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Steam distillation as water-based STB extraction method?

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downwardsfromzero

downwardsfromzero

Boundary condition
A friend told me he had been thinking about steam distillation for the past couple of days.

69ron said:
you should be able to do this directly from the bark. You put powdered bark in basified water, then heat the water to 90 C and the DMT should collect on the cold finger. It should be a very easy way to get DMT. But some other crap might also collect on the cold finger. It all depends on what else vaporizes at 90 C.
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My friend was thinking of using a steam generator (eg, pressure cooker with tube attached to steam outlet) to blow steam through some kind of basified bark and then pass it out through a combined cold finger and Liebig condenser setup. He's always just daydreaming but I'll ask him how it goes. He reckons that DMT is volatile enough that it should come over with the steam quite merrily. What do you guys think?

Steam distillation is usually used to extract volatiles with a boiling point above 100degC, by virtue of combined partial vapour pressures and all that shenanigans...
 
Those words from me were just a theory. It might not work at all, but it's worth a try.

YOU CAN STEAM DISTILL FREEBASE MESCALINE, but it’s very inefficient. However, DMT boils at a much lower temperature than mescaline, so it’s more likely to work better with DMT.

You can distill mescaline and DMT using normal alkaloid distillation methods without using water. Any alkaloid that can be vaporized like DMT can be distilled. But its tricky to do for the average kitchen chemist.
 
this is the most obvious extraction method ever. if you have glassware and your not just distillling the shit, just... wow. please do. i know your smart people but this is just common sense.

i do have a question though: would you just use a solvent to get it out of the condenser after it crystalizes in there?
 
SWIM is also interested in steam distilling basified MHRB. It all works out conceptually at least. He is in the process of acquiring a distillation setup, as well as soxlhet extractor, for other scientific and academic pursuits, and he figures why not get the most out of it. Once he has his glass in house, he'll run some experiments with distillation techniques. He's very excited about the prospect of removing the need for large quantities of dangerous chemicals.

Fuego: SWIM figures that if the DMT does deposit inside the condenser, the most likely case if it is used traditionally (i.e., cold media), then it can be filled with non-polar solvent and run with a heating media instead of a cooling one; the DMT should melt into the solvent pretty easily. Then the solvent can be removed and either evaporated or freeze precipitated. Alternately, warm media can be used from the beginning, during the heating of MHRB solution; if the collection vessel is being ice-bathed, DMT should deposit there instead.

SWIM's idea, which is purely conceptual: Use a double-necked boiling flask to contain and heat the basified MHRB solution; have one neck either closed-off or attached to an addition funnel (for replenishing any evaporated water), and the other attached to a Liebig condenser arranged vertically (via 3-way 75* distillation adapter and 105* adapter). The condenser is filled with hot water, and it leads either into a cold finger or a flask submerged in an salted ice-bath. Heat the apparatus to 90C, and let it sit for a few hours. SWIM has never done this, so he has no idea about numbers or yields. This set-up is not traditional steam-distillation because steam isn't the heating agent in the solution, the hot-plate is. Alternately, you can have two flasks set up and connected to each other such that when water is evaporated in one, it leads to the other and bubbles through the solution. Again, all theoretical and yields are unknown. This method seems better too because the heat isn't directly applied to the solution, and the evaporated water will be consistently 100C; however, more water will end up in the collection vessel. SWIM is planning on doing a whole mess of experiments with different set-ups to see how it goes as soon as he gets his glassware.
 
Well, the cells could be lysed by pulverizing the bark and freezing it in water several times. That should be enough to destroy most of the cell walls. In any case, suppose you set up a solution of MHRB and and lye water at normal ratios (i.e., 1g MHRB : 1g lye : 15mL water), then if you can heat up that solution to 80 or 90C, freebase DMT should theoretically come out of the solution at its boiling point, along with whatever other compounds come out at that temp. Water can be added to the solution to keep the pH at a sufficiently high level. In any case, it's all theoretical like you said. When SWIM gets his chemistry setup, he'll start in depth work on this subject.
 
Has anyone actually tried vaporizing DMT at 100 C? I have, and nothing vaporizes. People keep saying it boils below that but I can't confirm this... just stick a small test tube with some freebase in boiling water and see what happens. All it does is melt, not a hint of boiling or vaporization!

My guess is you really need to let the vigorous steam carry it away, like in classical steam distillation of essential oils (and limonene): 90 C would not be enough.
Then, once it's distilled, how to separate it from the water? Just let the water evaporate, or would an extraction with nonpolar solvent be needed?

Anyway: if it works the result would be very pure. Good luck!
 
Good point. Steam distillation seems the most appropriate way. To get the DMT out of the resulting solution, the distillate can then be distilled again; since the DMT base isn't soluble in water, and it has such a small boiling point in comparison, and there won't be scores of other macromolecules from the MHRB bouncing around, this second round of distillation should yield actual crystals. Or the water can be evaporated, but an extraction with nonpolar solvent is also a viable option.

Here's what wiki has to say: "Highly pure DMT crystals, when evaporated out of a solvent and deposited upon glass, often produce small but highly defined white crystalline needles which, when viewed under intense light, will sparkle. The crystals appear colorless under high magnification."
 
Nzym said:
Here's what wiki has to say: "Highly pure DMT crystals, when evaporated out of a solvent and deposited upon glass, often produce small but highly defined white crystalline needles which, when viewed under intense light, will sparkle. The crystals appear colorless under high magnification."
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swim has tried this via sublimation under reduced pressure (in vacuo.. approx. 50mg dmt freebase in a small amount of varsol). dmt appeared on the coldfinger as a clear residue, not crystalline. not sure why, but dmt isn't easy to recrystallize on a coldfinger, especially when using small samples.
though rest assured, by using this technique (distillation or sublimation) at the proper temp, anything you recover will be pure dmt
 
Yes, that's a great advantage. That must have been very pure dmt Benzyme, supersoft to inhale... sublime!

I think I'm going to do a test run with 50 grams of mhbr next week, I have a condenser home-made of copper pipe. The copper wouldn't be a problem would it?
Any dmt crystals inside can be flushed out by running it for a short while without cooling water, no problem.

So.. how about taking 50 grams of mhbr powder, 20 grams of lime, 350 ml of water, distill that (boil vigorously). To check for remaining dmt in the boiling flask, this residue can be extracted with naphta while still warm - no need for losses, it's possible that most of it stayed behind. Yield should be 0.3-0.5 g.

I hope the boiling breaks down the cell walls and Ca(OH)2 is basic enough. No boiling lye please...
 
Well, today I made an attempt.
A few errors made, a few things learned...

At first just clear water was coming through (tasted funny, a strong Mimosa fragrance, not unpleasant!) but as I increased the heat, behold! Some tiny dust-like crystals were floating in the water, I could faintly smell DMT too. BUT unfortunately I estimate it can't be more than a few milligrams from 20 grams of bark after half an hour of boiling, I'm starting to think it's just not worth the effort...

And lime/bark clumps stuck to the flask, too much heat dried it out and voila, a crack in the flask :( Stirring required! Maybe one more attempt with a steel kettle. Foam was no problem.

Following the plan, I'm now extracting the residue with naphta, the first pull is in the freezer. I suspect most of the DMT was still in the residue, it's really hard to boil it off.

If using lye instead of lime, the temperature would be higher, maybe more DMT will vaporize?
 
tryptographer said:
Well, today I made an attempt.
A few errors made, a few things learned...

At first just clear water was coming through (tasted funny, a strong Mimosa fragrance, not unpleasant!) but as I increased the heat, behold! Some tiny dust-like crystals were floating in the water, I could faintly smell DMT too. BUT unfortunately I estimate it can't be more than a few milligrams from 20 grams of bark after half an hour of boiling, I'm starting to think it's just not worth the effort...

And lime/bark clumps stuck to the flask, too much heat dried it out and voila, a crack in the flask :( Stirring required! Maybe one more attempt with a steel kettle. Foam was no problem.

Following the plan, I'm now extracting the residue with naphta, the first pull is in the freezer. I suspect most of the DMT was still in the residue, it's really hard to boil it off.

If using lye instead of lime, the temperature would be higher, maybe more DMT will vaporize?
Click to expand...
So, the person who tried this way-back-a-when is still an active member!

The point with "proper" steam distillation is to produce the steam in a separate vessel and send it via a nozzle through the crude plant material/extract/soup. This should help prevent cracking of the flask.

Tryptographer - did you ever perform a further attempt using a steel vessel?
 
Wow, that's an old thread! Nowadays I'm more an occasional lurker than an active member...

No, I never pursued this, not having the proper apparatus, like you say. Kits for steam destillation of essential oils are available, but quite pricy. Yields are probably too low to bother...
 
Thanks for getting back.

I suspect this method would only be of use to those with both plenty of time and plenty of steam at their disposal.
 
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