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DMT solubility and rapid freeze precip questions Options
 
uggmr
#1 Posted : 9/21/2009 6:53:18 PM
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Does anyone have any data on the solubility of DMT in naptha at different temperatures? I know it's difficult to be exact, fats, water in the solvent those sorts of things will alter things. Basically what percentage of the DMT in totally saturated 60C naptha can remain at 0C?

This is leading onto whether it is worth sticking your precip jar on top of some dry ice, or even liquid nitrogen? In fact, if you were to pour your naptha onto a thin layer of liquid nitrogen, so it boils through the solvent and cools it rapidly, what would you expect? Frozen naptha melting to contain very small crystals? What about using something else above naptha's freezing point, but still cooling it rapidly. Can you get crystals too small to get caught in coffee filter paper?

Finally, will DMT precipitate on it's own, from a fairly saturated solution, without temperature changes?

Thanks all, sorry if these seem like annoying questions, just curious.

Max
 

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romiir
#2 Posted : 9/24/2009 11:29:22 PM
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uggmr wrote:
Does anyone have any data on the solubility of DMT in naptha at different temperatures? I know it's difficult to be exact, fats, water in the solvent those sorts of things will alter things.


With some quick calculations based on some average numbers, I would estimate that room temperature naptha solubility of spice to be around = 2.04081633 mg/ml but take this with a grain of salt for accuracy. All solvents can hold more material at higher temperatures and less material at lower temperatures, this is why if SWIM pulls with a hot solvent and then cools it, it will become super saturated (ie: the solvent can no longer dissolve the amount of material which is dissolved in it, so it precipitates.

uggmr wrote:
This is leading onto whether it is worth sticking your precip jar on top of some dry ice, or even liquid nitrogen? In fact, if you were to pour your naptha onto a thin layer of liquid nitrogen, so it boils through the solvent and cools it rapidly, what would you expect? Frozen naptha melting to contain very small crystals? What about using something else above naptha's freezing point, but still cooling it rapidly. Can you get crystals too small to get caught in coffee filter paper?


According to physics/chemistry the closer you get to freeing the napatha, the better, however if you heat it back up, the same thing happens in reverse and the napatha will re-uptake what was precipatated out. (if watched, it will melt back into the napatha like ice melting into water, kinda)

SWIM thinks that liquid nitrogen would be overkill since you can't filter frozen naphtha very well.. Unless swim used a vacuum filter apparatus which could suck up the thick gel-like napatha.

uggmr wrote:
Finally, will DMT precipitate on it's own, from a fairly saturated solution, without temperature changes?

No, the solution has to become SUPER-saturated for precipitation. Basically this means that the solution must have a temperature lower then the temperature at which it was saturated. If the solution is already saturated, and more material is added it will not dissolve, the same goes for the solution with a lower temperature, it all of a sudden loses the ability to dissolve as much material as it previously had, so particles precipitate out of the solution.

Coffee filter paper will catch most crystals and if they are really small you may want to wash the paper with alcohol afterward to remove the crystals stuck in the paper. However you may find that the return on this process is not economical unless you brew your own ethanol. (Solvents are expensive, evaporating them is evaporating money.)

uggmr wrote:
Basically what percentage of the DMT in totally saturated 60C naptha can remain at 0C?

Not sure, although you can compare your yield to what the theoretical yield is and find out!

uggmr wrote:
sorry if these seem like annoying questions, just curious.

No such thing as a bad question! I think I speak for the community when I say we are happy to help as much as we can.

Best of luck!, Hope this helps you on your quest to enlightenment!

Edit:
romiir wrote:
uggmr wrote:
Finally, will DMT precipitate on it's own, from a fairly saturated solution, without temperature changes?

No, the solution has to become SUPER-saturated for precipitation. Basically this means that the solution must have a temperature lower then the temperature at which it was saturated. If the solution is already saturated, and more material is added it will not dissolve, the same goes for the solution with a lower temperature, it all of a sudden loses the ability to dissolve as much material as it previously had, so particles precipitate out of the solution.

Slight correction:
If a solution of something dissolved in napatha was left to sit with the lid open, it would eventually start to become supersaturated as the solvent leaves the container. This is why many tek's say to evap partially and then freeze precip. It greatly increases the supersaturation of the napatha by changing the amount of napatha to the amount of material ratio. (X mg/ml when you remove ml you still have as many mg, so your solution is more concentrated...)
 
endlessness
#3 Posted : 9/24/2009 11:36:31 PM

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I dont know about the numbers of solubility, but you already got some good answers.. One thing that SWIM knows from experience: When making recrystalization, he uses 30ml of warm naphtha (at maybe 50c) to pick up 1g impure dmt, which leaves a goo of impurities in the bottom and picks up most of the dmt.
 
GreenDMT
#4 Posted : 10/6/2018 5:57:12 PM

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uggmr wrote:


Finally, will DMT precipitate on it's own, from a fairly saturated solution, without temperature changes?



Yes, only if leave your solution for long period of time, Swim once left low saturated naphta which didn't precipitate in freezer, instead he forgot the solution in a friedge at 4 degree and after 3 weeks he got from there one crystal of .3 and another time he forgot a solution which was freez precip once and put in a jar and after 3 weeks at room temperature there is a circle of crystals on a wall of they are still small
 
 
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