratio again might end up getting a little expensive.. actaully, i think vinegar is cheaper than distilled water).. what the pH of 5% acetic acid? ie vinegar? i guess you could just use straight vinegar the whole way through.. - i tend to simmer the bark + acidic water for around 1-2 hours thinking that that would accelerate the process of dmt-out-of-bark and in-to-water - the excess naptha, i guess it depents on your technique, but adding 100mL to those 5L HDPE jugs in the tek.. the 100mL sits on the basified water but because of the large surface area it's very very hard to pull off using a baster or whatever. if you were using a sep funnel then it's probably ok, but again this is a spend an extra $1 for (better) guaranteed success. but using 250 250 and 500 on the last your almost certain not to leave any behind (by the last pull, anything not already recovered will be so diluted in that 500, again leaving a little behind is little to no concern)
 
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also, if someone was following this tek with 2000g of pre-powdered MHRB, would step 2, require anything different. Just trying to think ahead how this is gonna work If using pre-powdered would the liquid poured off the first cook leave anything behind, or would it all be liquid, if so what would the next 2 water/vinegar mixes be added to? Or would nomans tek be more suited to pre-powdered mhrb? SWIM said he plans to try this tek on a small scale first. but would still like to hear from anyone who has done this tek with pre-powdered mhrb before he starts. SWIM is starting to think fuelite might not be that good for extraction but he has found something with 50% hexane and the remaining in hexane isomers? which may be better he hopes.
 
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like i said before, heat is the key to getting the dmt into the solution. even if you let it sit overnight it should be fine, but just make sure that when you put the solvent in first everything is HOT 😉 Tek is fine for 2kg of MHRB. Perhaps though for the acid stages use a 1:1 ratio of water:vinegar rather than 3:1 (this will be added to the finalised tek) Pre-powdered means just that. Your bark is not (and never will be) soluble in the liquid for the acid cook so you most definitely will have a bunch of bark powder floating around in there. Just make sure that when you do your cook you let it sit for about three hours before pouring off; this will let the majority of the bark settle back down to the bottom so you are only pouring off liquid (and later you will still want to filter more via muslin cloth) Perhaps do half Coschi style and half Noman style and see which product you prefer? :D Fuelite should be ok, but perhaps just double the amount just to be sure (a waste of solvent, but more spice will be recovered)
 
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[quote:8bfd17f852="DVSnz"]Or would nomans tek be more suited to pre-powdered mhrb?[/quote:8bfd17f852] If your friend uses that tek for pre powdered bark he may have to add up to 50% more water to keep the solution from turning to unextractable mud. It'll work, just make sure there's room in the container and dont add any naptha if the solution is thick and sludgy.
 
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[quote:07dd444a95="Coschi"] Perhaps do half Coschi style and half Noman style and see which product you prefer? :D[/quote:07dd444a95] Thats what SWIM is currently planning :p
 
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[quote:8b662245a9="Noman"][quote:8b662245a9="DVSnz"]Or would nomans tek be more suited to pre-powdered mhrb?[/quote:8b662245a9] If your friend uses that tek for pre powdered bark he may have to add up to 50% more water to keep the solution from turning to unextractable mud. It'll work, just make sure there's room in the container and dont add any naptha if the solution is thick and sludgy.[/quote:8b662245a9] and 50% more lye also?
 
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you could get away with using less of everything yeah. The main thing is the initial acid cooks you want enough acidified water to cover your powdered bark and leave it some room to move around. Stick with the three cooks and etc.. some changes though: *use HCl to acidify your distilled water to pH 4 for your acid cooks (and don't let it boil, just enough heat so that a little steam rises from the mixture) *only basify to pH 12 you can still reduce your combined initial acid cooks but do it slowly, and depending on the extraction vessel your working with you can decide how much solvent to use for pulling, but you could use as little as 100mL/pull
 
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Coschi, why those changes? I know the tek is set up for larger amounts, which is pretty awesome indeed as swim's next venture will be of a slightly larger scale, and will be giving Lextek a good hardy go. (Looking forward to it 8) ) The boiling down is EXACTLY what he needed, as multiple vessels containing basified slurry is not what he has in mind. Also, this dude I know would like to introduce himself to the court of enlightened, as a "newbie" in your realms. Hello! (Has studied much and had great success on first go, while learning much in the process. HEAT IT UP!!!) Couple questions aside from the first, just to solidify knowledge: 1) Any loss due to simmering the acetate? Does anything "ride" the steam? 2) I forgot. PS- Thanks Noman- You are wise with the ways of spice. Your tek speaks volumes in its simplicity and product. After checking many teks and tidbits of info, yours seemed to combine everything that works, and for a newbie it is the shit. I really like the fact this is a rather "organic" science, where exactness doesn't need to be met. Although in the future swim really wants a good scale and thermometer. And PH meter. Just for kicks. QT- Day 61.... hahahaha!!!!
 
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Someone made fair point of the possibility that dmt.acetate is a lot less stable than dmt.hcl (acetate salts in general in fact), and during boiling down the dmt.acetate getting more and more surrounded by unused acetate ions can result in dmt.acetate being broken down. Apparently dmt.hcl doesn't encounter this problem as severly Also extra high/low pH, seems unnecessary, and a little disrespectful to subject such a precious molecule to such extreme conditions
 
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Hello,

since swim bought some Mimosa Hostillis in Brazil. swim itends to realize his first spice extraction from the mimosa hostillis. After reading various technics he decided that Lex`s Tek (V. 1.0) is most suitable and understandable for him. So far he is very happy about the tek and he`s looking forward to feel the result. Anyway there are 2 Questions about this Tek:

In part 6: "Defeat Step 2: Basify" Lex`s says

That the solution of acidic water & DMT acetat has to be basified with Sodium Hydroxid until the solution reaches a pH of 14!

In part 7 "Final Shellite Extraction" Lex`s says:

"We will now extract the DMT base from the basified solution with Shellite.
As previously explained, adding Sodium Hydroxide (base) to the acidic water + DMT Acetate
solution converted the DMT Acetate salt to the DMT Base which is insoluble in our polar solvent
(water) and soluble in our non-polar solvent (Shellite)."

in the following explanations of part 7 Lex`s says:

"1. Measure 250mL of Shellite
and add it to the acidic water.
Heat the mixture in a hot
water bath and shake."

At this point swim asks, why to put shellite in acidic water? In Part 6 he orders to put Sodium Hydroxide into the acidic - DMT Acetat solution, to become basified. So, after swim`s understanding there is no more acidic solution, because it`s basified. For swim it seems that it`s just a writing error and he might mean; the Shellite has to be added to the basified solution?


The 2nd question would be: After putting the Shellite into the basified solution and it`s seperated. Were swim has to expect the non-Polar Shellite Layer? Regarding to the instrcutions before, swim would expect the top layer ??? It`s not mentioned exactly..

thanks
 
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Something is out of order.>!?

Setp 6 - I think it means one "basifies" the acidic extract... you flip the pH so dmt is no longer soluble. This should be later than the 'step 6', huh..?!`

Step 7 is a de-fatting - skip that if you have MHRB. Only green plant stuff needs to be defatted (ie acacia bark, P. viridis leaves etc). This comes before basifying, and certainly does not need heat ..!?


I alwys wonder - what's all the facination for heating things..?! Maybe some of us are in a hurry ..!?

Heat helps with the acid-soaking as it speeds things up but what for..!? Giving the acid-extraction more time to occur at room temp achieves exactly the same result - 99.9% of dmt is out and soluble in 2 acid-soaks of 8 - 12 hours each, a pH 2. AND you solubilize the other alklaloids too - red jungle spices are destroyed by heat, they say ...

Heating a basified extract is aboslutely counter-productive ! Guaranteed you'll get more contaminants in the naphtha if you heat it to reduce emulsions or for whatever 'reason' ! It makes no sense to add heat to a lye-stew tek, imo ...


And hey ! what does this mean for Jeebus sake >!?

"The solution of acidic water & DMT acetat has to be basified with Sodium Hydroxid until the solution reaches a pH of 14."


... Are you sure you don't mean a pH of "15" ... ~? 😉

A lye-solution you add in 10 ml squirts might have a pH of "14", but that's the concentrated stock-solution of lye, ... not the extract.


Hey everybody ... ! what pH should turn the purple acid extract into a jet-black colour..? NOT 14 - that is ridiculous, 1000 times overkill ! Not 10 ... but ... anyone know..!?

The slippy, jet-black colour is when you STOP adding base - you've basified enough and the pH will be between 11 and 11.5.

If intending to do a big batch tek, why not use concentrated mineral acids like HCl instead..? You will have lower volums and give it just 8 hours at room temp and you don't need to make the mess cooking it
 
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" I think it means one "basifies" the acidic extract... you flip the pH so dmt is no longer soluble. This should be later than the 'step 6', huh..?!`"

"Step 7 is a de-fatting - skip that if you have MHRB. Only green plant stuff needs to be defatted (ie acacia bark, P. viridis leaves etc). This comes before basifying, and certainly does not need heat ..!?"

Part 6 is about defating / flipping pH.
Part 7 is about the final extraction


Part 6: Defat Step 2: Basify
Once again, in preparation to extract the DMT from the acidic water solution, we are going to
basify the liquid.
This will again convert the water-soluble DMT Acetate salt into the water-insoluble DMT base.
Note that no plant gunk exists in the vinegar solution; the solution at this point consists only of
acidic water + DMT Acetate.
1. Slowly add 60 grams of
Sodium Hydroxide to the
solution to raise the pH to 14.
Use a digital pH meter or
litmus paper to determine the
pH of the solution.
Note that the solution has
been placed into a new
vessel.



But anyway SWIM question related to part 7 (Final Extraction)

Part 7: Final Shellite Extraction
We will now extract the DMT base from the basified solution with Shellite.
As previously explained, adding Sodium Hydroxide (base) to the acidic water + DMT Acetate
solution converted the DMT Acetate salt to the DMT Base which is insoluble in our polar solvent
(water) and soluble in our non-polar solvent (Shellite).
1. Measure 250mL of Shellite
and add it to the acidic water.
Heat the mixture in a hot
water bath and shake.
2. Allow the layers to separate
and siphon and separate,
keeping the non-polar layer
this time.
Repeat step 1 two more times
and combine the Shellite
extractions.
Again, for the third pull add
another 30 grams of Sodium
Hydroxide (to reheat) and
extract with 500mL of Shellite.

SWIM asked why he advised; to put the Shellite into accidic water, it makes no sense in relation to the procedure in part 6 (were acidic solution is basified) so from this point off, i´m telling me, the shellite has to be dropped into the basified solution with spice-base, so that the spice can go into a medium where it`s soluble --> Shellite. The other thing is were can swim expect the non-polar layer (shellite) when it`s seperated, on the bottom or top ?
 
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Yes you got it right, but SWIM adds shellite to acidified extract FIRST, just before basfying. That way the moment the pH jumps up, the dmt has a 'safe refuge' ... Don't mix and heat the acid+shellite, let them be separate layers then add lye. Just swill it once the squits of lye-solution are added to change colour to black.
 
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Well, in the Tek it self (and also in Thread "DMT Extraction Overview - 2. Nonpolar Extraction of Freebase" DMT Extraction Overview - FAQ - All your basic questions and answers - Welcome to the DMT-Nexus) it is mentioned to add FIRST, the lye into the acidic solution to basify and then add Shellite to the Lye Solution, heat it in a water-bath, shake and then wait until it seperates. Where is exactly the advantage of your tek (adding Shellite into the aciddic solution, before adding lye) ? You said that the Spice has a "safe refuge" but what is happening if it don`t has? I mean the spice just becomes a freebase by adding lye, so it should stay save in the Solution anyway, until the Shellite is added and it can move into it!

Is it just a point of avoiding artificial heating? I do expect that both ways are working, but I´m not certain, if they are, because of missing experience. So, what is the precise advantage of adding Shellite before adding Lye to basify, does the spice go more easily into the Shellite, or what is this about ?!


Thank you !
 
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