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Is it possible to purify DMT by sublimation? Options
 
blue.magic
#1 Posted : 7/7/2018 8:26:44 PM

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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?
 

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Camponotus
#2 Posted : 7/9/2018 6:27:12 AM

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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
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benzyme
#3 Posted : 7/9/2018 4:22:42 PM

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

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downwardsfromzero
#4 Posted : 7/9/2018 5:53:29 PM

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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:
Quote:
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.
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sublimator2.JPG (2,974kb) downloaded 124 time(s).
sublimator.jpg (4,513kb) downloaded 123 time(s).
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blue.magic
#5 Posted : 7/10/2018 3:06:25 PM

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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
#6 Posted : 7/11/2018 10:44:26 AM

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

from

Q & A
It's the job that's never started as takes longest to finish. - J.R.R. Tolkien

How long will this last, this delicious feeling of being alive, of having penetrated the veil which hides beauty and the wonders of celestial vistas? It doesn't matter, as there can be nothing but gratitude for even a glimpse of what exists for those who can become open to it. - Alexander Shulgin
 
blue.magic
#7 Posted : 7/12/2018 2:10:10 AM

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Camponotus wrote:
“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 Smile
 
benzyme
#8 Posted : 7/12/2018 2:22:18 AM

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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.
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downwardsfromzero
#9 Posted : 7/13/2018 3:57:08 PM

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benzyme wrote:
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.
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“To be GOVERNED is to be watched, inspected, spied upon, directed, law-driven, numbered, regulated, enrolled, indoctrinated, preached at, controlled, checked, estimated, valued, censured, commanded, by creatures who have neither the right nor the wisdom nor the virtue to do so. To be GOVERNED is to be at every operation, at every transaction noted, registered, counted, taxed, stamped, measured, numbered, assessed, licensed, authorized, admonished, prevented, forbidden, reformed, corrected, punished. It is, under pretext of public utility, and in the name of the general interest, to be place under contribution, drilled, fleeced, exploited, monopolized, extorted from, squeezed, hoaxed, robbed; then, at the slightest resistance, the first word of complaint, to be repressed, fined, vilified, harassed, hunted down, abused, clubbed, disarmed, bound, choked, imprisoned, judged, condemned, shot, deported, sacrificed, sold, betrayed; and to crown all, mocked, ridiculed, derided, outraged, dishonored. That is government; that is its justice; that is its morality."
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blue.magic
#10 Posted : 7/15/2018 3:47:21 AM

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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 Smile - 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
#11 Posted : 7/15/2018 3:58:25 AM

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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.
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blue.magic
#12 Posted : 7/21/2018 10:19:04 PM

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benzyme wrote:
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
#13 Posted : 7/22/2018 12:43:18 AM

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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.
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