Is it possible to purify DMT by sublimation?

[blue.magic]

The subject says it all. I wonder wheter vaporized DMT will deposit and form crystals.

I was thinking about a setup with a small beaker with some DMT in it and round bottom flask filled with ice on top.

There will be a thermocouple probe (standard K-type wire probe for TM-902C) stuck between the beaker and the hotplate to control temperature.

Alternative setup: Closed petri dish with DMT and ice-filled beaker on top.

Yet another setup: Erlenmeye flask with DMT and glass cotton plugged in on top.

What do you think? Is this doable?

 

[Camponotus]

would work definitely but don‘t know about the setup!
there would probably be a potential loss of some spice according to ron and some impurities may will evap along with the spice and condense with it
there‘s an old thread about it with a similiar setup on the nexus
would be better for seperating dmt from another compound like 5meo if both are nearly pure or something like this
perhaps it would work well for cleaning too but your setup has to be very genious with different stages and temperatures and much complicated stuff and settings... most likely

on the initial question yes it will probably form crystals you can see it in the pipe sometimes

 

[benzyme]

there is wide variability of vaporization temperatures, as polymorphism exists with this compound.

 

[downwardsfromzero]

Typically sublimation would be carried out under reduced pressure using a side-arm test tube fitted with a cold finger - preferably with a ground glass joint.

The set up described in the OP:

a small beaker with some DMT in it and round bottom flask filled with ice on top.[...]
Alternative setup: Closed petri dish with DMT and ice-filled beaker on top.

would equate to short-path distillation as the temperatures required at normal atmospheric pressure would melt the DMT.

You need to use a vacuum, preferably after purging the apparatus with inert gas.

A couple of pictures are attached.

 

[blue.magic]

Thanks. I will try that some day. Unfortunately, I don't have the coldfinger trap or the short-path distillation apparatus. But will try it.

As for the atmosphere: Would dry CO2 suffice?

 

[Camponotus]

“At temperatures below 300C, gaseous CO₂ can be considered "inert gas" as is commonplace in the food industry.“

from

Q & A

 

[blue.magic]

“At temperatures below 300C, gaseous CO₂ can be considered "inert gas" as is commonplace in the food industry.“

from

Q & A

Thanks for doing the search for me. It's not that I am so lazy - but I run several projects and just postponed my search until having some spare time...

Okay so I imagine running just some reaction to produce (dry) CO2 to flush the apparatus, then run this tiny-scale experiment. No need to get a gas bomb

 

[benzyme]

I’ve tried this 10 years ago with this app, hotplate, an IR thermometer, and a Gast DOA-P104AA. it’s not as straightforward as you’d think.

 

[downwardsfromzero]

it’s not as straightforward as you’d think.

The low-ish m.p. of DMT doesn't help here, it's likely a pretty stiff vacuum will be needed to get the vaporisation temp. down to a sensible level. This is loads easier with a compound with a more forgiving balance of melting point and vapour pressure, such as caffeine.

Also it's a bit of a trick to have the minimum gap between the crude solid and the condensation resublimation surface without the two solids growing together. At least you (benz) have the proper sublimation head which allows the easier removal of the cold finger. The apparatus depicted in my photos has rather a small aperture through which to be removing the cold finger and will probably require some kind of workaround.

 

[blue.magic]

As for the vacuum, something like 100 mbar is still reachable with my lab pump (diaphragm type).

But it seems there are more factors at play and the substance won't cooperate so easily.

I originally though that would be easier as that happened normally in my humbe oil pipe - but the conditions and the deposition rate wasn't ideal of course...

I am bashing my head against the wall now for not going to study chemistry and doing IT instead... feeling like having wasted my life.

 

[benzyme]

there are two known polymorphs. one melts/vaporizes at considerably lower temps than the other...and a simple re-x won't separate them. fractional distillation might, but dmt is dmt, and having a mixture of the polymorphs doesn't make it any less pure.

pub chem lists the b.p. as 60-80C, no mention of reduced pressure.

 

[blue.magic]

dmt is dmt

Yep. As long as it is pure, I don't care that much about looks.

The purified DMT would be used for re-x anyway (to grow larger crystal from solution).

Another possible application of such high purity DMT would be a source for a clean fumarate salt for IV application (although I will probably never do this).

 

[benzyme]

one of the intersting aspects I’ve found from reading about Raman spectroscopy is its ability to
elucidate polymorphs. Pehaps I and/or Loveall will be able to investigate this structural phenomenon once we fine-tune the specs.

 

[Trickster]

I’ve tried this 10 years ago with this app, hotplate, an IR thermometer, and a Gast DOA-P104AA. it’s not as straightforward as you’d think.

I tried sublimation with the device in picture and 2-stage oil pump delivering 15 microns of vacuum. I ran it for 30-40 min. Not a slightest sign of sublimation. Should I have waited for longer?

 

[Trickster]

there are two known polymorphs. one melts/vaporizes at considerably lower temps than the other...

Am I right assuming that the boiling point of both polymorfs would be the same? After all liguids are structureless, regardless of the crystalline form they had before being melted.

 

[benzyme]

thermodynamically speaking, the less sterically-hindered isomorph would melt at a higher m.p., I'm not sure what this translates to as a b.p. range. Every value listed in lit. is at reduced pressure, something like 160C @ 0.6 torr.

 

[Brennendes Wasser]

I was placing some crystal white Spice from what I believe that it is nearly 100 % pure on a hot plate and started to heat it up, and it started melting at 80 °C Oô. Kind of extremely high regarding other sources.

Also it started to give slight vapor from 144 °C onwards, but no real evaporation still until 160 °C. At least at 165 °C a vaporizer works great with the same spice ...

So in this case that would sound like it being 100 % the higher melting polymorph, but I guess that sounds strange that it is 100 % of this species O:

 

[Ulim]

If anyone goes further with this we need images of the result.
I know from my vape that you get beautiful patterns of dmt on the glass.

Sublmimation might not work but i dont see why a shortpath wouldnt work. Also just filling it into a long tube then dipping the end into mineral oil at 150c and then collecting the crystals that wander up the flask would be an easy way to do a quick, simple and dirty distillation.

The tube might need a bend in it thought to prevent the dmt from flowing back down.