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I would like to know what you have learnt through experience about recrystallisation

Dmt-74

Dmt-74

Esteemed member
Hi

What you would tell yourself if you could go back in time to when you were just getting started?

What are your top tips?

What should people be careful to avoid?

Thanks!
 
Wrap the container with the warm, saturated solvent in it in a towel or other solvent-resistant insulation. Allow to cool slowly to room temperature before transferring to the fridge for a few hours, then transfer to the freezer overnight. Otherwise keep disturbances to an absolute minimum.

Use of a secondary container, which allows the base of the precipitation vessel to be insulated as well as holding the insulation in place around the sides, will also be advantageous. It's a good idea to have this carefully prepared in advance.
 
Transform said:
Wrap the container with the warm, saturated solvent in it in a towel or other solvent-resistant insulation. Allow to cool slowly to room temperature before transferring to the fridge for a few hours, then transfer to the freezer overnight. Otherwise keep disturbances to an absolute minimum.

Use of a secondary container, which allows the base of the precipitation vessel to be insulated as well as holding the insulation in place around the sides, will also be advantageous. It's a good idea to have this carefully prepared in advance.
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Aaaah ok, interesting, I just always shoved the pyrex dish straight into the freezer, perhaps that's why I always got tiny crystal clusters. Thanks for the tip!
 
To get seemingly forever growing crystals: keep it in a jar at room temperature with a very tiny hole in the lid, this way the solvent will very slowly evaporate and the DMT dropping out of solution will expand the crystals forming.

The biggest drawback of this route however is that you will not reclaim your solvent, so it is pretty bad for the environment.


Also I would like to emphasize that #1 don't from @Transform: never, ever create a hazardous environment where you find yourself in a place with too much solvent in the air. Flash burns, among other, are a very real thing!


Kind regards,

The Traveler
 
Lots of airflow!

When I slow evap, I'll keep it all in a jar with the lid off. As the volume decreases, I'll transfer to one with a smaller area, preferrably before any crystals have really started forming in order to get bigger crystals.

One love
 
not sure if its helpful or not but wish i knew before, when you finish dissolving in n-heptane for re-x make sure to remove from heat bath and be extra patient, waiting allows for the goop to fall all the way down and makes you have to avoid doing it multiple times
 
If you get the concentration just right, you end up with bigger crystals within a few hours. You have to make sure it stays undisturbed, do it at night before going to bed. Your solution should be saturated, but not so much that the crystals would fall out too quick. Try to play around with different concentrations and see how it goes. In my experience, if you get it a right, most of the DMT would fall out at room temp, some amount in the fridge, and you could simply skip the freezer part and instead pour off the solvent and either slow evap or salt it out. I usually salt out the tiny left over amount with benzoic acid.

If you want really big crystals, then go for a minimum saturation, and do a slow evap, likely over a month or so.
 
Pandora said:
I have learned:

R-ex makes pretty xtals and gorgeous little clear shards but a significant and sometimes disturbing percentage of the yield is lost.

So when R-ex is done I retrieve the puck of dross and save it to throw into my next batch of basified MHRB soup.
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Interesting thanks, must try this
 
Btw in following extractions I began to implement a double water wash, pre-freeze precipitation which significantly decreased yield loss in subsequent re-x’s.
 
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