Apochrahyll
Rising Star
- Merits
- 42
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- Thread starter Apochrahyll
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DCM is a great solvent for DMT extraction, so long as you follow the appropriate safety procedures. That being said, I see a few issues with your method:
1) You're trying to do a dry tek, when you should be doing a wet tek. The DCM won't grab many goodies out of your bark if you've only minimally basified it, especially since it would be way more efficient to have liquid to liquid extraction.
2) I would switch in NaOH as the base (forget the sodium carbonate). The ethanol in Endlessness' tek is semi-polar, don't forget. However, DCM is very very non-polar, so you need to make sure your DMT is completely freebased in order for it to be pulled in any great quantity in the DCM.
3) If you have the proper glassware and a condenser, you could do a reflux with the DCM and basified bark soup for 15min, then let it cool to room temp and pull the DCM.
Also, remember that you'd be hard pressed to get anything out of 10g of bark. Think of the terrible efficiency of using such a small amount, plus the fact that there'd only be like 100mg, if that, of potential goodies to be had. I think if you use NaOH with DCM and do either a STB or A/B tek instead of a dry tek, you should be fine.
EDIT: I just reread your OP. You never checked pH! There's your problem, you didn't measure the pH. Also, why would you salt it back into vinegar? DCM evaps so easily. I feel bad to say this, but you need to do more research. It sounds like you sort of just bought some chems and started playing around.
1) You're trying to do a dry tek, when you should be doing a wet tek. The DCM won't grab many goodies out of your bark if you've only minimally basified it, especially since it would be way more efficient to have liquid to liquid extraction.
2) I would switch in NaOH as the base (forget the sodium carbonate). The ethanol in Endlessness' tek is semi-polar, don't forget. However, DCM is very very non-polar, so you need to make sure your DMT is completely freebased in order for it to be pulled in any great quantity in the DCM.
3) If you have the proper glassware and a condenser, you could do a reflux with the DCM and basified bark soup for 15min, then let it cool to room temp and pull the DCM.
Also, remember that you'd be hard pressed to get anything out of 10g of bark. Think of the terrible efficiency of using such a small amount, plus the fact that there'd only be like 100mg, if that, of potential goodies to be had. I think if you use NaOH with DCM and do either a STB or A/B tek instead of a dry tek, you should be fine.
EDIT: I just reread your OP. You never checked pH! There's your problem, you didn't measure the pH. Also, why would you salt it back into vinegar? DCM evaps so easily. I feel bad to say this, but you need to do more research. It sounds like you sort of just bought some chems and started playing around.
Well, it's not so much that DCM can't ever be used in a dry tek. Rather, you want the DCM to encounter as much DMT as possible, so that the DMT can dissolve into the solvent. However, with the q21 tek, the DMT is almost completely inaccessible to the DCM. This is because the bark, as you said, needs to undergo some amount of cell lysis to release the alkaloids. Also, liquid to liquid extraction is many times more efficient than a dry tek, because liquids' molecules are more energetic and free to move about and interact, while a paste is not. Think of trying to dissolve solid salt in water versus mixing saline solution and water. Which takes longer to become homogeneous? Also, the sodium carbonate is really not a suitable base to use with DCM, because it doesn't freebase enough DMT to be pulled by the very non-polar DCM. You want to use NaOH with DCM, to split open the cells so that the alkaloids are available and to sufficiently freebase all of the DMT.
As for the backsalting, you'd still have to convert to freebase anyway, which would just add an unnecessary step in which you might lose yield. If I were you, I would just get some NaOH (lye) and do Earthwalker's Tek but with DCM in place of naphtha. But when you do, be sure to measure pH! A pinch of this and a pinch of that doesn't work in chemistry.
As for the backsalting, you'd still have to convert to freebase anyway, which would just add an unnecessary step in which you might lose yield. If I were you, I would just get some NaOH (lye) and do Earthwalker's Tek but with DCM in place of naphtha. But when you do, be sure to measure pH! A pinch of this and a pinch of that doesn't work in chemistry.
One would hope, although the bark may be weak so you never know. I think the reason you didn't get anything is because none of the DMT was freebased, or at least not enough to be significant. 10g of bark is very little to begin with, so when you don't properly base the alkaloids you're not going to get much of anything at all. Also, don't forget economies of scale. 100g is way more efficient than 10g, because you lose an amount of DMT in the extraction and cleaning up processes that is probably about equal to your entire yield with 10g. So, with such a small amount of bark, you probably won't get any product at all unless you were doing a liquid to liquid extraction with a fair bit of lab-ware/glass-ware (for example, doing a reflux of the DCM and basified bark soup would lyse the cells better without losing solvent).
Apochrahyll said:
Yep. It just doesn't raise the pH enough. It's good for converting DMT acetate to a base if you already have goo, I would imagine (I've read some reports here of doing things like that). But once again, your bark could be just as important in that it may be weak/bunk or you're not using enough. Remember, you need to use enough bark so that any product that gets wasted/lost along the way isn't your entire yield. 10g isn't enough to fulfill this requirement
EDIT: I tried using sodium carbonate for my first extraction as well, and I didn't get anything at all from 100g of quality bark. I'm not really sure why people continue to recommend it for extractions, because I've never seen someone use it for one successfully. All the eco friendly teks only ever turn out a brown goo if anything :|
EDIT 2: Maybe try an acid boil before basing to help lyse the cells and mix the salts into solution. That always seems to help yields, though if overdone can preclude the precipitation of crystals in favor of brown goo.
- Merits
- 42
The use of dichloromethane, and other chlorinated solvents, is really not advised in kitchen-level extractions. Apart from the carcinogenicity of chlorinated solvents, they can also react with tertiary amines such as DMT, creating unwanted impurities(*).
The chloromethylation side reactions generally do not proceed very rapidly, so by employing proper methods and equipment, such as a quick liquid-liquid extraction in a separating funnel and subsequent immediate concentration of the extract in a rotary evaporator, the complications are minimized. Additionally, in a well-equipped laboratory the chlorinated solvents can be handled in a fume hood.
IMHO chlorinated solvents should be avoided if the above methods and precautions are not available. Use them only with regular A/B extractions where the contact time between chlorinated solvent and DMT (and the operator) can be minimized.
(*) http://www.sciencedirect.com/science/article/pii/S002196730081643X
The chloromethylation side reactions generally do not proceed very rapidly, so by employing proper methods and equipment, such as a quick liquid-liquid extraction in a separating funnel and subsequent immediate concentration of the extract in a rotary evaporator, the complications are minimized. Additionally, in a well-equipped laboratory the chlorinated solvents can be handled in a fume hood.
IMHO chlorinated solvents should be avoided if the above methods and precautions are not available. Use them only with regular A/B extractions where the contact time between chlorinated solvent and DMT (and the operator) can be minimized.
(*) http://www.sciencedirect.com/science/article/pii/S002196730081643X
Apochrahyll said:
These teks are designed for optimization, and it is best to follow them as written whenever possible, especially if you are new to the process. I do realize that some materials are harder to get depending on location and other factors but for Q21's lime tek, all the foodsafe ingredients can be found online, on Amazon even.
Or, if you happen to be in the states, Walmart carries pickling lime (calcium hydroxide) which is the proper/optimal base needed for this dry tek. Lye is not really suited for this tek, and I would not recommend using it, as Q21 suggests.
If you do want to use lye, I second what Heyt said about using Cyb's tek with Earthwalker's cleanup steps. Following this tek to the letter always produces great results, assuming the bark isn't bunk.
If you can't find naphtha, what about Bestine? It is sold as rubber cement thinner (it contains n-heptane). This can sometimes be found in craft, hobby, or hardware stores. Or anyplace that might sell rubber cement.
Anyway, hopefully your next extraction goes well! Be safe and good luck to you!
