DMT Precipitate At Room Temp! Check this out!

[just999]

First time I did Cybs Max Ion tek.
After 3 pulls I wrapped my container with plastic foil because I wanted to do 3 more pulls on the next day. As you can see the pulls were still containing some impurities from the mimosa mix. (I always seperate and wash thhe clean NPS with sodium carbonate in a seperation funnel.)

So take in mind... these are 3 pulls (~150ml) room temperature with a lot of impurities and no pre evaping!







Have you guys ever seen this before? 150ml NPS / 100g bark...It is not even a little bit conentraded. It was sitting like 15 hours and formed crystals at room temperature....


Even after 3 more pulls (they were totally covered with Naptha) and some shaking the crystals did not moved. I had to heat the NPS in a water bath to make it ready for freeze precipitation. So I putted it into the fridge (after pre evaping). About one hour later I got huuge islands of crystals... Ive never seen this before....

I was like a young child which got some candys *_* So happy!
After I putted it in the freezer and waited 12 hours I received the most fluffiest and biggest , totally white crystals ever!

Just wanted to share this with u guys Sry for my bad english. And sorry for not taking pictures of the final result. But I guess you guys know how DMT fluffy crystals look like ^^

 

[downwardsfromzero]

Nice pics.

Slow evaporation from near-saturated naphtha may have helped here.

 

[just999]

Might be true. But still surprising because slow evaporation would have made a "ring" on the glas and not this concentrated crystal.

This was the last time I am using Naptha. It cant even dissolve DMT at room temperature. I covered the crystals with 150ml more Naptha, shaked and waited for about an hour and nothing dissolved. Maybe I need to say that Im using pharma naptha from Germany. It is very very light. 100ml of this Naptha can evaporate off in about 15 minutes. I guess the properties of my naptha are quite different to VM naptha which the US guys are using. VM naptha also contains a lot of other solvents like Hexan

Thats why I made a 7th pull with Xylene which yielded about 400mg red jungle acetat

The only positive thing with my naptha is the quality of my crystals. I can do 3 hot pulls and the crystals are totally white and clean. And its pharma grade

 

[null24]

Those are beautiful xtals, perfect!
No, I've never seen that. I've seen precipitate at room temp, yes, but like you said not like that. More like clumpy wax that settles out, not 2 or 3 perfect representations of DMT crystals stuck to the side of my vessel.

I think you're probably right about the naps lighter property being the culprit. IDK, it's pretty.

 

[FranLover]

So cool!

 

[just999]

Thank you guys

Maybe I keep this thread alive. I have so much Naptha left... I ordered a huge amount before I started to do Jungle extractions only. I will do some more research on this. Just for fun ^^ Lets see what kind of room-temp crystals I can grow with some cleaning and pre evaping :lol:
PS: I found some pictures of the final result on my phone. Maybe I will share them too. They´re looking really nice. The best ones Ive ever had

 

[downwardsfromzero]

Might be true. But still surprising because slow evaporation would have made a "ring" on the glas and not this concentrated crystal.

The use of plastic film to cover the beaker has helped to prevent this by keeping the area above the liquid solvent saturated with solvent vapour. Of course, slow overnight cooling coupled with (visible) dust as nucleation points will also have been a major contributing factor in the formation of these rather handsome crystals.

 

[Nereus]

You know what puzzles me? Rendering "red jungle acetat" pulled with xylene... how does one perform that process, I wonder?

 

[just999]

What do you mean with rendering?

You can do a simple sodium carbonate conversion using a little bit hot water to dissolve the jungle acetat. After this use the sodium to make a paste. It will form hard rocks... brake them up...let it dry until totally dry.... powderize it... and pull with 99,9% IPA or dry Aceton.

Eveporate this and it will leave nice brwon xtals

 

[Nereus]

What do you mean with rendering?

You can do a simple sodium carbonate conversion using a little bit hot water to dissolve the jungle acetat. After this use the sodium to make a paste. It will form hard rocks... brake them up...let it dry until totally dry.... powderize it... and pull with 99,9% IPA or dry Aceton.

Eveporate this and it will leave nice brwon xtals

I am familiar with the conversion method of salts to freebase.

What I did not understand was how were you able to pull dmt acetates out of a basic (alkaline) aqueous plant mix?

Technically and practically that is impossible.

Maybe I had not read the entire post correctly, thus the misunderstanding, but judging by one of your earlier posts I'm led to believe otherwise.

I made a 7th pull with Xylene which yielded about 400mg red jungle acetat

Not trying to sound weird, I just thought this post needs some clarification if you feel up for it.

Congratulations on your nice crystals, by the way!

 

[just999]

Ahh sorry. I thought it would be obvious that I salted out with Vinegar if I am talking about Acetat. So yeah I did 2 hot vinegar pulls on my 7th Xylene pull. At the moment I am waiting for the IPA to evaporate. Lets see how much it yiels after this conversion

 

[just999]

Mama look at me I did it again







2x 50ml naptha pulls on 100g MHRB. Crystals habe been formed after one night at room temperature. The glass was wraped with one layer of plastic foil

 

[Th Entity]

Its not good idea for your mama to have account in a forum where you share the results of your illicit activity, i dont think your mama will be proud, at least mine wouldnt.

This is nothing special, unique or magical, it's quite honestly a newbie mistake.

From the very beginning of this post i already knew that your Naphtha contains mostly low boiling point hydrocarbons - pentane, hexane. Then i read those posts of yours which proved my guess:

Maybe I need to say that Im using pharma naptha from Germany. It is very very light. 100ml of this Naptha can evaporate off in about 15 minutes.

I think your Naptha is mostly pentane and hexane, this is why you couldnt dissolve the DMT at room temp, aliphatics dont dissolve indoles at room temp very much thats why its suggested to use heat when using aliphatics as extraction solvent. They dont dissolve DMT very much at room temp but they do at higher temps which makes them perfect candidates for re-x solvent. The main requirment for a re-x solvent is for the solute to have:
-Minimum/low solubility at low temp
-Maximum/high solubility at high temp

So why the DMT precipitated at room temp?
When you added your low boiling point naptha to the basified mix and you stirred/heated the two phase system, the solvent starts collecting the freebase DMT, if you left the solvent stirring/heating for too long in the two phase system in open container undoubtedly some evaporated, in this case enough evaporated to almost saturate the solvent, and when you transfered the warm solvent to room temperature within few hours the DMT was precipitating as the solution cooled (I bet if you leave the solution in a beaker close to its volume without anything to cover it the precipitation will be even faster, but that will be crude precipitate, small crystals, lower purity) this happened because generally solutes are more soluble in warm solvents than cold solvents, so if you have saturated DMT/Naptha solution at higher temp, as soon as the temperature starts to drop, the solubility of the DMT in the solvent starts to drop also, so your solvent becomes super saturated and cannont longer hold the DMT within the solution, in the presence of nucleation sites the crystals precipitated/crystallized out of solution. Actually what you had was a close to perfect ratio of solvent/solute for recrystallization.

If you get a solvent super saturated with solute you can see the crystals precipitating out of solution within 10-15 minutes instead of hours at room temp(if there are nucleation sites), hell..even if you transfer super saturated solution from hot glassware to cold glassware you will get instant precipitation.

It is not even a little bit conentraded. It was sitting like 15 hours and formed crystals at room temperature....

Are you sure about that? :lol: you indeed concentrated it in the extraction process due to the solvent low boiling point and the heating/stirring.

I had to heat the NPS in a water bath to make it ready for freeze precipitation. So I putted it into the fridge (after pre evaping). About one hour later I got huuge islands of crystals

If you had placed it directly into the freezer you would have gotten bigger crystals, instead you basically crashed it out instead of crystallizing it.

This was the last time I am using Naptha. It cant even dissolve DMT at room temperature. I covered the crystals with 150ml more Naptha, shaked and waited for about an hour and nothing dissolved. The only positive thing with my naptha is the quality of my crystals.

Yea pentane/hexane, aliphatics in general dont only have hard time dissolving the freebase DMT
at room temp but the impurites also so yes..you can expect nice white crystals.
Try using Heptane, it won't evaporate as easily during extraction unless you heat the two phase system to 80-90 C.

 

[mickster003]

Just wanted to share this pic from Swim

Left is from freeze precipitation and the right
Is from the remaining naptha reused three times
Then evaporated

 

[just999]

Thanks for this great explanation. I didnt know that I use Naptha with high proportion of Hexane.
These all make sense to me.

If you had placed it directly into the freezer you would have gotten bigger crystals, instead you basically crashed it out instead of crystallizing it.

I dont think so. The freezer would have crashed them out much faster. As you already said above. Dropping the solvent into a cool evap dish would have crashed out the crystals instantly.

I never heat my 2 phases. I only heat up the Naptha a little bit and drop it in the cold basic mix.
Heating up the whole mix will give me yellow crystals.... I prefer 3 cold Naptha pulls and after this 3x D-Limonen to pull out the yellow stuff to make Fumarat with FASI


I was planning to buy some Hexane for recrystalisation. I think now I dont need to buy it anymore when you are right

 

[Th Entity]

You are wrong again.
If i understood correctly, you had 3 pulls (with total volume of 150ml) in Xml container covered with foil and for 15 hours the DMT crystallized out of solution at room temp and you heated the solvent to redissolve the crystallized DMT back into solution prior freeze precipitation, depending on the size of the container and the fact that it was covered it took the solution more time to cool down to room temp, and thanks to the ratio of solvent/solute (near perfect for crystallization) the crystals started slowly forming as the solution slowly cooled, yielding bigger and purer crystal formation, at this point if you placed the Xml container with the crystallized solute/solvent mixture in the freezer you would have crystallized (more/the rest) of the DMT, instead you heated the container to remelt the crystals back into solution and then placed the Xml container containing the solution in the freezer which caused the solute to rapidly precipitate instead of crystallize, yielding smaller and less pure crystal formation. Not to mention that you probabbly further reduced the volume of the nonpolar when you heated the crystallized solute/solvent mixture.

What i suggest is for you to familiarise yourself with Crystallization/Precipitation, Recrystallization and Saturation and Super Saturation and read/learn more before you make a claim.

As you already said above.

- Dont use this term, i know what i said, im not sure you understand what i say, and im not sure you make difference between different definitions in chemistry.

I never heat my 2 phases. I only heat up the Naptha a little bit and drop it in the cold basic mix.

It doesn't matter a lot, how/when it happened, it happened. Obviously!

P.S. - Its MUCH more complicated than that and i cant explain everything here, i probably missed to point out something, but thats ok because the information you provided in your intial post was unclear to begin with and one cannot expect to obtain clear answear from unclear question/claim.
Make sure your future posts are more clear and provide as much information as possible regarding your problem, without ruffling too many feathers.
Good Luck
:thumb_up:

 

[Jees]

...I was planning to buy some Hexane for recrystalisation. I think now I dont need to buy it anymore when you are right

I tend to believe the same :thumb_up:

 

[just999]

Sorry for not talking to clearly . My English is just horrible. That´s why I try to make it short... I thought it would be better than a big text with a lot of mistakes . Noone like to read that.

instead you heated the container to remelt the crystals back into solution and then placed the Xml container containing the solution in the freezer which caused the solute to rapidly precipitate instead of crystallize

Yes that would be embarrasing... I didnt explain it correctly.

I heated the solvent after the 6th pull. That means 150ml more were added after taking this picture from my first post. I had to reheat it to dissolve the crystals. Otherwise I wouldt have been able to do the sodium carbonate wash. After this washing step the clear room temp. Naptha was transferred into a new glass vessle. Ofcourse I put this into the refrigerator before freezed it. And yes it didnt crashed out instantly but formed very big fluffy clear crystals over the night.


I know all of this sounds very unexciting now... Before your post I didnt know that I am probably using Hexane. And it was the first time that I used this kind of tek. It also was a new MHRB source. I never have been able to though that 150ml solvent would be saturrated enough to perform such a kind of crystalisation. Not with these impurities.

 

[Th Entity]

Sorry for not talking to clearly . My English is just horrible. That´s why I try to make it short... I thought it would be better than a big text with a lot of mistakes . Noone like to read that.

Indeed no one like to read unclear, misinformational long texts, you are correct.
By the way, English is not my first language either, i don't accept this as a justification for someone to write posts like that.

I heated the solvent after the 6th pull. That means 150ml more were added after taking this picture from my first post. I had to reheat it to dissolve the crystals. Otherwise I wouldt have been able to do the sodium carbonate wash. After this washing step the clear room temp. Naptha was transferred into a new glass vessle. Ofcourse I put this into the refrigerator before freezed it. And yes it didnt crashed out instantly but formed very big fluffy clear crystals over the night.

And

Even after 3 more pulls (they were totally covered with Naptha) and some shaking the crystals did not moved. I had to heat the NPS in a water bath to make it ready for freeze precipitation. So I putted it into the fridge (after pre evaping). About one hour later I got huuge islands of crystals... Ive never seen this before....

Now you say that to the 3x pulls (total of 150ml) you added another 150ml then you reheated to dissolve the crystals that precipitated during the 15 hours to make a Na2CO3 wash, then you placed it into the fridge then into the freezer. Ok, earlier you said you had 3x pulls (total of 150ml) and then you decided to heat the NPS in a water bath to dissolve the crystals to make it ready for freeze precipitation. And YOU said this:

I prefer 3 cold Naptha pulls and after this 3x D-Limonen to pull out the yellow stuff to make Fumarat with FASI

Sniff..sniff, smells like trimethylamine. (low conc. trimethylamine to be exact)

:lol: :lol: :lol:
:!: i am done here, i cannot continue this madness. I was going to make this post longer with explanations, however i don't want to continue to waste my time trying to explain things that have already been beaten to death. Again its not as simple as you say/think it is and its not as simple as i try to explain it to be. You are changing your statemets from post to post, you leave your audience guessing and your writing is unclear and misinformational. Good luck, if not something else, i hope you atleast learned something from me. If not then i wish you the best.
Cya buddy!

 

[Th Entity]

Please, dont take it personally, i have issues at the moment and i am in a bad spot you have nothing to do with it and i apologize for my tone and rudeness.