freeze precip ontop of crystals grown @ room temp

[concombres]

I have 0.5g dmt, previously recrystallized twice, forming crystals in ~12ml naphtha at room temp in a shot glass.
There are some nice little crystals formed higher up, & a layer of smaller, interconnected crystals on the bottom of the shotglass.
I'd like to freeze precip & speed up crystal growth, but i feel like the fast change in temperature is going to cause very small crystals to crash out & form a layer of powder ontop of the already formed crystals rather than continue to grow larger crystals from the pre existing ones.
i'm sure theres someone around the nexus who has tries this.
I'd like to hear what the results are like before trying it. Crystal chunks are much easier to remove from a shotglass than powder.

 

[Orion]

You're absolutely correct, you can't crash out nice shards if the temperature changes too quickly, it has to be a slow gradual shift. Having a solution sit at room temperature - saturated enough to start crystal formation - is a good idea. Then once growth stops, take it to the fridge. Once growth stops again, then you can take it to the freezer, but about 95% of the crystals will already be out by that point.

 

[concombres]

Thats what i've been doing with re-x so far. I'm never quite satisfied with the size of the crystals that grow though.
I'd like to grow crystals with a slower, more controlled temp change.
i have figured out a simple method to heat the solvent & cool by 1°c every 24hr, but once room temp is reached, i hit a wall. I'm unaware of any fridge/freezer combo with that type of control over temperature settings.

 

[DansMaTete]

You can put the glass in an insolated container and put this in the fridge. The most efective insulation make the biggest xtals.

 

[concombres]

You can put the glass in an insolated container and put this in the fridge. The most efective insulation make the biggest xtals.

Could you elaborate on this?
I'm curious as to what the insulation does for temperature change. Does it just slow down the rate at which the solvent cools or does it only allow for the temp to drop to a certain point, holding in heat enough to keep from reaching the same temp as the enviornment around the insulated container?

I'd have never thought to insulate & i actually like this idea alot.

 

[Earthwalker]

You can put the glass in an insolated container and put this in the fridge. The most efective insulation make the biggest xtals.

Could you elaborate on this?
I'm curious as to what the insulation does for temperature change. Does it just slow down the rate at which the solvent cools or does it only allow for the temp to drop to a certain point, holding in heat enough to keep from reaching the same temp as the enviornment around the insulated container?

I'd have never thought to insulate & i actually like this idea alot.

Mmmmm I'm gunna try this out myself , very simple ideas are often the best !!:thumb_up:

 

[DansMaTete]

It just reduces heat transfer and so, slows down the temperature drop. If the insulation is really good, it needs hours to loose few degres which is what you want.

In fact, you can use this trick from room temp to freeze temp : you put the shot glass (i would use something with a lead to not spill out some of the naphta) in the insulated container strait after the pulls, then leave it at room temp for a while (more than few hours) then fridge 24h and freezer 24h.

And pictures of the result are welcome :want:




peace