Sure I'll post pics of the full vacuum/ultrasonic chamber set up in a little while, tbh I didn't do anything to the actual ultrasonic tank itself and it's just a regular 6L one from harbor freight, basically identical to the vevor one too. Surprisingly enough it can hold full 29 inhg vacuum without the tank imploding on itself, and the lid flexes a little but still holds vacuum and that's after I cut a 4" hole out of the center for a sight glass lol. Will update with pictures a little later
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TEK impatient mans high yeild high purity STB extraction (mimosa hostilis root bark)
- Thread starter g2x666
- Start date
This topic contain a TEK
Here is some pics of the vacuum chamber set up. Basically just cut out a hole for a sight glass, used 3m window weld (used to install windshields on cars, shits amazing basically urethane paste but once it dries it does not come off, and is structurally very strong) and put a port for the vacuum line with a ball valve and quick connect so I can pull vacuum and unhook the pump, and then put another port for a vacuum gauge and I added a little valve to release the vacuum. I used random shit I had laying around the house for all of it, fittings and all that was stuff I've collected over the years. I put rubber washers that I bought from some hardware store and washers on each fitting to sandwich the rubber washers against the lid to make a air tight fit. For a gasket I used this dental mold making shit I acquired from a friend that's hella expensive so I wouldn't recommend, any sort of silicone rtv would work I would just rub some oil onto the tank and let the rtv skin over before squishing the lid on to set the shape. Fairly simple but getting it to have no leaks did prove to be a bit of a struggle at first lol. I also made a few jar lids with the quick connect and ball valve on top too so I can vacuum purge heptane just out of a jar without having to use the tank.
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That is a ghetto build lol. I'm impressed, but those adhesives and sealants have gotta be susceptible to heptane vapors. The gaskets in the pump itself are surely susceptible to heptane vapors, so this will be an interesting experiment how long the pump lasts doing this.
Ultrasonic passes through glass. I don't think researchers are actually rawdogging their reactions in the ultrasonic basin. Usually people just place their vessel in the bath.
Ultrasonic passes through glass. I don't think researchers are actually rawdogging their reactions in the ultrasonic basin. Usually people just place their vessel in the bath.
That's unheard of. Even over 3% in the study is suspicious. Keep in mind they were only using 5g samples. One theory is they selected the perfect layer of bark and it would be pretty easy to do that with 5g vs 100g. Their sifting technique also could have concentrated desirable particles.
As far as I can tell, the rotovap was only used as an analytical tool to quantitatively separate the solvent from the solute. It's a repeatable way to get a measurement, would be good for g2x666's 10+ batch experiment. But if you don't need that kind of data, it's not necessary and certainly doesn't increase the yield.
Yeah I have been playing around with different ways to do it. The lye doesn't bother the gaskets or stainless, and I don't do anything vacuum with heptane in the ultrasonic tank. Also the last vacuum pump I had ran nitric acid fumes ( nitrogen dioxide, Instantly rusts any steel on contact) through it quite a few times and the actual electric motor took a shit before the pump ever failed. I'm not worried about some heptane tbh. It definitely is a little ghetto tho lmao but that's just me messing around with shit I have on hand for the time being, once I have it figured out how I want it I'll get new parts and do it properly (probably after this set up fails). Also there are no real.gaskets inside this kind of vacuum pump, just the one that seals the oil from leaking out really. They use little plastic pieces that slide in and out while the shaft spins inside of an eccentric circle, the pump itself is surprisingly durable. It's the motors on these things that tend to shit out. But it was 50 bucks on temu lmao so I'm not worried, plus I'll just rebuild it when something does break.
On a side note I did get my rotovap set up but had to make my own sealing tube that covers the spinning glass tube so it's also a little ghetto lmao but hey as long as it functions properly I'm happy. Gonna use my ultrasonic cleaner as the water bath and have a ultrasonic rotovap lmao it'll be an interesting experiment also
This is what I've been using for the heptane and naptha evap, and I use anther jar for a cold trap before it hits the pump (not cause I'm worried about the pump mostly cause I want to reuse solvent lmao). And just for fun a picture of my rotovap with the basic vacuum distillation set up hooked up to my ghetto but surprisingly functional receiver tube. If you can't tell I just kinda like building shit (professional welder/ Fabricator) so experimenting with various tools and equipment is as much fun as smoking the spice for me lol. And I use shit I already have as much as possible, hence the homemade tube instead of paying 400 for the glass one off eBay. 165 bucks in all together for the rotovap and distillation kit, can't beat it lmao
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RitualOpossum
Established member
would the 3L ultrasonic cleaner be useful just to implement into any extraction tek as a step inspired from this one?
From what I can tell, when the bark is in the part of the process where you soak it in lye and are doing the naptha pulls, using the ultrasonic cleaner is definitely helping with pulling the spice out of the soup for sure. Even the stuff that I had more shredded or even chunky bark pieces I threw in are more of less disintegrated after a few ultrasonic baths
Ultrasonic probe does indeed break cell walls but they are magnitude stronger than a ultrasonic bath and also many times more expensive. I think the weakest probe is like 800 watts and that is all focus on a single probe/point not the bath.
I also use ultrasonic bath but more a means to increase extraction rate.
Ahhhh I didn't really notice the difference on that picture between the probe and bath. I will say this though, the ultrasonic cleaner is significantly more aggressive when everything is under a vacuum and submerged in water. So far the best way I can find to use it is to place jars in the ultrasonic bath filled halfway up with water, attach my vacuum lines to the jar and have it under vacuum while heating and using the ultrasonic function. Especially for evaporation it's very aggressive, I'm gonna try getting some half gal mason jars to do the test runs in coming up
Now under vacuum and ultrasonic bath I’m sure it does better since you are removing air pockets and solvent completely entering.
Be aware that higher temps reduces efficacy of cavitation. I assume you are heating to have higher solubility of the alkaloids but idk if you get much benefit. Since you have rotovac why not do cooler pulls with excess solvent then reduce down. Do like more pulls than normal and you can do mini salting to test if actually pulling anything extra.
Benzoic salting tek on here is very useful for this.
That's what I had in mind when I brought up backsalting. That instant precipitation with BASN is too satisfying and efficient not to use.
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I missed that great post! This is the page I go to for solubility info. It's not a very complete database.
Psychedelic Compounds Chemical and Physical Properties - DMT-Nexus Wiki
This paper has some solubility data
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the paper listed above shows significant differences in yield, 5 different solvents & 5 different yields. what are your thoughts on this ??That's what I had in mind when I brought up backsalting. That instant precipitation with BASN is too satisfying and efficient not to use.
View attachment 112424
I missed that great post! This is the page I go to for solubility info. It's not a very complete database.
Psychedelic Compounds Chemical and Physical Properties - DMT-Nexus Wiki
wiki.dmt-nexus.me
This paper has some solubility data
Can you quote or screenshot what you're talking about? If you mean Table 2, that's solubility in five different solvents, not yield.
Oh actually I guess it's not solubility, that is a table of yields. But they only did one pull, not an exhaustive extraction. What they yielded in one pull reflects solubility relative to each other. Basically, DCM has a higher DMT solubility than n-Hexane, so their one pull experiment yielded a lot more with DCM.
"The fact that n-hexane has the lowest polarity of all
organic solvents contributed to avoid the formation of
emulsions when combined with aqueous phase and thus it
was the highest volume of solvent separated in the final step
of the extraction. On the other hand, its low polarity
certainly accounts for the lowest DMT concentration found,
as the DMT molecule possesses an amine group that conveys
polarity to it.
Studies have shown that the solvent dichloromethane
reacts with DMT to produce N-chloromethyl–N,Ndimethyltryptamine
chloride (Brendt et al., 2008; Dunlap
& Olson, 2018). The biphasic state where dichloromethane
and aqueous solution were in contact extended over a week.
Considering these results, it is highly possible that some
amount of DMT may have been lost to the aqueous phase
during extraction, since the resultant reaction compound
described has ionic nature. Taking this into account, it is
surprising to see that dichloromethane was the solvent with
highest DMT concentration. As our samples for
analysis were dried and stored at −20 °C, we assume that
this reaction did not take place after the extraction procedure
ended."
The study left a lot of questions unanswered, since they couldn't measure the purity of the DMT or what else the solvents may have extracted. I'm a little confused myself, but I'm still pretty amateur at reading science papers.
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