official extraction help thread

[psilocybin]

Any questions or problems you may run into during an extraction can be asked to get other members input in this thread.

 

[drpotato]

to reiterate something in my big wall of text; many people inadvertently just use distilled vinegar as their only source of water, and totally bypass the use of home tap water, or use so little it never has any impact. unlike adding too much lye, theres no consequences in using too much vinegar.

also, maybe get a test tube and shake the heptane with water and a single grain of lye to alkalize it, and without, and just get an idea of how its behaving

 

[Transform]

to reiterate something in my big wall of text; many people inadvertently just use distilled vinegar as their only source of water, and totally bypass the use of home tap water, or use so little it never has any impact. unlike adding too much lye, theres no consequences in using too much vinegar.

also, maybe get a test tube and shake the heptane with water and a single grain of lye to alkalize it, and without, and just get an idea of how its behaving

Test tubes are so underrated!

Get a test tube rack as well though
But yes, diluting the vinegar is kind of helpful, indeed. There's no real point in adding more than a 1:1 molar ratio of acetic acid for the DMT, so the rest of the liquid volume might as well be water - otherwise it's largely a waste of lye when neutralising the excess of acid.

If the lye, heptane and water all behave themselves, it might be a batch of bark with a higher than usual content of saponins, or similar.

 

[Pyramids]

a few things cause emulsions, you can get it because something is disrupting the barrier between phases, like an emulsifier, anything can become one of these but, if your material seems kinda foamy that could do it. Otherwise, if the phases are too similar, one reason excess lye is advised is its affinity for water is so great it crashes other things out, but its also just endlessly soluble and results in potentially, extremely dense water, this is half of why overbasing is done, besides reducing solubility of literally anything else and altering the charge on the water, it also just straight up makes the water much denser, a barely ph14 alkaline sodium chloride brine will perform similarly to like, 10% lye solution in many situations. the greater the density difference the more rapidly you should see seperation occur.
instead of something interfering with surface tension via some weak surfactant, something that can occur is physical emulsifiers, which need only be very fine particulates. calcium silicates and fluoride precipitates can cause this, basically just common stuff in your tap water. they form annoying precipitates that dont go away once they form, they show up looking like a waxy skin that wraps around the smallest bubbles of your solvent, and they kinda flake away a bit once things do settle. what they are is just solvent wicked around particulates too small to interact with the main volume of solvent, so they stay trapped floating in the water. these can be avoided by using demineralized water. if you have copper in your water, it interacts with calcium and soluble silicates to form the absolute most annoying form of calcium silicate, sulfate, or perhaps just silica, imperceivable quantities of this will clog a vacuum filter.
the lack of seperation may resolve if you add a bunch of salt, just make sure its not pool salt that contains calcium or magnesium, or else youll get a bunch of precipitate. its handy to keep a bottle of salt slurry on hand, full of a saturated brine, it makes the water more dense and adding it can do things that may give insight, like crashing stuff out, or settling at the bottom and clarifying the solution there indicating a density problem, or running tests in a test tube.

if you go with a quicklime base method, you can use calcium chloride to saturate your solution.


a hot bath is needed to get heptane to dissolve your DMT, heptane is a poor solvent for DMT, which is kind of the point. this is why i dont use naptha or hexane anymore for my initial pull, it has to actually be hot or else it wont do very much. a long contact time will more than make up for a lack of stirring though. and the hotter it is, the more it will seperate, this is almost universal in fact, most things that emulsify in water will seperate when heated close to boiling.
Its probably fine to just shake it like crazy into danger-milk while warm, but not so much vapors present a pressure problem, then put it in a hot water bath at 60C or whatever is recommended for heptane, and once it seperates, thats probably going to pull most of it. if your vessel permits, actually pushing it past 80 or almost simmering with a quick stir at the end, would be ideal.

to avoid the hot bath, use a solvent DMT is actually soluble in. toluene, DCM, chloroform, ether, maybe ethyl acetate but you need to salt it and be really gentle with basifying (sodium/potassium carbonate) or youll hydrolyze it and end up with ethanol, limonene, xylene, and if you salt the living daylights out of it, even acetone and isopropanol have precedented phase seperation, though thats highly experimental, and not neccesarily as applicable to a DMT wet process, dry maybe, but not wet.

using other solvents, you then end up with oil or goo that must be dissolved in hot heptane after the solvent is removed, and recrystalized. ideally it ought to be mini AB'd as this will fix any polymerization that occured, and in the case of DCM/chloroform, you might want to defat it first. unless exceptionally pure, DMT wont crystalize out of anything its VERY soluble in, or may struggle to. So thats the tradeoff, two extractions, granted the second one scales down to like 50ml or something, otherwise you have to deal with hot hex/heptane.

if you have a test tube, try experimenting to see what salt and heat does to the seperability after violently shaking it. similarly, what effect demineralized water has. PS, distilled vinegar used as your sole water source satisfies this too.

gratitude for the reply, drpotato!

I've been reading all over the nexus that heptane pulls at room temp, not actually the case?

I think i'll just go with the hot bath method if you think that might result in some usable goo.

 

[Pyramids]

Can you show us the labels of both your heptane and your lye? Your situation sounds like there's some kind of detergent effect involved somewhere.

One more thing - what kind of water are you using?

Thanks, Transform. I am using distilled water. There's more info on the heptane here.

 

[Pyramids]

to reiterate something in my big wall of text; many people inadvertently just use distilled vinegar as their only source of water, and totally bypass the use of home tap water, or use so little it never has any impact. unlike adding too much lye, theres no consequences in using too much vinegar.

also, maybe get a test tube and shake the heptane with water and a single grain of lye to alkalize it, and without, and just get an idea of how its behaving

I ended up with 650ml distilled water (as per Cyb's tek) + 60ml vinegar and 50mg lye. I then added another 300ml distiled water and 20g lye (when the heptane refused to rise).

Somehow the hot bath failed as well... 0 separation after several hours at 70c

 

[Transform]

Thanks, Transform. I am using distilled water. There's more info on the heptane here.


View attachment 109087View attachment 109088

Well - that all looks fine. Is it the same batch of bark as the previous, trouble-free extraction with naphtha?

What about trying with adding a bit more heptane? Sometimes the bark will "eat" a bit of solvent to start with.

 

[Pyramids]

I ended up with 650ml distilled water (as per Cyb's tek) which included 60ml vinegar and 50mg lye. I then added another 300ml distiled water and 20g lye.

Well - that all looks fine. Is it the same batch of bark as the previous, trouble-free extraction with naphtha?

What about trying with adding a bit more heptane? Sometimes the bark will "eat" a bit of solvent to start with.

Yeah, same batch of MHRB.

So, I ran another batch of Cyb's Hybrid ATB tek today after picking up some naptha and everything is working as it should. I'll freeze some pulls tonight but everything has finally gone according to plan, which indicates that something was getting thrown off by that particular batch of heptane. Frustrating as hell, but ultimately happy to have solved it.

Regarding the previous batch, I will add some more heptane to it, thanks (unless I should add naptha?)

 

[Transform]

Regarding the previous batch, I will add some more heptane to it, thanks (unless I should add naptha?)

If you try heptane first, and it still doesn't work, there's always the option of adding naphtha afterwards. Then again, the naphtha might be the secret sauce here - if this aspect of the puzzle really interests you, splitting the extraction in half and trying with one or other of the solvents in its own portion would be another way of going about it.

Then there's this:

Thread 'A fix for emulsion(?) Seemed to work for SWIM!'

Jul 31, 2011

Swim had emulsion in a lye/Naptha extraction. With little patience he took the turkey baster and sucked the emulsion up and instead of discarding it, he stuck the emulsion filled turkey baster deep into the mhrb/water/lye mix and squeezed the bulb very slowly until it was emptied. Naptha rose to the top and mhrb/lye/whatever that made up the emulsion was gone. swims turkey baster has an injection needle on the end of it. The needle has been ground flat and crimped into a slit because swim found that the slanted head of the needle let air go in while transferring pulls to an empty jar...

• DimensionlessBeing
• Replies: 15
• Forum: FAQ Q&A

And maybe a few more results from searching "break+emulsion"

Search

forum.dmt-nexus.me

 

[drpotato]

i find emulsions break much quicker when theres already an established layer or mass of solvent, otherwise micro-beads will struggle to overcome one anothers surface tension and merge.
sucking emulsion through a vacuum filter is always a god tier solution though. the hand pumps used for brake line purging are the best ones ive encountered. i recommend using a nice flat buchner however you get one, with the cheapest purpose built fast filter paper disks, but then with a rubber gooch, they come as a set of concentric rings. you can also put a normal funnel with a cotton plug in them, and gently get results that way as well.
dont get the fritted glass ones, they look fancy but you cant really wash them, esp for stuff that is insoluble like calcium precips, they have specific utility which isnt applicable here.

 

[Pyramids]

i find emulsions break much quicker when theres already an established layer or mass of solvent, otherwise micro-beads will struggle to overcome one anothers surface tension and merge.
sucking emulsion through a vacuum filter is always a god tier solution though. the hand pumps used for brake line purging are the best ones ive encountered. i recommend using a nice flat buchner however you get one, with the cheapest purpose built fast filter paper disks, but then with a rubber gooch, they come as a set of concentric rings. you can also put a normal funnel with a cotton plug in them, and gently get results that way as well.
dont get the fritted glass ones, they look fancy but you cant really wash them, esp for stuff that is insoluble like calcium precips, they have specific utility which isnt applicable here.

Cool! will try it out, thanks. I had some luck yesterday on a different batch using my magnetic stirrer (rather carefully), sucked the emulsion right into it's vortex portal.

is the tek that you generally follow available to view somewhere? or is it more advanced science that I likely wouldn't comprehend...

 

[habitualexplorer]

Hey all. I have a few questions I'm hoping to get some help with. I have so far attempted 'Cyb's Hybrid ATB Salt Tek' twice with powdered Acacia Acuminata of the narrow phyllode variety. These were the conditions for each run:

Run 1: Everything followed explicitly except instead of using Naptha right away, I opted for Xylene and carried out two pulls, and then merged both pulls with vinegar/water, which has since been basified and I intend to carry out Naptha pulls on it as per the tek guidelines soon.

Run 2: Followed cyb's tek to the letter, only I decided to blend the already powdered AA even further, resulting in a substantially finer material.

Questions concerning Run 1:

1-1: Upon adding xyelene, I noticed almost immediately a large amount of crystals forming between the base and xylene, sitting in their own plane right above the interface of the base/solvent. How much, if at all, would this have been with DMT? I suspect the xyelene was so effective at pulling that perhaps either the DMT or other alkaloids had no option but to crash out at the warm temperatures of the liquid.

1-2: Building upon the previous question, it was impossible to pull the crystals without disturbing the base layer, but I didn't want to leave them in the event it was DMT crashed out in solution, and therefore I scooped them up (and surely some base product too) after the xylene pulls, added it to a dish and left to evaporate, leaving behind what you can see in the images below. Assuming there is valuable substance in there, I intend to recrystallize as per the final step of Cyb's tek using just heated naptha, or would a mini A/B be more appropriate?


Unscraped Scraped

1-3: When transferring the xylene to the water/acid mix, I used the same ratios in Cyb's tek (200ml water/60 ml vinegar), however I did it in 3 stages, adding the entirety of the xylene each time to 1/3 of the water/acid mix, mixing, separating and pulling. I did this all quite quickly, only allowing the xyelene to separate once after a good roll each time. Furthermore, the addition of the xylene to the acid/water mix again resulted in the formation of a defined crystal layer, which was also extracted after the clean xyelene, and added to the pan to evaporate as per question '1-2' above. So my question is, should one spend a lot more time mixing the xyelene and acid/water mix and allowing to separate multiple times, or does the uptake of alkaloids into the acid/water mix occur quite quickly?

Questions concerning Run 2:

1: I believe I have an emulsion, and I believe it might be because I powdered the product far beyond what is required, allowing tiny particulate matter to cling to the solvent. After adding 50ml of Naptha, I was only able to get about 20ml out, and I noticed a distinct band of particulate matter directly below the clear band of naptha. Based on the image below, would you agree? I have tried adding more water/lye, additional salt, and am currently attempting a vibrational separation with the bottle atop the washing machine on a spin cycle, no success so far. If no luck I will attempt to filter the particulate matter and continue.






Apologies for the long-windedness.

 

[Transform]

1-1: Upon adding xyelene, I noticed almost immediately a large amount of crystals forming between the base and xylene, sitting in their own plane right above the interface of the base/solvent. How much, if at all, would this have been with DMT? I suspect the xyelene was so effective at pulling that perhaps either the DMT or other alkaloids had no option but to crash out at the warm temperatures of the liquid.

There's no way that crystalline DMT would crash out of xylene even at freezing temperatures, let alone at or above room temperature. DMT is way too soluble in xylene for that to happen. There might be the slenderest chance that crystallisation occured from out of the water, but I'd be 99.9% certain that it was something other than DMT. What exactly, it's foolish to speculate in absence of an actual sample, or at least a decent close-up photo of the material.

1-2: Building upon the previous question, it was impossible to pull the crystals without disturbing the base layer, but I didn't want to leave them in the event it was DMT crashed out in solution, and therefore I scooped them up (and surely some base product too) after the xylene pulls, added it to a dish and left to evaporate, leaving behind what you can see in the images below. Assuming there is valuable substance in there, I intend to recrystallize as per the final step of Cyb's tek using just heated naptha, or would a mini A/B be more appropriate?

Either will do - I'd suggest the former, as what you've collected seems unlikely to be of further interest, therefore making it undesirable to expend unnecessary effort. Also, in future it might be wiser to keep those isolate fractions separate, just in case they're not of the same composition, i.e. -

the addition of the xylene to the acid/water mix again resulted in the formation of a defined crystal layer, which was also extracted after the clean xyelene, and added to the pan to evaporate as per question '1-2' above.

should one spend a lot more time mixing the xyelene and acid/water mix and allowing to separate multiple times, or does the uptake of alkaloids into the acid/water mix occur quite quickly?

The transfer of DMT freebase from the xylene into the acidic aqueous phase occurs via proton transfer at the interface between the two liquid phases, so a continuous rolling action for a minute or two will maximise that area of interphase contact while (hopefully) preventing emulsions.

I believe I have an emulsion, and I believe it might be because I powdered the product far beyond what is required, allowing tiny particulate matter to cling to the solvent.

Your inference here seems likely to be correct, unfortunately.

I have tried adding more water/lye, additional salt, and am currently attempting a vibrational separation with the bottle atop the washing machine on a spin cycle, no success so far. If no luck I will attempt to filter the particulate matter and continue.

You may indeed have to make your best attempt at separating the dirty xylene and then filtering it - but it may prove easier to pull straight from the dirty xylene into acid and filter the acid back-pull instead. The acid phase might separate more readily from the xylene than the basic one does; this is something that you'd do well to check out at the test tube scale first.

Apologies for the long-windedness.

No worries - rather a thorough and well-considered line of questioning than a series of brief, ill-defined grunts.

 

[drpotato]

Cool! will try it out, thanks. I had some luck yesterday on a different batch using my magnetic stirrer (rather carefully), sucked the emulsion right into it's vortex portal.

is the tek that you generally follow available to view somewhere? or is it more advanced science that I likely wouldn't comprehend...

i dont really do teks. i did them starting out to get a sense of what was happening, but mostly just because with processing plant material its substantially an art in addition to science. the fine details of DMT forming crystals or some nuanced behaviours like with FASA are a bit tricky, as is the processes that involve solids, which is why i always strain my acid soup and thoroughly filter it. But the overall chemistry is pretty simple, its a poorly or usually under the circumstances insoluble base, and extremely soluble salt, and that is exploited to migrate it between mediums, which are also tuned to be selective. almost nothing but DMT migrates under the circumstances (fats dont form salts for example in acid).
magnetic stirrers can help a bit, as long as its not stirring so hard that it can pull solvent out of the layer that forms. and depending on the emulsifying agent involved, there might not be any amount of stirring you can do.
a vibrator is moreso what you want, i use one on my seperatory funnel sometimes, but lately i found that it might be better to custom build something that uses a solenoid fed a pulsed signal, because then i have control over the stroke distance in addition to frequency, wheras a rotary vibrator motor has a fixed stroke (shaking distance). sometimes ultrasonic helps, but it can as easily cause a dispersion too, into literal DMT petro-milk. Once when i did FASA all i got was instant milk, i think i uploaded a video once though where i put it in an ultrasonic bath and about 60-80% of it all instantly congeals into a blob of oil/goo, but a lot of it simply did not, its not a consistently useful option, but it has its moments.

a method that ive seen done to good effect is called something like, a bibbler, which involves using a peristaltic pump to pump warm solvent into the bottom of a vessel, where it rises up to the top. this is done for a day or two and is done instead of shaking. since the droplets never disperse theres no problem with emulsion, and the pump can handle solids to a degree, but i think you gotta use sodium or potassium carbonate instead of hydroxide, and that means your bark will probs have to be freeze-thawed to open up fully, the benefits of hydroxide over carbonate are pretty much only micromechanical in nature. that and carbonate makes things all foamy so it cant be used with acid, or you need to neutralize the acid from a prior stage using a minimal amount of hydroxide, or other basic salt