First time extraction Q21 very low yield. Why?

[maktub2020]

Hi there!
After navigating the forum for some time and doing a succesful rue extraction, I decided to go for my first MHRB extraction.
I chose Q21 Wiki - Q21Q21's Vinegar/Lime A/B Extraction Tek Lime tek, because where I am, I haven´t been able to find lye. I used 100 Gr of root bark. It was shredded but I managed to powder it, with a good blender. I couldn´t find Naptha, I used "Wundbenzin" That according to members of the forum is the same and works fine. It is medical grade and doesn´t leave any traces when evaporating. I did three pulls but 3 and 5 days a part, so a reasonable amount of dmt should have been extracted. The total yield has been 0.10gr
I had a lot of trouble decanting the solvent. it is very "slippery", "oily", I don´t know how to describe it but it just slides along the edges of the bowl or jar, making really difficult to pour it in the precipitation container.
Also the solvent evaporated quite a bit in the freezer, even being wrapped in cling wrap several times in both directions.
I don´t know what went wrong. The produce looks very good (I still haven´t tried it) but I am surprised about the tiny yield. I don´t know if there is another tek that uses lime instead of lye or what to try different on the next extraction.
I still have quite a bit of MHRB.
Any ideas or suggestions would be greatly appreciated.
Thanks!

 

[Icon]

Is that photo of the three pulls combined?

Do you have a dedicated freezer for this? The solvent vapors can penetrate thin plastic films like saran wrap. If there was a lot of evaporation, anything else in the freezer in thin plastic wrap is gonna be contaminated.

I had a lot of trouble decanting the solvent. it is very "slippery", "oily", I don´t know how to describe it but it just slides along the edges of the bowl or jar, making really difficult to pour it in the precipitation container.

Not sure what you're describing here. Are you saying the bark mash is slippery? If so, you might have used too much water. Could add more calcium hydroxide to dry the mash out to a more crumble consistency. Put a lid or plate over the top of the bowl to hold back the mash when pouring off the solvent.

3 days, 5 days, too long to wait between pulls. Especially if you left solvent in the mash during those days, the solvent can get incorporated into the mash and make the whole thing more oily as time goes on.

 

[maktub2020]

Thanks for the answer.
Yes I do have a dedicated freezer.
I let it sit as described in the tek, just the bark mash, without the solvent. When I added the solvent was in a hot bath and let it sit for a bit more than half an hour.
What was very slippery was the solvent itself. I haven't been able to find a good and clean way to pour it in the precipitation container.
And yes, sadly, the picture is the three pulls combined.
Thanks!

 

[Transform]

If your bark wasn't properly powdered, that will impact initial yields. Also, it was found that naphtha (Wundbenzin) doesn't have quite the same penetrating power as solvents like limonene or xylene. One way round this would be to pre-soak the bark in dilute vinegar - use just enough liquid to moisten it so that it clumps - then run it through a few freeze-thaw cycles.

Furthermore, a light naphtha like that makes a relatively poor solvent for DMT (which, otoh, means that freeze precipitation works so nicely). Warming the lime/bark paste in a bain marie (NO NAKED FLAMES!) would help to improve your yield, assuming the bark is of a suitable quality.

If you've kept the bark paste you may well be able to get considerably more yield by doing a few more warm pulls, or by using one of the other solvents. [In the latter case, it should be borne in mind that better solvents aren't amenable to freeze precipitation so an alternative method of DMT recover must be used.] Just having the bark/lime mixture sit for a few days may already have helped set more of the DMT free throsgh a slow digestion of the bark's cellular structure.

There will also be a small but significant amount remaining dissolved in the naphtha you've already used. This DMT can be recovered in any of several ways, like mini A/B ( )

 

[maktub2020]

It was very well powdered, I´d say. I did all the pulls in warm baths and pre soaked the bark in vinegar, as described in the tek.
I still have the bark/lime mixture. I also have a bottle of "Washbenzin / White spirit". Would that be better than the wundbenzin?
I´ll try to find D-limonene.
I have the feeling that the solvent i used was not adecuate for this.
Thanks!

 

[Transform]

Yes, your Waschbenzin might be a little less selective and thereby more effective for the pulls. Ime, it took quite a lot of pulls even with waschbenzin to get stuff out of the lime paste. The Wundbenzin will still come in useful for recrystallisations, of course.

 

[doubledog]

I've had similar issues in the past and it turned out that solvent used (also some kind of clean european benzin) was the issue.

 

[maktub2020]

I've had similar issues in the past and it turned out that solvent used (also some kind of clean european benzin) was the issue.

What did you use instead?

 

[doubledog]

It was my learning period, so tried various approaches with different kind of benzin, but then also toluene.