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Reasonable yield expectations

C

CokFLHX

Esteemed member
Hello all. It’s been awhile since I’ve been on here.

I wanted to get some opinions because I think something isn’t right.
With MHRB, the average yield is 2%, right?

For some reason I can’t figure, I am not getting anywhere close to 2%.
In my last extraction, I did 400g of bark, in four 100g chunks if you will. Basically I do it 100g at a time, but I’ll do two to four of them at once.

I like to do do a A/B. I don’t measure amounts, I adjust for pH. Before I basic, I like to filter the bark material out with cheesecloth. I call it a run. I’ll filter out the bark, and that’s one run. I usually do three runs, with three pulls on each run.

With 400g total MHRB, my yield is only 1.5g.
I should be getting AT LEAST 5g out of 400g, correct? Or could the bark not be the best or something?

The way I extract, is to powderize the bark, then I make an acidic solution from RO water, with hydrochloric acid added until it reaches a pH of 2-4. About 250-300ml per 100g of bark.

I then do three freeze/thaw cycles of the acidic bark slurry. After the third thaw; I filter it through a cheesecloth, squeezing out all the liquid I can before putting the solid ball of bark into another jar and adding more acidic solution for the second run.

After filtration, I dissolve 50g of salt in 100ml of RO water, and add it to the extract.
Then I add lye to 200ml of RO water until it reaches a pH of 12 or higher, and add the base solution to the extract until the pH measures 12. Mix vigorously. Then I add 75ml of Heptane for the pull.


Is there something screwed up or wrong with this procedure? Why am I getting such low yields?

The first run yielded 1.5g the second run yielded .5g, and I haven’t finished the third run yet. However usually the third run doesn’t produce much at all.

Can anyone shed some light or give some advice on this?

Thanks for your time.
 
I have read that not all MHRB is equal. Maybe you happened across a low yielding batch.

By doing 100g batches you've made the volume a more manageable size, but since you're performing them simultaneously with identical methods you got the same results for each. You jeopardized 400g before running a smaller test run.

I don't have years of extractions under my belt, but one difference I noticed in your method from the ones I've done is that my bark came pre-ground to almost dust and I did not filter it out of the soup before the NPS pulls. So, perhaps you should have ground your bark finer and/or left it in the soup instead of filtering it out.

After rereading your post, I didn't see you mention using any heat. I used a hot water bath (140-160 f degrees) throughout the process.

Did you keep the MHBR that you filtered out? If so, you could try again using heat & leaving the bark in during the basifying & the NPS pulls.

More experienced folks may chime in with tips other advice.
 
Aside from the possibility of poor yielding bark, here's a few thoughts:

You have adopted a method of freeze-thawing bark in acidic solution.. while on the one hand this effectively will break the bark down, I suspect the solubility of DMT HCL in near frozen water is a fair bit lower than boiling water. I think you have a good idea here with the freezing of material in solution, however I would go the extra step and boil it after it has thawed. Simply allowing it to thaw and then straining off the liquid very likely isn't going to effectively pull alkaloids.

Realistically you would be much quicker and just as thorough to do 3 X 1 hr simmers/boils. Even throwing in a fourth would still be quicker than freeze thawing 3 times over.

Hopefully you've not thrown out your bark and you can simply simmer it in acidic solution for an hr to see if there's stuff left over. If that doesn't get anything more out then your bark is probably low yielding.

Is your heptane/base mixture warm? If you are adding your lye to recently thawed solution, it may not be warming it to the required temp for efficient heptane solubility of DMT. Cold heptane will not produce as much as warm/hot.
 
I mentioned in the original post that I strain the bark and run the extract, in the first run, after three pulls, I had a net yield of 1.8g from approx 400g of bark.

First pull of second run did better than I expected with a yield of 1.6g.

So instil have two more pulls on run 2, and then 3 pulls on run 3. Hopefully, I was too hasty with my post and I’ll have a better yield than I expected.

With 400g of bark, I should end up with at LEAST 6g total yield, correct? That would be 1.5%. I will be sure and update the thread when I’ve extracted all I can.

As far as my methods:
I usually warm the solution in a heat bath, but for some reason I had the idea that too high of heat, as with boiling, would be detrimental or destroy the spice. I don’t know where I got that idea, but I’ve always been careful not to let any part of the extraction get hotter than 130 or 140 degrees F.
I would like to get specific confirmation, but it sounds as though, these concerns are unfounded since there is more than one suggestion to boil the acidic solution. Can someone weigh in on this?
Also, will mst household kittchen pots and pans be okay to use for boiling or heating the low pH acidic ir high pH basified solutions? I don’t have a stainless steel cookware. I just have an old pot with a nonstick coating. So I only d water heat baths. It would be more effective and quicker if I could heat directly in the pan however. Any advice on this is also welcome.

I like to heat my solvent before adding it to the basified solution. BecUse the hotter the solvent the more csn be dissolved in it, however in realty I’m sure the temperatures equalize so fast that it isn’t as effective as I would like.


Thanks for the replies so far. I love this site. Lots of hepful folks who all mean well. It’s pretty
 
I think from 400g of bark, anything above 2.4g is worthy of gratitude nowadays. 3.2g deserves a smile, and 4.8g can be toasted with your favorite beverage. 6g, add a biscuit (cookie) or a slice of cake :D

Sounds like you may have more on the way, so maybe get a nice glass ready ;)

As far as warm solvent goes, both the heat capacity and the volume of the aqueous phase are so much greater than that of the NPS that you ought to warm the base soup for this to have a meaningful impact. It may lead to a more deeply-colored product, of course, which seems to be down to oligomerisation, mainly - even if people have called it "plant fats" for years.

I would strongly recommend getting hold of some stainless steel pans (thrift store?) if you possibly can. They will last you a lifetime.
 
Okay. What about my concerns about boiling? Will bringing the bark solution to a simmer or low boil have any adverse effects? Like I said, I can’t remember where I picked up the idea, but I’ve always been careful not to let it get too hot out of fear of damaging the final product or affecting yield
 
Well, like @acacian mentioned, you've done cold to warm brews so far and can use some more heat with an additional couple of brews on the remaining material. This should show whether any further yield is to be had with the aid of simmering or boiling. Thermal and pH-driven decomposition of, say, yuremamine, may act to increase the final yield, and/or it could be that boiling improves the release of intracellular DMT to this end.

Accounts by @ms_manic_minxx do seem to suggest that a lid-on, gentle simmer will give superior results when compared to an open, rolling boil. Maybe this is part of the background of the advice you've heard, to avoid boiling the bark?
 
@CokFLHX DMT HCL will be stable in boiling water. You may also have read posts of mine discussing the possibility of extended high heat degrading DMT with certain plants, but Mimosa hostilis isn't one of those plants.. it was in the context of some Australian Acacias that can get some wierd chemical complexes going on in certain conditions.

People have been doing standard A/B (which usually includes boiling material) on Mimosa for many years now and its not been shown to reduce yields. That said, I quite admire a cold extraction and if you can make it work then more power to you. Cold solutions are generally much easier to do pulls from as they pull a lot less unwanteds. I do cold extracts fairly often but also fortify with ethanol in my acidic solution.. and I let it sit for days. I do think people overthink extraction with MHRB a little at times.. simple A/B extraction if done thoroughly should pull whatever DMT is in there. Ensure that material is dry and ground as fine as possible, boil/simmer in acidic solution (fortified with a little ethanol reduces required simmering time), squeeze from material THOROUGHLY. You can even add a little water to the bark once you've recovered as much of the liquid as you can.. this will free up any of the solution trapped in the plant material. Bring to pH 12 (optionally add salt )and if using naptha or heptane pull while base mixture is still warm. For a potential 6g of DMT then 3-5 X 100ml pulls should be sufficient if your base mixture is warm.. that's your bases covered. No reason why you won't recover all of the alkaloids.. or at least the vast majority.

I'm interested in your approach though and look forward to seeing whether boiling the material gets anything more.. if not, then your freeze thawing of bark in solution is probably fine. The fact that your yields with each soak became less indicates that you may be on track.

For testing different plants I like a quick A/B, but once I know the content of a plant, I like to take it slow and gentle.. utilizing an approach where you can efficiently pull the alkaloids from the plant without much other gunk migrating over.. It makes for a much more smooth sailing process once basified and doing NP pulls. I work during the week, so having material chipping away in cold solution during my work week is by no means lost time.. in fact its a few hours that I don't have to stand over a pot and I can write beats. Come the weekend, its ready to be strained and the rest of the extraction is a dream.. no emulsions, fast separation, less undesireable precipitate, cleaner extract. It's like the fine aged wine/cheese of DMT extraction 👌.. and more time to reflect on my intentions

@Transform I've often wondered whether the addition of salt during the acidic phase would be effective to break down material if doing cold soaks? Would the reduced solubility in salty solution outweigh the benefit of breaking down the bark quickly? When doing cold soaks I'll often use 50:50 ethanol to water and a little acid .. so I imagine that would balance out any change in solubility as DMT is pretty damn soluble in ethanol. May your chemical wizard mind weigh in on this question ;)
 
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Yeah. I’m kinda weird about final product purity. My very first extraction, I ended up with orange goo. I know now there is nothing wrong with the goo but at the time I thought I messed something up. Thst started my preference for pretty white crystals. I had the idea, although somewhat misguided, that the color of final product was a reflection of purity. The whiter the more pure, is what I used to believe and I still like it as white as I can get. I only use Heptane that is sourced by cans of Bestine.
I read somewhere that Heptane is a "pickier" solvent than naphtha. As in it will precipitate whiter, more pure crystals because the other plant alkaloids don’t as readily dissolve into Heptane as much as they do with naphtha. Again, I don’t know how accurate or true that statement is, but habits are habits, and I much prefer to use heptane.

I have noticed that by straining the bark out during the acidifying stage, adding salt, and pulling with heptane produces the pure white crystals without needing to water wash or re-ex
 
Oh! I nearly forgot I had another question!

So sometimes, after the solvent has separated, there is a layer in between that looks like a sludge. Is that a mini layer of emulsion? It’s more noticeable when using a separation funnel. Is that emulsion or pilymerization, or do you know what I’m even talking about without pictures? Some runs have it, some don’t. But it makes it hard to siphon the solvent all out.

What is this layer? Should it be discarded or is it a secret dmt saturated layer of good stuff that needs a mini a/b?
 
Well, since I’m here asking them…..

Are there any advantages or disadvantages to using different acids to increase the ph when acidifying MHRB? For example, are there any advantages of using hydrometric acid in RO water as opposed to vinegar, other than the volume required? I like how a drop will do ya with hydrochloric. But it’s nasty stuff and you have to take care when working with it. I’m pretty sure different acids make different salt compounds with the dmt, right? Is there any evidence of one being better to the other?
 
CokFLHX said:
Oh! I nearly forgot I had another question!

So sometimes, after the solvent has separated, there is a layer in between that looks like a sludge. Is that a mini layer of emulsion? It’s more noticeable when using a separation funnel. Is that emulsion or pilymerization, or do you know what I’m even talking about without pictures? Some runs have it, some don’t. But it makes it hard to siphon the solvent all out.

What is this layer? Should it be discarded or is it a secret dmt saturated layer of good stuff that needs a mini a/b?
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Yeah, you are spot on. Heptane is more selective than naptha - as to how much more selective I'm not exactly sure. I've not used heptane before and prefer to use non selective solvents with the plants I use. But naptha is pretty selective too as far as solvents go. Compared to solvents like toluene, DCM, limonene, chloroform or xylene it is very selective. It is less powerful though. The less selective solvents will often get everything in 1-2 pulls and don't require any heat.

So sometimes that layer of 'sludge' can be emulsion, (possibly even some kind of reaction caused by the addition of solvent into the mixture?). You'll know if its emulsion as the phases won't have a distinct separation. But if you have a clear distinct separation between the phases and you see it there at the top of the polar phase, then it would be other precipitates from the plant which are rendered insoluble at high pH levels. DMT definitely isn't the only thing to fall out.. all sorts of wierd and wonderful stuff can precipitate. It varies significantly plant to plant. Some plants have crazy amounts of other precipitates that crash when base is added.

If it is not a perfect separation and you think it is emulsion I would siphon off a little bit of that sludge with the solvent and then dilute with water which will aid in separation. You can optionally run through a coffee filter or cotton bud. If there's solvent trapped in it then that will often separate it.

Re: acids.. I think if boiling/simmering it is fairly inconsequential. Perhaps in your case since you are using cold solution, the choice of acid may be of more importance. I'd like to know @Transform 's thoughts on that.. as I'm speculating. What do you mean by RO water? I never use HCL for DMT extraction.. I've always been satisfied with vinegar or citric acid. But I'm sure HCL is fine..

Yeah different acids create different salts.. hydrochloric acid protonates DMT to form DMT hydrochloride.. and in turn citric forms DMT citrate, sulphuric - DMT sulphate, vinegar - DMT acetate and so on and so forth. In the plant it most likely occurs as DMT tannate (from the tannic acid in the bark).

Something to keep in mind too is fortifying your solution with a little ethanol will also increase solubility. Since your dealing with such cold solutions it should speed things up a fair bit.. I'm surprised to see very few people use ethanol in extraction, as its great stuff.

A cool trick I use ethanol for: soak material in ethanol for desired time and then boil off ethanol until its about 100ml.. add cold acidic water. Instantly lots of tars and resins crash out and you can just skim em off. They are sticky and hard to get off your fingers.. you only have to imagine how stuff like that might be contributing to emulsions. The DMT remains dissolved and you end up with a much cleaner solution.
 
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I work in a utility. Steam turbines, ect. We have a water treatment facility that uses big reverse osmosis filters to treat the make up water. I have done jugs that I keep filled from there. Whenever something calls for clean water, I have ultra clean, almost 100% pure water
 
Update:

I may have been a little hasty….

As I mentioned, I like to acidify the bark, then strain it, which I call a run. The strained bark is then added to more acidic solution and strained again for another run. Usually three runs with three pulls each will net all the alkaloids.

So far,I’ve netted a total yield of just under 5g, and I’ve yet to do the third run, and the last from run 2. My guess is I wil net around 6 grams out of 400g MHRB.

I started a separate extraction following Cyb’s Max Ion tek and the first pull from 100g MHRB netted 1.56g. So I’m happy about that. Max ion is more time consuming, but it’s seems fk get the job done
 
I need to do a water wash. The last time I did one I lost about half of my yield. Messed something up. This time I will keep the water just in case, but as long as the water and solvent are both hot, it should be fine, right? I should have lost so much last time. There is no way half the yield was in impurities that came out in the wash. Just no way. Same with this time. It’s mostly white, but with some junk in there I’m trying to get rid of. I did a reex and the solvent looked to be stained so I imagine the resulting crystals will be yellow or orange. I know it’s fine, but I like the pure white crystals. Any advice is appreciated.
 
CokFLHX said:
I need to do a water wash. The last time I did one I lost about half of my yield. Messed something up. This time I will keep the water just in case, but as long as the water and solvent are both hot, it should be fine, right? I should have lost so much last time. There is no way half the yield was in impurities that came out in the wash. Just no way. Same with this time. It’s mostly white, but with some junk in there I’m trying to get rid of. I did a reex and the solvent looked to be stained so I imagine the resulting crystals will be yellow or orange. I know it’s fine, but I like the pure white crystals. Any advice is appreciated.
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Pure water may still contain appreciable amounts of dissolved CO2, which could lead to dissolving some of your product away (acidity). This brings us back round to sodium carbonate washes. I wonder if this would reduce the amount of coloured material which gets washed away, yet I also fail to see why oligomeric material would get pull from solution preferentially. Yellow solvent can still deposit white, or off-white, crystals, though.
 
Transform said:
Pure water may still contain appreciable amounts of dissolved CO2, which could lead to dissolving some of your product away (acidity). This brings us back round to sodium carbonate washes. I wonder if this would reduce the amount of coloured material which gets washed away, yet I also fail to see why oligomeric material would get pull from solution preferentially. Yellow solvent can still deposit white, or off-white, crystals, though.
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Good point. I’ve also found this to be the case. White crystal can also colour solvent yellow. Also IME mini A/B cleans spice up much more than a sodium carb/hydroxide rinse.
 
So another update. A water wash was unnecessary. After drying out, the crystals weee nice pretty, and white. Just like a re-ex is supposed to accomplish. I just worry too much. Ha
 
CokFLHX said:
I need to do a water wash. The last time I did one I lost about half of my yield. Messed something up. This time I will keep the water just in case, but as long as the water and solvent are both hot, it should be fine, right? I should have lost so much last time. There is no way half the yield was in impurities that came out in the wash. Just no way. Same with this time. It’s mostly white, but with some junk in there I’m trying to get rid of. I did a reex and the solvent looked to be stained so I imagine the resulting crystals will be yellow or orange. I know it’s fine, but I like the pure white crystals. Any advice is appreciated.
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What kind of water did you use? Distilled or tap? Tap water contains all kinds of nasties, especially in certain regions of the world, even highly developed ones *looking at you USA*.
 
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