are excellent tools for getting exceptionally pure products that vaporize and solidify at moderately low temps (in vacuo) from crude extracts; they require the least hassle, assuming a vac source is available.

swim is looking into acquiring one of these

can also function as a righteous vap *edit* no it can't

Make sure you have a good reason to buy it before getting one. It is considered a "duel purpose item" by the DEA.

SWIM purchased a non-vacuum sublimator and was told by the seller he had to provide a reason for the purchase just in case the DEA wants to ask about its sell. SWIM did not know sublimators were watched items. That REALLY SUCKED. Of course SWIM provided them with a valid reason for needing one which was acceptable. SWIM doesn’t like the fact that he’s now on their list. If you don’t give a reason, it is more suspicious and you’ll likely get reported. So if asked, provide a good reason.

Aside from that rather grim reality, the sublimator is a great device. And you don’t need a vacuum sublimator unless you’re sublimating very sensitive things. Actually a vacuum sublimator is a little tricky to use because the vacuum changes the vaporization point of the chemicals you’re sublimating, so you’ll need to adjust for that. Also, the chemical being sublimated can go into the vacuum tube in some cases. SWIM likes the non-vacuum sublimators that do not have a cold finger. Cold fingers are a pain to deal with.

Here’s the kind SWIM likes:



If you have a non-vacuum sublimator and a digital hotplate that is accurate you can easily separate alkaloids from each other and other things. For example, set your hotplate to 90 C, and the sublimator will heat up to about 65C (depending on the hotplate and sublimator of course) and you’ll see the DMT vaporized away and get trapped in the condenser. It’s like you’re smoking the DMT, only it’s getting trapped in the condenser. It’s a really cool idea.

With a sublimator you can get complete separation of DMT, 5-MeO-DMT, and 5-HO-DMT (bufotenine). They all vaporize at completely different temperatures ranges. DMT vaporizes below 100 C (at 60-80 C), 5-HO-DMT vaporizes above 300 C (at 320 C) and 5-MeO-DMT vaporized in between there (at about 120 C I believe, I can’t find the reference for the boiling point, but the melting point is 67-70 C).

hmm
perhaps swim will deal locally, with cash
the store where swim goes sells without questions.
swim bought liters of denatured EtOH and methylene chloride there, and swim mainly extracts/distills essential oils for aromatherapy.

SWIM has never used sublimation for anything useful except a few experiments. He's never tried sublimating DMT, 5-MeO-DMT or 5-HO-DMT, he was just speaking hypothetically. I think a vacuum sublimator would be needed to sublimate those. He’s read about sublimating DMT, and they used a vacuum sublimator.

A vacuum sublimator is probably your best bet if you are planning to use it for things that don’t sublime at normal pressure.

Of course you could distill DMT, 5-MeO-DMT, and 5-HO-DMT without a vacuum, but that’s not quite the same process and I don’t think a sublimator would work for that.

Does anyone know the sublimation details for DMT, 5-MeO-DMT, and 5-HO-DMT?

I'm still wondering if an improvised kitchen setup is possible for simple spice purification... it could be a nice alternative for naphta recrystallization. I'm thinking of a simple test tube, loosely closed at the top, gently heated at the bottom where the raw spice is. The point is to maintain the temperature gradient for a while until all the spice has migrated to the cool end of the tube, and the nasties are left behind (in theory).
When inhaling, I notice that this is happening all the time, unintended: the vapor/mist quickly recrystallizes on cold surfaces, this stuff seems to be very pure!

If too much DMT is oxidized to DMT-n-oxide, maybe fill the tube with CO2.
Also: find something suitable (rounded) to scrape it out of the tube...

I'll try this on a small scale, I'll let you know how it went.

SWIM tested this and it doesn't work for DMT in a normal sublimator. It all vaporizes away. You need a system where the condenser is NOT above the boiling flask, so that when the DMT cools down to a liquid it doesn't fall back down into the condenser. Plus, you need a super long condenser or it needs to be super cooled, or it all just vaporizes away.

Yes, as usual you're right 69ron. I tested this yesterday, it did condense on the walls but it flows back. You get the infamous 'creeping spice' that can happen with glass pipes if the flame is too small. The drops that did stick haven't crystallized a day later, it's probably DMT-n-oxide. I don't think it all vaporized away though.
Oh well, it was worth a try... I imagined slow growing pure spice crystals on a cold finger but that's just a fantasy

so swim ordered the micro-sublimator posted in the original link, and is going to have to experiment.
he's already set up an improvised vapor trap (which will sit in an ice bath for the experiment) to catch any spice vapor that escapes. the same trap has a manometer attached, so he can monitor the pressure as needed


heh there's lots of snow in his area, so he has an unlimited supply for the coldfinger and icebath

he also got this for electrochemical reaction experiments, 48 bucks on the 'bay.

Good luck, please post your results! Very advanced stuff going on here...



69ron, do you mean in vacuum?
In normal pressure it doesn't boil away in hot water. Just tried it by sticking a test tube with a bit of spice in boiling water - that would be a neat way to vaporize but it just doesn't at that temp! Melting yes but boiling or sublimating... no. Isn't it less volatile than often assumed?

SWIM did not try it in a vacuum. It should work in a vacuum if the vacuum is right.

It won't vaporize in boiling water? That's weird. It's the freebase right?

Yes it's the freebase.
Just verified it again with higher purity spice, even tried to suck up some vapor but no, it just melts at 100 C, it certainly doesn't boil. I have no idea why everybody seems to think it's even more volatile than water??? Confusing MP with BP?

It's easy to verify: just stick a small test tube with some spice in boiling water and see for yourself!

alright, SWIM's just done an STB extraction on 100g, and has a good deal of yellow oil. he'll likely get his sublimator tomorrow or tuesday in the mail.

anyone know the boiling point of DMT? a couple sources say 60-80C, that's a pretty wide range.

SWIM needs to readjust for vacuum, he's looking at performing the sublimation at around 48C at 22"Hg (estimated from a nomograph)

what swim has learned: STB with DCM is dirty. he's convinced that even recrystallizations with heptane will yield crystals with plant lipids in them. the spice was pink, and smelled sort of floral and fishy, but somewhat like plastic. the sublimed residue from a 50mg representative sample was very small and clear. he feels he'll need to do an a/b on what he has, and is contemplating what to do with his freeze precip (slightly yellowish-white crystals in heptane)

You mean on the cold finger? Must be very pure stuff, that's a succes for the sublimation purification unless the yield is just too low..

DCM should be more efficient than naphta, hey you didn't get any jungle spice did you!?
Actually, why not defat afterwards - much less solvent needed, no emulsions... and you see the white DMT appear on basifying - no black sludge

One thing about recrystallization: DMT tends to 'oil out' because of its low melting point. If the solvent is too hot, on cooling the DMT won't form crystals but tiny droplets that spoil the purification process because they absorb the contaminants. Perhaps keeping it below the MP, say 40 C, and using a bit extra solvent is better.

good advice

gonna process the pink spice with an a/b to clean it up more, and use a warm recrystallization solvent to rinse off the coldfinger when attempting again

What about fractional sublimation?

This can be used to completely separate DMT from 5-MeO-DMT because they will both sublime at very different temperatures under vacuum. I have no idea what the temperatures and vacuum setting to use are though.

If one could use this tech on a Diplopterys extraction, they could get 5-MeO-DMT that is completely free of DMT. 5-MeO-DMT is still legal in many countries.

hmm

what does this procedure entail? can a standard micro vacuum sublimator be employed?
never heard of it but it seems like an advanced technique, certainly worth investigating

No special equipment is needed, except accurate temperature control and either no vacuum or a very consistent vacuum.

For example, if item A sublimes at 100 C, and item B sublimes at 200 C, they can easily be separated using sublimation. If you have an accurate hotplate with your micro vacuum sublimator sitting on it, setting the hotplate to 150 C should make the micro sublimator reach an internal temperature of about 110 C near the bottom of the flask. That would sublime all of item A onto the cold finger if run long enough. After it appears that no more of item A is subliming, you gather item A from the cold finger and save it. Then you run it for 1 hour at the same heat setting to be sure all of item A is gone. If the cold finger comes out clean, then all of item A was sublimed. If not, collect it and clean the finger and run it again for another hour and it should come out clean. Next turn the hotplate up to about 250 C to make the micro sublimator reach an internal temperature of about 210 C near the bottom of the flask. Item B should start to sublime completely free of item A.

You can make a sublimation apparatus on the cheap for about $20-$30. Get a flask, a thermometer, a test tube, some dry ice/liquid nitrogen, and a hot plate.

Heat up an oil bath to your desired temperature. Duct tape around your test tube so that it fits into the flask nicely and seals. Put your material into the flask. Add dry ice/liquid nitrogen to the test tube. Wipe any condensation off with a cloth and then stick it in the flask. Stick the flask into your oil bath. You should be able to get most of it onto the test tube in one go.

I have no idea how well DMT sublimes, as I've never had a sample of it (being illegal).

no kidding



one could also make a melting point apparatus using the same equipment (sans dry ice)