freeze precipitation help please!

[monty p]

SWIM has done 2 successful freeze percip's, SWIM has a third one in the freezer. It has been in there about 24hrs now and there is quite a bit of lovely clean looking white dmt sticking to the jar as expected, but, there is also some (what seems to be) white dmt floating in the naptha. SWIM is still a novice extractor and has not seen or read about this, can anyone enlighten SWIM as to why this may be?

Thanks in advance for any suggestions!

 

[tele]

It is completely normal to have some of the crystals floating around in the solvent, however the reason why this happens is unclear to me... To get them out, one might consider pouring the naphtha off through a coffee filter.

 

[monty p]

thanks tele, will try that

 

[tele]

thanks tele, will try that

It's also possible just to pour the solvent off very slowly, but one has to be extra careful not to lose the floating crystals. I think it'll be easier to secure with that filter. It will just be as "insurance" if any might fall through. Keep as many as you can in your precipitation container, even if they are floating.

 

[Swarupa]

I love pouring through a coffee filter, the filter drys so fast & you have these super light soft fluffy shiny happy crystals

 

[DiMiTriX]

the floating crystals are due to unclean suface of your jar in swim opinion

 

[journeyman]

Gotta disagree about it being an unclean surface. It seems that after i clean my precip pans super well, many individual crystals will form on the glass with a fair amount of floaters. But the second run on the same pans without cleaning them never has any floaters ever and the crystals are always in a thin sheet all on the glass. This is in my own experience though and i just imagine our techniques differ.

By the way, why do my crystals always melt when i pour them through a coffee filter? I just cannot seem to master that technique..there are never any crystals on the filter when its all said and done, but some usually freeze precip out of the solvent the second time.

 

[Xt]

I get a vibe that lots of people try to precipitate each pull individually. This is not ideal.
I would recommend doing every single pull... combining them all, evaporating to 50% volume then freeze precipitating out for maximum efficiency.
Trying to precipitate each pull individually just doesn't make sense and surely must cause many people problems.

 

[Ellis D'Empty]

I've noticed, that at least IME, that I seem to only get a lot of floating crystals when I have a THICK layer of them on the jar, that layer is almost ALWAYS trapped naphtha inside of it as well.

I suspect it has something to do with getting it cold fast and having the crystals no where to latch on, or something of that nature.

 

[hexagonal]

I get a vibe that lots of people try to precipitate each pull individually. This is not ideal.
I would recommend doing every single pull... combining them all, evaporating to 50% volume then freeze precipitating out for maximum efficiency.
Trying to precipitate each pull individually just doesn't make sense and surely must cause many people problems.

i'm curious, why is the evap necessary? is there any risk of evapping dmt along with the solvent? Also, if you don't evap, you can reuse the solvent for the next pull.
, and combining pulls would leave you with varying degrees of purity, no? Please help me understand.

 

[Entheojen]

i'm curious, why is the evap necessary? is there any risk of evapping dmt along with the solvent? Also, if you don't evap, you can reuse the solvent for the next pull.
, and combining pulls would leave you with varying degrees of purity, no? Please help me understand.

The initial evaporation isn't necessary, but I don't understand fully why some people prefer it.

There's no risk of DMT evaporating at room temperature.

Yes, if you don't do an initial evap, you can reuse the solvent (after a freeze precip so the DMT isn't put back into the MHRB mix)

 

[SpiralNeuroEclipse]

Combining pulls would result in having a consistent purity, i.e the waxier pulls etc. so you would have a uniform purity level, an average if you will.

If you precip each pull separately, that will result in varying degrees of purity. It is easiest to simply combine, evaporate about 50% of the volume of solvent to super saturate the solution, and freeze precip all at once.


Then you can take a look at your purity, and if you arent happy with it, just do a recrystallization with hot heptane to enjoy fluffy snow white crystals

 

[hexagonal]

thanks Entheojen and Spiral.

time to look for some heptane!

 

[Xt]

I get a vibe that lots of people try to precipitate each pull individually. This is not ideal.
I would recommend doing every single pull... combining them all, evaporating to 50% volume then freeze precipitating out for maximum efficiency.
Trying to precipitate each pull individually just doesn't make sense and surely must cause many people problems.

i'm curious, why is the evap necessary? is there any risk of evapping dmt along with the solvent? Also, if you don't evap, you can reuse the solvent for the next pull.
, and combining pulls would leave you with varying degrees of purity, no? Please help me understand.

The evaporation is not necessary but, it does help considerably. There are several factors on how much DMT the solvent may hold. One is temperature hence the freeze precipitation. Another other is saturation.

If you evaporate a portion of the naptha, there is less of it but the same amount of DMT (DMT does not evaporate). This leaves the solvent much more saturated, when the temperature drops the saturated solution (or super saturated solution) is unable to hold that much DMT per ml and it precipitates much more readily.

You could just evaporate the naptha to the point where it clouds up white when blown upon. The clouding is DMT molecules floating about.

You don't need to re use the solvent for each pull. Precipitating each pull individually is innefficient and simply makes more work for yourself.
As SpiralNeuroEclipse mentions, combining the pulls and precipitating results in a uniform... precipitate.

Not meaning to come across like im being rude but, if you think about the principles at work, it makes sense.

I personally prefer an A/B with limonene crashed out with Fumaric acid saturated IPA, an IPA boil to clean, and then CaC02 / H20 converting to freebase with a Recrystallization. This is because naptha stinks, Limonene is far more pleasant to work with and i feel the method is more elegant then the old STB.
Plus STB it is a little wastefull on solvent when done like this.

But you didn't ask about that so ill leave it there. STB works fine, especially if precipitated like above.

I hope this helps.

 

[mumbles]

For best results evaporate your solvent down until you see spice clusters precipitating. Unless you are checking every 15mins this is really only possible with larger amounts.

 

[hexagonal]

The evaporation is not necessary but, it does help considerably. There are several factors on how much DMT the solvent may hold. One is temperature hence the freeze precipitation. Another other is saturation.

If you evaporate a portion of the naptha, there is less of it but the same amount of DMT (DMT does not evaporate). This leaves the solvent much more saturated, when the temperature drops the saturated solution (or super saturated solution) is unable to hold that much DMT per ml and it precipitates much more readily.

You could just evaporate the naptha to the point where it clouds up white when blown upon. The clouding is DMT molecules floating about.

You don't need to re use the solvent for each pull. Precipitating each pull individually is innefficient and simply makes more work for yourself.
As SpiralNeuroEclipse mentions, combining the pulls and precipitating results in a uniform... precipitate.

Not meaning to come across like im being rude but, if you think about the principles at work, it makes sense.

I personally prefer an A/B with limonene crashed out with Fumaric acid saturated IPA, an IPA boil to clean, and then CaC02 / H20 converting to freebase with a Recrystallization. This is because naptha stinks, Limonene is far more pleasant to work with and i feel the method is more elegant then the old STB.
Plus STB it is a little wastefull on solvent when done like this.

But you didn't ask about that so ill leave it there. STB works fine, especially if precipitated like above.

I hope this helps.

yes, this helps considerably. I think it's good for me to know a little more about the chemistry side of things because none of this is very intuitive to me. So no, you don't come across as rude but thinking about the principles hurts my head a bit so it's really a matter of taking in tiny chunks of technical information at a time You explained clearly and it makes sense to me now!


I'd love to try a food grade extraction but limonene seems a bit harder to find around here.

thanks!