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soxhlet exctracter

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SWIM uses 91% IPA in a Soxhlet with chacruna all the time and gets really good DMT yields from it. Something else must be going wrong.
 
Attention All Shipping said:
Another failed IPA extraction, this time with 91% IPA. I'm not going to be using IPA again. Same issues as previously with 3 layers forming & nothing freeze preciping out of heptane at all. Got to say I'm very frustrated with this whole soxhlet process, still I'm blaming the IPA rather than soxhlet.
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Methanol/ethanol in for the form of denatured alcohol did not work for my sugar glider, but he ordered from the only Netherlands/Holland vendor in the "Suppliers" thread in General Chat to not have a single bad review. Perhaps it is because his sugar glider's Thermolyne hot plate does not stir from 100 - 1000 RPM but in fact it does stir at nearly 0 RPM :p
 
69ron said:
SWIM uses 91% IPA in a Soxhlet with chacruna all the time and gets really good DMT yields from it. Something else must be going wrong.
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I've found what the problem was. Turns out the Heptane I was using isn't actually Heptane - or if it is it's gone off somehow. I used that same batch of Heptane in a noman tek extraction on new bark & nothing freeze precipitated out at all. I evaped a little and it produced oily gooey residue. To test I added some FASA to the heptane and it precipitated out in clouds eventually leaving a hard orangey yellow residue with that distinctive smell at the bottom of the jar. I'm seriously pissed off as I'd got the 'heptane' from a reputable chem supplier (Mis**al NI) in a 5L quantity & they'd been reliable in the past, though now it looks like I've got a more non-polar solvent than Heptane.
At least it resolves my issues over efficacy of the soxhlet/IPA. Thanks to everyone, particularly 69Ron, who helped troubleshoot this.
 
SWIM was interested in the idea of getting an aforementioned 500ml Soxhlet Extraction Apparatus that has a 50/42 female top, 24/40 bottom, and comes with a 50/42 male bottom Allihn Condenser. SWIM also thought it would be a good idea to reuse the condenser as part of a fractional distiller. Is this feasible? SWIM is considering low-budget ideas, and both distillation and soxhlet setups would already be sharing a hotplate and lab stand.

The distiller would most likely consist of a (all 24/40) flat bottomed boiling flask, a Vigreux Column, a 3-way distilling adapter w/ thermometer, and possibly some sort of 50/42 to 24/40 adapter in order to fit the Allihn.. and then most likely no drip adapter. Is this silly? Should SWIM consider a separate condenser for the setup?
 
How are you gentlemen !!

So anyone care to summarize best practices for this procedure?

1. It's still not clear to me which solvent is preferable: IPA, ethanol, acidified IPA/ethanol, DCM, heptane (I don't have access to that one), naphtha, water, acidified water (and which one of citric, HCl, acetic, etc. is preferred).

2. Extraction time is also not clear. I've seen 4-6 h thrown around, but no explanation where that comes from and whether yield will be increased much by going higher (I'm actually using a Gregar extractor which does continuous extraction, so it should be faster).

3. Also, as for post-processes, I see that at least for MH root bark it's not necessary to defat. Any other recommended post process?

(for my own use only) I can also configure the Gregar for liquid-liquid extraction, so I'm wondering if there is any benefit to a two step procedure (for example, when people extract essential oils with DCM which gets more out than alcohol, that carries over plant waxes as well so a second extraction with alcohol is usually done on the resulting semi-liquid resin).

4. Finally, any home chemist here ever try column chromatography as a purification step? I don't have a column but it should be possible to DIY one, and alumina or silica gel are cheap.

Cheers
 
@69ron
SWIM has finally got a decent amount of chacruna (~ 150g of wet leaf), SWIM would love to use DCM but its too rare. Planning on using IPA 100% 125ml, would need to add 12.4ml of H20 to get to 91% is that right?
1. How long does SWIY run it in sox to get 99% of product?
2.SWIY said that he gets around 1% is that wet or dry weight?
3.

Also SWIM is planning on trying an extract on Banisteriopsis caapi, would IPA pull harmine and DMT? at what %?

Cheers mate!
 
D_Juggz said:
@69ron
SWIM has finally got a decent amount of chacruna (~ 150g of wet leaf), SWIM would love to use DCM but its too rare. Planning on using IPA 100% 125ml, would need to add 12.4ml of H20 to get to 91% is that right?
1. How long does SWIY run it in sox to get 99% of product?
2.SWIY said that he gets around 1% is that wet or dry weight?
3.

Also SWIM is planning on trying an extract on Banisteriopsis caapi, would IPA pull harmine and DMT? at what %?

Cheers mate!
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125 / 0.91 = 137.362637362637363
137.362637362637363 - 125 = 12.362637362637363

Yeah, that's close enough to 91%.

It's really hard to say exactly how long to run the Soxhlet. It depends on many factors (solvent used, solvent to plant ratio, solvency of desired molecule, etc.). In most cases 12 hours is plenty enough. Sometimes as little as 8 hours. Sometimes as long as 18 hours! It all depends on what you're extracting. For DMT, 12 hours is plenty. 8 should do it. If it has running water as the coolant, then you can run it overnight unattended. You'll want to watch it for the first 30 minutes or so just to make sure everything is working properly. I don't recommend running it unattended until you get really used to using a Soxhlet.

That 1% yield is dry weight. It varies anywhere from 0.1$ to 1% depending on the source plant used. Hawaiian chacruna is usually going to give the best yields.

That last question I'm not sure about. SWIM has never extracted caapi before, he's only made tea from it. SWIM extracted peganum harmala several times and alcohol is not good for that because it degrades harmaline. But caapi doesn't have much harmaline, so alcohol could work ok for it.
 
Swim's has read this thread many times. She did a lot of experimantation and wasted many hundreds grams of perfectly good mhrb. To avoid further losses she would appreciate comments from the Chemistry High Priests and anybody with relevant experience.

69ron said:
....
Another tip, if you powder your herb and mix it with a little diatomaceous earth (about 4:1 of herb to DE) for improved drainage, you can fit far more herb into the Soxhlet and extracting time is improved.
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Swim's last 5 test extractions yielded almost no spice. Earlier mhrb from the same batch used to produce ~1.4% of very good spice.

For these experiments she used her home-made Continuous Solid-Liquid Extractor. Earlier she did more than a dozen extractions with consistent high yiled.

She started to experiment in order to eliminate one nagging problem - clogging. She bought a bag of Becogur 3500 (a respectable DE brand for water filtering) and proceeded to mix it with mhrb in various proportions. One time she used DE and mhrb only. Other times she combined it with perlite, vermiculite and coarse sand.

First four extractions she did with vinegar acidified water. Last extraction she did using 91% IPA + vinegar with subsequent A/B. This is not her first IPA extraction. Ealier she used to get ~1%, although with lot of hassle.

There is only one common factor in all 5 extractions - DE. She has to confess of one sin. In all extractions DE/mhrb ratio was higher than 1/4. She kept adding more DE because her extractor kept clogging. Even in the last IPA extraction where there was no clogging the ratio may have been ~1/3.

Questions:

1. Did anybody who used DE in mhrb extractions notice yields lower than usual/expected?

2. Any ideas as to possible reasons why this happened?

3. What would be a second/third best (to acidified water) solvent for mhrb extraction in extractors?
 
Where does your soxhlet clog? down the bottom or it just wont drain through the entire body evenly?
SWIM has had the same problem with MHRB powder, never tried DE though. Seems like it may be the solution to SWIMs problems....
I dont see why DE would cause reduced yield, unless the solvent wasn't making contact with the bark sufficiently...or something like that.

Swim personally gives up on trying to run powders through a soxhlet, its way too hard. Stick to ground up seed, leaf or cactus i think.
 
I have not been nearly as persistent with my soxhlet and powdered MHRB as some of you. I have had clogging problems with straight fine powder. I have put it in a 'tea bag' made of filter papers, but not enough solvent actually seems to penetrate the tea bag. I have placed a cotton ball filter at the bottom of the soxhlet, loaded the powdered MHRB, and then cotton on top and the solvent does not penetrate the MHRB mass much at all.

I have sworn off attempting to use the soxhlet to extract from any dense powder. It is a waste of good plant material. However, I am contemplating buying shredded MHRB and testing the waters with that material. Other shredded and looser materials seem to cause no clogging issues in my somewhat limited experiences.
 
D_Juggz said:
Where does your soxhlet clog? down the bottom or it just wont drain through the entire body evenly?
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At the bottom. Swim is able to stir the mhrb through the condenser with a long stiff wire all the way to the cotton ball at the bottom.

D_Juggz said:
SWIM has had the same problem with MHRB powder, never tried DE though. Seems like it may be the solution to SWIMs problems....
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Swim thought that too.

D_Juggz said:
I dont see why DE would cause reduced yield, unless the solvent wasn't making contact with the bark sufficiently...or something like that.
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That is not the case. Swim's mhrb lost its color almost completely. Also the extractor has been reloaded 3 times with the same mhrb. Swim is almost sure that DE is the culprit. She did 5 test extractions with zero yield. In all cases DE was used. Well, maybe too much of it?

Earlier swim used this particular extractor a dozen time with good yields. It would be interesting to have 69ron's opinion on this issue.

D_Juggz said:
Swim personally gives up on trying to run powders through a soxhlet, its way too hard. Stick to ground up seed, leaf or cactus i think.
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There are a few experiments swim is planning to run.

1. Using ethanol and methanol for primary extraction. Swim gave up on IPA.
2. Experimenting with various filters at the bottom of extractor to alleviate clogging.
3. Freezing/thawing/microwaving/defatting mhrb prior to running extraction.
4. Extracting from less finely ground mhrb.
 
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