Cold Solvent (Shellite/naphtha) for Extraction?

[Dimethylentity]

Alloo fellow minds!!! This is my first time posting. I have been learning from this place for a while and just love it and its inhabitants. I hope to melt right in

I figured why not open up with an idea i have in my noggin...

Cold solvent (Shellite/naphtha) seems to pick up less alks overall but is more selective towards deems..
When hot solvent is used different alks in the solvent seem to precipitate out separately if slowly cooled. Deem seems to be the last alk to precipitate out so that means the deemsters are the first (and maybe only) thing to be picked up by cold solvent... The way i see it is if the solvent is very cold then it becomes saturated with the only alks it can hold at those low temps (deems) and becomes full before it heats up enough to start absorbing the other alks..

Saw a tek video for acrb were the guy used ice cold solvent and says he reckons it binds with the dmt better.
Could what i described be the logic behind that statement or am i completely off track here?

cold acrb tek here: adds solvent at 25mins 30secondsish

Also if anyone know where part two of this tek is i would love to know

 

[downwardsfromzero]

he reckons it binds with the dmt better.

Not exactly. It's to do with the individual temperature/solubility curves for each of the compounds concerned, although the pulling temperature is still a bit of an ongoing debate.

Ensuing mindramble:

But - maybe partition efficiency even is somehow better at a lower temperature, even if the actual solubility is lower. I'm imagining how intermolecular forces between the naphtha alkanes and the DMT molecules will be varying with temperature. The optimum point could be colder than the commonly accepted value of around 45°C.

Cold naphtha will be more selective for DMT although it will be less saturated, meaning more pulls will be required for a comparable yield than in a warm extraction.

Careful observation of hot-pulled naphtha as it is chilled may help facilitate separating 'other' substances from the DMT before it is freeze precipitated. By my reckoning, no-one has reported trying this - so there's a little project for the willing to try.

A definitive temp/sol curve for DMT in naphtha is not likely to be forthcoming because of the variability of naphtha (a mixture) and the polymorphic nature of DMT.


Interesting first post, welcome to the Nexus!

 

[padawan]

Careful observation of hot-pulled naphtha as it is chilled may help facilitate separating 'other' substances from the DMT before it is freeze precipitated. By my reckoning, no-one has reported trying this - so there's a little project for the willing to try.

I've tested this a lot using Acacia freeze precips. I only use hot naphtha. The pulls are piss-yellow, indicating plant oils as expected (no prior defats at this stage, just A/B - although I've tried various defat methods and abandoned them). But here's the thing: make sure the pulled solvent is saturated by using appropriately small volumes, then a bit of fan-evapping, then once the liquid is cloudy blow directly on the solvent and you'll see the alks precipitate instantly. Stick it in the freezer for 12 hours, no longer. The alks will crystallize and the solvent will remain piss-yellow with the oils, which you can pour off (I've tested - no more alks, then you can run through an activated charcoal filter and re-use later). The oils take longer to precipitate than the alkaloids, so don't leave in the freezer for too long or they'll end up mixed in with the alks. For second and subsequent pulls, keep your previously crystallised alks in the dish for crystal seeding and before adding each pull stick it in the fridge for 10 minutes to cool and pour over the freeze-cold crystals to ensure nothing melts. Using this method I don't even need to re-ex the combined pulls unless I'm being picky.

Works for me.

 

[pete666]

When I pull heptane while doing mini-A/B after initial extraction by toluene, subsequent salting and basification, I am heating the solution to 60C. Then wait till it cools down to room temp, which clears it up. Then decant and freeze-precip. I have tried to pull with just room temp heptane, without heating and cooling down, and the heptane was far less saturated.

 

[Jambra]

"although I've tried various defat methods and abandoned them"

I've noticed Acacia sourced crystals come out very yellow without a defat, do you still get yellow crystals? One Xylene wash before basing produces clean white crystals however. Good tip on reusing the crystallising tray, I imagine this would produce bigger crystals too?

 

[padawan]

I tried defatting after the combined acetate reductions and it was just too messy and time consuming to separate. Also tried combining NP pulls back into a acid solution and siphoning off the oily NP then re-basifying and pulling, which works great but doubles the effort and I can get the same result with a simple re-x (once there is a critical mass of oils in the crystals they seem to coagulate together easily and the alks pour off leaving a film of viscous oils).

My rule of thumb now is to judge how saturated the pulls are by seeing how easily they cloud, and the density of the alkaloid cloud after a few minutes of fan evapping. The more saturated the NP pull, the fewer hours I stick it in the freezer. For really saturated pulls I only keep it in the freezer for perhaps 8-10 hours. Combined with crystal seeding, this enables the alkaloids to precipitate out very quickly before the oils begin to harden and settle amongst the crystals. So I just pour the majority of oils off with the NP once removed from the freezer. The rapid crystallisation means I only get crystal clusters of perhaps 7mm diameter, which is OK. Slower cooling would produce larger crystal structures but would also allow the oils/fats to combine with the alks. Even without a re-x the end result only has a slight yellow tinge but otherwise sparkling little goodies. One simple re-x cleans it up to very high purity, if I'm inclined.

 

[downwardsfromzero]

Excellent data, thanks padawan.

+1 :thumb_up:

 

[blue.magic]

With room temperature naphtha and room temperature soup, I get lower yield (about 0.5-0.6%) of pure white crystals.

What works for me is slightly heated soup, up to 40 °C but not more. At 45 °C too much oils are pulled out. The sweet spot seems to be between 35 and 40 °C.

The above applies to Zippo lighter fluid, 1 500 ml of concentrated filtered tea from 250 grams MHRB and three subsequent pulls: 75 ml, 50 ml, 50 ml.

Sometimes I do first pull at room temperature, then heat the soup for the next pulls.

I use distillation apparatus to reduce naphtha down to about 40 ml, which is then put into freezer.

 

[downwardsfromzero]

Blue magic, what's the boiling range of your naphtha?

I tried distilling some DMT-loaded heavy naphtha once and the DMT co-distilled. Obviously the naphtha was a bit too heavy (sold as BBQ lighting fluid - great for freeze precip, incidentally, but product needs recrystallisation).

 

[starway6]

if the puled napatha is.. [very saturated].. i find that crystals will form very quickly sitting at room temperature without using a freezer...

I just quickly pull out most of the napatha with a pipette and save it in another jar because it still has dmt and plant fats in it..

after this i tilt the vessel so it will drain the left over napatha resedue ..and at the same time a computer fan is placed in front of it drying the crystals...

ive found that with acacia confusa the poured of napatha containing dmt fats and other things will evaporate into what ive called a thick yellow honey dmt that is very powrerfull regardless of the fats in it...and this yellow honey seems to have more visual colorfull effect with strong body high..

why this yellow stuff has been more effective that the nice white crystals im not shure?

 

[blue.magic]

Blue magic, what's the boiling range of your naphtha?

Approx. 90 - 130 °C (194 - 266 °F). This is only rough numbers as last time I distilled it I used just the heating mantle's own thermometer.

The vapour temperatures taken at still head were similar.

It's the Zippo lighter fluid.

I use distillation to reduce naphtha before freeze precipitation. Of course I am concerned about precipitating from the heavy fraction but so far it works perfectly.

I am however considering heptane for further extractions as recycled naphtha loses lighter components and this will lead to less consistent results over time.

 

[padawan]

ive found that with acacia confusa the poured of napatha containing dmt fats and other things will evaporate into what ive called a thick yellow honey dmt that is very powrerfull regardless of the fats in it...and this yellow honey seems to have more visual colorfull effect with strong body high..

why this yellow stuff has been more effective that the nice white crystals im not shure?

Interesting. How do you administer the goo? liquid pad? Any side effects from the oils/fats?

And does it vaporize similarly to crystallised FB?

 

[starway6]

ive found that with acacia confusa the poured of napatha containing dmt fats and other things will evaporate into what ive called a thick yellow honey dmt that is very powrerfull regardless of the fats in it...and this yellow honey seems to have more visual colorfull effect with strong body high..

why this yellow stuff has been more effective that the nice white crystals im not shure?

Interesting. How do you administer the goo? liquid pad? Any side effects from the oils/fats?

And does it vaporize similarly to crystallised FB?

i just let the yellow creme continue to evaporate to the dryness of wax.. then cut small doses out of it and put it on top of a peice of chore boy in pipe bowl and vape it..

can be vaped other ways like on top of some herb sandwich style..

this is done without defatting with total jungle alcoloids still in the wax...

the crystal is much cleaner but it seems to take a larger pile to get desired effects but even then still not as strong as the honey dmt..

 

[starway6]

forlonger trip and best visuals [smoke some rue powder] or drink some rue tea 30 minutes before vaping the spice...!

 

[Dimethylentity]

he reckons it binds with the dmt better.

But - maybe partition efficiency even is somehow better at a lower temperature, even if the actual solubility is lower. I'm imagining how intermolecular forces between the naphtha alkanes and the DMT molecules will be varying with temperature. The optimum point could be colder than the commonly accepted value of around 45°C.

Hmmm Interesting.. Figured the curves would open up as it warms and create room for the other alks to start crowding the pull..
Definitely gonna do some experiments on the matter, will post any findings here

Good to be here. Was going nuts just talking to SWIM about this stuff..

 

[Dimethylentity]

Stick it in the freezer for 12 hours, no longer. The alks will crystallize and the solvent will remain piss-yellow with the oils, which you can pour off

Yea 10-12 hours for the "piss yellow" pulls seems to be good. Left a pull in the freezer for almost 20 hours and it spat the yellow all over the xtals and the solvent was almost clear again. Tho the pull may have been overly saturated from evaping down before freeze.
Got something else am writing up thats sorta to do with this.

 

[Dimethylentity]

why this yellow stuff has been more effective that the nice white crystals im not shure?

Had a similar experience with some yellow waxxy oil goop that was gotten from some pulls that were shaken very roughly.. I'll add some pics.

Had some of the stuff on top left (15-20mg) thinking 'hmm this is more crystaly therefore is will be more potent effects and not much happened from it. THEN had some of the diarrhea looking stuff on the bottom (again 15-20mg) and HOLY MOLY!!! It came on so hard and fast! B-e-a-utiful open eye visuals and was communicationating with the Buddha paintings in the room! Something along the lines of 'Ahhhaa i seeee what you mean! The tasty fattys and oils, OM NOM NOM NOM', then preceded to laugh like a mad man for quite some time

Judged the spice before trying it based on preconceived notions of technicalities of purity, something that will never be done again...
Seems to be a synergy of sorts with the other alks and fats.
Is that what would be considered jungle spice??

 

[downwardsfromzero]

I am however considering heptane for further extractions as recycled naphtha loses lighter components and this will lead to less consistent results over time.

Surely once the composition of the naphtha stabilises, presumably ever more towards the heavier fraction (octane/nonane, given the boiling range) things will become more consistent?

Given that you're distilling your naphtha anyhow, perhaps you could fractionate it before using it so that the composition would be more stable from the start. Then you'd have the heavier fraction for pulls and the lighter fraction for recrystallisation.

Of course, simply buying heptane would be much easier :lol:

 

[starway6]

why this yellow stuff has been more effective that the nice white crystals im not shure?

Had a similar experience with some yellow waxxy oil goop that was gotten from some pulls that were shaken very roughly.. I'll add some pics.

Had some of the stuff on top left (15-20mg) thinking 'hmm this is more crystaly therefore is will be more potent effects and not much happened from it. THEN had some of the diarrhea looking stuff on the bottom (again 15-20mg) and HOLY MOLY!!! It came on so hard and fast! B-e-a-utiful open eye visuals and was communicationating with the Buddha paintings in the room! Something along the lines of 'Ahhhaa i seeee what you mean! The tasty fattys and oils, OM NOM NOM NOM', then preceded to laugh like a mad man for quite some time

Judged the spice before trying it based on preconceived notions of technicalities of purity, something that will never be done again...
Seems to be a synergy of sorts with the other alks and fats.
Is that what would be considered jungle spice??

yup...that looks like the yellow stuff ive had and it shure is strong! i think some rue tea before vaping this stuff would tame its intensity some.. but should make the visuals nicer and the duration some what longer!

Ive never vaped honey dmt with rue yet ..but the next time i get a chance i will combine the two!:thumb_up:

 

[Northerner]

Careful observation of hot-pulled naphtha as it is chilled may help facilitate separating 'other' substances from the DMT before it is freeze precipitated. By my reckoning, no-one has reported trying this - so there's a little project for the willing to try.

I've tested this a lot using Acacia freeze precips. I only use hot naphtha. The pulls are piss-yellow, indicating plant oils as expected (no prior defats at this stage, just A/B - although I've tried various defat methods and abandoned them). But here's the thing: make sure the pulled solvent is saturated by using appropriately small volumes, then a bit of fan-evapping, then once the liquid is cloudy blow directly on the solvent and you'll see the alks precipitate instantly. Stick it in the freezer for 12 hours, no longer. The alks will crystallize and the solvent will remain piss-yellow with the oils, which you can pour off (I've tested - no more alks, then you can run through an activated charcoal filter and re-use later). The oils take longer to precipitate than the alkaloids, so don't leave in the freezer for too long or they'll end up mixed in with the alks. For second and subsequent pulls, keep your previously crystallised alks in the dish for crystal seeding and before adding each pull stick it in the fridge for 10 minutes to cool and pour over the freeze-cold crystals to ensure nothing melts. Using this method I don't even need to re-ex the combined pulls unless I'm being picky.

Works for me.

This is very close to what I do, ended up at the same place for the same reasons.

99.9% of my alks come out in 2 pulls though, the first giving >75% of the yield and the second the rest. A 3rd pull rarely gives more than a single lonely xtal. For this reason I clean my dish between the two pulls.