Precipitating DMT at room temperature?

[1ce]

I had a thought, and maybe somebody more knowledgeable might be able to give some insight to my question.

So, what if we used 2 imiscible layers. A top layer as the organic layer that contains our alkaloids, and a bottom layer in which DMT is not soluble in. Couldn't we just evaporate off the top layer and let the DMT precipitate through to the bottom?

I.E. naptha over water. Acetone or DCM would be fantastic choices due to their volatile nature. Except acetone is miscible in water and DCM would form a layer at the bottom.

Assuming we could simply do this, wouldn't it be favorable since we don't loose spice trapped in solvent?

 

[Gone-and-Back]

This sounds like it would work, but you also need to think of what else will be coming across into your extract. If your evaporating your solvent, your final product will contain all the fats and oils that the naptha pulls as well. If your not going for a very pure end product, then I dont see why it would be a problem.

For all we know, the fats and oils may be soluble in the water as well, and will just transfer from the naptha to the water and could be redissolved through further agitation, leaving behind the freebase DMT. If this works, now your going to have to find a way to filter it. You could try pouring it through coffee filters, and then scrape it all off once its dry, but this can become a long and annoying process.

Another way of retrieving would be to place the filter paper after filtration into a jar with alcohol, and shake it around to redissolve the DMT, remove the filter, and recrystalize by slowly evaporating the alcohol.

The only way to find out if it works is to give it a try though. If you have some extractions you can play around with, give it a go and report back with what the outcome is.

 

[1ce]

Yeah I definitely would like to try it. I have a vacuum filter I can absolutely cheat with to expedite results. If all those fats can be removed by a simple recrystalization then the overall yield could potentially be a little better since none of our spice will be trapped in the naptha anymore. I have an extraction that may have a pull or two left in it. I'll give it a go, -including recrystalizing so we have a full range of results.

 

[1ce]

You know I had another idea I'd like to try first. What if I evaporated most of my solvent over distilled water. And freeze precipitated it. Could this facilitate better crystal growth by allowing the shards more room in the liquid to grow?

Also would they for suspension crystals between the two layers?

This way we could allow the crystals to drop out of the naptha while allowing it to retain the fats and oils. And perhaps even start their growth outside of the naptha away from the other organic contaminants trapped within the solvent.

I'm thinking if I use my D-H2O washing step to remove water soluble organics from the naptha then most of my precipitate should in theory be just DMT as the shards would potentially be formed outside of the naptha layer.

Does anyone see any problems with my reasoning?

 

[AcaciaConfusedYah]

Back salting would probably be an easier way to remove unwanted organics from the solvent. I don't really know how the two layers would work. Try it and let us know.

 

[1ce]

I'm trying it now. I don't think I used near enough water though. It froze too quickly causimg the DMT to crystalize prematurely, trapping the solvent. I'm going to let everything thaw and let the crystals redissolve and try with a larger volume of water.

More water should postpone ice formation and allow the DMT to fall out of the solvent. This was another problem I saw because the two layers were forced to co-exist in such a small space. I'm sure this is why I have solvent trapped in my shards.

Update:

I let my solvent evaporate while I took a nap. In short, my nap was too long. So I'm trying to recover my spice from 700ml of water. >.<

 

[1ce]

Well this *kind* of worked. The tricky part was I had to continuously remove it from the freezer and into the fridge to prevent the ice from forming. Fully evaporating the solvent on top of the water merely leaves you with an oil that floats on the surface and adheres to the sides.

When I pour my saturated hot heptane for recrystalizing, I have crystals form immediately. (Within seconds) Perhaps if I were to use a long double shotglass with a minor amount of --near-freezing water and crash this with the heptane, I wonder if I could get xtals to crash out. Then maybe store it in the fridge for a few hours.

Maybe afterwords, I can suck out the water and move it to the freezer.

My next extraction I think I will try this with 100mg.

 

[acacian]

i'm not sure i understand the advantage here to the normal precipitation method or even jsut evapping the solvent into t a dish?

 

[1ce]

That's what I'm trying to work out. The advantages I'm trying to accomplish is resucing the amount of DMT left in my solvent. Also I'm hoping it will make harvesting easier. Whwn I harvest alot of the spice is stuck in a way that leaves a powdery residue that I can only collect by introducing it to my next re-x solvent.

I've introduces (drops of) water to a precipitation. In my experiment they formed ice bubbles at the bottom. I did not have any residue amd the crystals came off the glass very easily. The water also played no significant role in the drying of the crystals. If anything I came to the conclusion that the ice crystals helped prevent DMT from being melted by warming solvent.

 

[AcaciaConfusedYah]

Not sure if this would work, but:

What if you mixed the water with a small amount of DMT saturated ethanol. Would it keep the water from freezing and be saturated enough so the DMT from the NPS doesn't dissolve in the ethenol? Or would the ethanol mix with the nps?

How about saturated saline for the water layer?

 

[1ce]

Not sure if this would work, but:

What if you mixed the water with a small amount of DMT saturated ethanol. Would it keep the water from freezing and be saturated enough so the DMT from the NPS doesn't dissolve in the ethenol? Or would the ethanol mix with the nps?

How about saturated saline for the water layer?

Saline would loose its solubility as the water gets cold unless I saturate it at a near freezing temperature. I've thought about recrystalizing with am azeotropic solution of ethanol/water [95.57%/4.43%]. Then diluting that with water to spread out the ethanol and increase the 'growing area' for my crystals. The solubility of water should take over the bisolvent solution at a cold temperature and the DMT solubility in theory is reduced dramatically.

Also if anyone is reading this have we tried fractionally freezing out acid salta of DMT as impurities? Also if we could do this during an acid boil and record numbers that certain impurities are being forced out via TLC testing... a freeze to a certain temperature point could make for an [safe] easy way to remove our DMT prior to basifying. Maybe we can use this to re-x DMT fumarate?

 

[downwardsfromzero]

For all we know, the fats and oils may be soluble in the water as well

Ummm.... fats and oils are not particularly noted for their solubility in water

Why not make a container out of ice - silicone mould in the freezer or some such, not too difficult. When you have your hot heptane, pour it straight into your cold-as-possible (store it in dry ice?) ice container. Wait a bit, keep it somewhere cold Pour off heptane, then allow container to melt on a filter arrangement to recover crystals...?

Of course, the ice will likely crack if you pour hot heptane into it, so take precautions. (Freezing boiled water makes ice with significantly fewer air bubbles.)

 

[1ce]

I've started experimenting with vapor diffusion but the holidays haven't left me with time to research the most optimal solvent pair.

 

[downwardsfromzero]

Looking back at the OP, you mentioned acetone. Carefully pouring DMT-saturated acetone onto water would allow the acetone to float a little (I suspect) so some of it would evaporate as well as dissolving into the water. And then there's the question of DMT's solubility in aqueous acetone. Pouring acetone solution of DMT into water will likely precipitate the DMT as very fine particles, or possibly an oil. (Sorry, bit of a stream of consciousness going on here - sat drinking green tea!)

Then there's ethanol. Aqueous ethanol dissolves non-polars better when hot and scarcely when cold, bringing vodka recrystallisations inexorably to mind. Or dissolve DMT in 95 - 100% ethanol, pour into water and observe the louche effect. Anyhow, so many experiments, so little time...

 

[1ce]

for diffusion to work the DMT soluble solvent must have a higher bp than the non soluble solvent. Dimethyl Sulfoxide would work except the FP is too high. And most people here would more than likely not respect the solvent.

 

[downwardsfromzero]

for diffusion to work the DMT soluble solvent must have a higher bp than the non soluble solvent. Dimethyl Sulfoxide would work except the FP is too high. And most people here would more than likely not respect the solvent.

Why should the boiling point matter? Flash point is another thing entirely...

 

[1ce]

for diffusion to work the DMT soluble solvent must have a higher bp than the non soluble solvent. Dimethyl Sulfoxide would work except the FP is too high. And most people here would more than likely not respect the solvent.

Why should the boiling point matter? Flash point is another thing entirely...

Because of science. Don't worry, the scientists know what they're doing.

I also meant FP being freezing point.

 

[downwardsfromzero]

That science being...? Sorry if I came across as patronising...

 

[1ce]

That science being...? Sorry if I came across as patronising...

You came across as being clueless.

 

[Orion]

That science being...? Sorry if I came across as patronising...

You came across as being clueless.

I think your flash point might be too low in this case