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soxhlet exctracter

Migrated topic.
I guess I'll just have to find the best option that fits into my budget and adjust the amount I can boil according to that, but I have a much clearer picture now.
Compared to the US labware in the UK is about 2x more expensive, so the options are very limited. I was even better of ordering the soxhlet from over there and pay the costly shipping prices.:(
 
Benzyme, I guess you have an adapter between the condenser and the soxhlet. How do you find using it that way? I won a 500 ml soxhlet on ebay with 55/50 upper joint and seeing how rare the condensers are in that size I'll might buy an adapter and a 24/40 condenser.

Is it a good idea to use a retort for distilling? Like this:
Retort%20500.JPG


Or something similar, maybe a distillation flask with a 24/40 joint, so I could attach a condenser to it (and it would make sense to buy a 55/50 - 24/40 adapter that way. There seem to be so many ways to distill (distillation heads, the three way adapters etc.).

I know it's offtopic, but I'll have to think about the future, so I won't have to buy the same things twice (like someone in another topic who has 2 or 3 condensers, because of different joint sizes). So many options it's confusing...
 

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hehe, retorts are so old-school, but effective for simple distillation.
24/40 is the US standard, and it's easy to find adapters. swim uses a 45/50-24/40 reducing adapter on the soxhlet.

for distillation swim uses (24/40): two 500mL rbfs, three-way adapter, 300mm liebig condenser (water inlet and outlet on same side), and vacuum take-off adapter. this is vacuum distillation
867662452-CIMG1628.jpg
 
Wow, didn't know that about the stirring, I'll use a stir bar next timw I use the soxhlet.

While there's been a lot in this thread about setting up & running a soxhlet there's been nothing about cleaning & good maintenance. Last few times a hot water & soapy liquid wash has been enough to clean all visible traces from my soxhlet, though now I've got some harder to shift residue stuck to the inside of the thin tubes. Can anyone suggest any good labglass cleaning products or a good way to safely clean a soxhlet of residue?
 
use a moderately basic solution (pH 10 or 11, lye or ammonia) to get the tough residue off (wear gloves and safety glasses); and don't worry...it won't compromise the structural integrity of the glass.

and a stir bar isn't necessarily needed (go ahead and use one if you have one); though it's good to facilitate boiling to some extent, and to prevent bumping
 
Why isn't IPA considered for use in any of the teks as a solvent? Is it just more ideal for this application and now for manual extraction?
 
SWIM uses IPA for a lot of different things. It's cheap and easy to get in USP grade OTC.

When extracting bufotenine from Anadenanthera colubrina, he uses 91% IPA in his Soxhlet. It works really well (but 99% IPA doesn't work well for A. colubrina).

IPA reaches the siphon point must FASTER than methanol can. So 10 hours of Soxhlet extraction with IPA means more extractions than the same done with methanol. This is not what you'd expect because methanol boils at a lower temperature, but it doesn't vaporize well. A lot of the methanol tends to re-condense before entering the Soxhlet so it takes much longer to extract than IPA does.

If what you're attempting to extract can be extracted with IPA or methanol, then use IPA. It will extract it faster in a Soxhlet.
 
I don't disagree with what 69Ron says, I just want to make the point that my experience with using IPA as a soxhlet extraction liquid isn't so rosy. May not be due to the IPA of course but I've not yet managed to get useable DMT from using IPA in a soxhlet (3 times).
 
Was that 99% IPA that gave poor results? How was the IPA used? Was the plant matter whole? Was an acid added?

SWIM found 99% IPA to be very poor for a lot of different alkaloid salts.


SWIM uses 91% IPA without any acid added for extracting bufotenine from A. colubrina. It works really well. Yields are usually 2-5% bufotenine.

SWIM has also used 91% IPA for DMT and gets very good results. That’s mostly from chacruna and chaliponga without any acid added. He gets yields up to 1% from chacruna which is really good for chacruna. SWIM rarely extracts from mimosa. Mimosa might give different results because it likely contains DMT tannate, and I don't think chacruna contains DMT tannate. Chacruna probably contains DMT citrate or something similar because it’s a leaf.
 
69ron said:
Was an acid added?
Click to expand...

Do acids evaporate with the solvent?
I thought that one of the advantages of the soxhlet was that it could reuse a small ammount of solvent by distilling it from the solution so it's allways just the clean solvent and things below it's boiling point that reach the material.
 
69ron said:
Was that 99% IPA that gave poor results? How was the IPA used? Was the plant matter whole? Was an acid added?
Click to expand...
The IPA was 99.9% it was used undiluited in the soxhlet without any acid being added. The mimosa being extracted from was fairly fine powder resulting in some drainage issues but these were resolved. IPA was only diluited and basified after the soxhlet.

Mimosa might give different results because it likely contains DMT tannate, and I don't think chacruna contains DMT tannate. Chacruna probably contains DMT citrate or something similar because it’s a leaf.
Click to expand...
Interesting, I haven't heard anything about DMT tannate before, do you think this could be an issue? I would've thought that it wouldn't make any difference as whatever form of DMT would be converted to a freebase & be obtained from a non-polar solvent pull- unless IPA causes a specific reaction with DMT preventing it from transferring to the non-polar solvent. Does this make sense or am I just speculating wildly?

Has anyone else experienced problems using IPA on mimosa?
 
T said:
69ron said:
Was an acid added?
Click to expand...

Do acids evaporate with the solvent?
I thought that one of the advantages of the soxhlet was that it could reuse a small ammount of solvent by distilling it from the solution so it's allways just the clean solvent and things below it's boiling point that reach the material.
Click to expand...

It depends on the type of acid used. Vinegar (acetic acid) will re-distill along with water, if water is used as the solvent. So will hydrochloric acid. Citric acid will not.
 
Attention All Shipping said:
69ron said:
Was that 99% IPA that gave poor results? How was the IPA used? Was the plant matter whole? Was an acid added?
Click to expand...
The IPA was 99.9% it was used undiluited in the soxhlet without any acid being added. The mimosa being extracted from was fairly fine powder resulting in some drainage issues but these were resolved. IPA was only diluited and basified after the soxhlet.
Click to expand...

SWIM has NOT had good results using 99% IPA to extract natural alkaloid salts from plant tissue. 99% IPA is better for extracting freebase alkaloids. 91% IPA is better for extracting alkaloid salts. A lot of alkaloid salts are insoluble in 99% IPA but very soluble in 91% IPA.

Attention All Shipping said:
Mimosa might give different results because it likely contains DMT tannate, and I don't think chacruna contains DMT tannate. Chacruna probably contains DMT citrate or something similar because it’s a leaf.
Click to expand...
Interesting, I haven't heard anything about DMT tannate before, do you think this could be an issue? I would've thought that it wouldn't make any difference as whatever form of DMT would be converted to a freebase & be obtained from a non-polar solvent pull- unless IPA causes a specific reaction with DMT preventing it from transferring to the non-polar solvent. Does this make sense or am I just speculating wildly?

Has anyone else experienced problems using IPA on mimosa?
Click to expand...

The DMT in mimosa is a water soluble salt. The pH of the plant matter is much too low for it to be freebase. The DMT salt in mimosa might be completely insoluble in 99% IPA like many other salts are. It’s believed that DMT is present as DMT tannate because tannic acid is the dominant acid in mimosa bark. Usually an alkaloid is pared with the most abundant and strongest acid found in the plant.

All salt forms have different characteristics. The salt form DMT makes a difference in terms of it’s solvent solubility, boiling point, melting point, etc. The difference between one salt of DMT and another can be dramatic. For example, DMT acetate is many times more soluble in water than DMT fumarate. DMT acetate is soluble in dichloromethane while DMT citrate is not. DMT fumarate is less soluble in acetone than DMT citrate is. DMT fumarate is very stable while DMT acetate is not. The differences are many.

The only time the DMT is freebased is when a base is added to it. At that point, it is highly soluble in 99% IPA. But most salt forms of it are either poorly soluble in 99% IPA or insoluble in it. 91% IPA has very different solubility characteristics than 99% IPA. Most DMT salts are soluble in 91% IPA.
 
69ron said:
SWIM has NOT had good results using 99% IPA to extract natural alkaloid salts from plant tissue. 99% IPA is better for extracting freebase alkaloids. 91% IPA is better for extracting alkaloid salts. A lot of alkaloid salts are insoluble in 99% IPA but very soluble in 91% IPA.
Click to expand...

That matches with the results of an experiment I ran last night to troubleshoot my IPA/soxhlet problems: I took the used MHRB powder used in last soxhlet, put in base water - as per Noman's tek - and pulled once with Heptane. The freezered heptane showed some (though not much) white specks present. I evaped some of it and though it showed little visible residue (ma not be done evaping) it did smell of DMT.
So it looks like the 99.9% IPA is not extracting the DMT, or only extracting it in minimal amounts. I had thought the problem was pulling DMT from the diluited IPA with Heptane/Xylene but I'm leaning against this now - at least as a sole cause.

All I have is 99.9% IPA am I right in thinking to convert to ~91% I'd jut add 8% water (8% of final volume) or is the maths more complex?

So different diluition strengths of IPA have different levels of solubility for DMT, have you experimented with different strengths and found 91% the best or is that just what you have handy?


The only time the DMT is freebased is when a base is added to it. At that point, it is highly soluble in 99% IPA. But most salt forms of it are either poorly soluble in 99% IPA or insoluble in it. 91% IPA has very different solubility characteristics than 99% IPA. Most DMT salts are soluble in 91% IPA.
Click to expand...
So it looks like my options are try 91% IPA or basify the MHRB powder or the IPA before extracting.

Thanks for sharing your experience & knowledge 69Ron
 
Yeah, just add water until it's diluted to 89-91%. 91% seems to be the best, but add much more water and too much junk gets extracted.

99% IPA is less polar than ethanol and much less polar than methanol. Many alkaloid salts are insoluble in it.

91% IPA is just polar enough. Most alkaloid salts are soluble in it.

70% IPA is too polar. Lots of water soluble junk is soluble in it.
 
Just want to clear up a point on the A/B
With IPA is it beneficial to acidify IPA (91% ths time) before soxhleting inorder to defat or is ok to just defat the IPA with naphta as is, at the normal fairly neutral ph? Or would it be just as well to acidify after soxhletting but before defatting?
If acidifying IPA is necessary what ph is best?
 
It depends on the alkaloid being extracted. With DMT, the pKa is 8.68 so at 6.68 99% is ionized and at 5.68 99.9% is. It’s best if the pH is at around 5-6. That should be the natural pH of mimosa, if I recall correctly, so there’s no need to add any acid during the defat, in fact, brining the pH lower than 5 would cause less junk to be pulled by the defatting process so it would make the final product less pure.

Just make sure the pH is not 7 or higher. If you defat three times at pH 6.68, the most DMT you might lose is probably less than 3%, at 5.68 maybe 0.3% because the rest is highly water soluble. You get cleaner results if you defat at 6.68 with a very slight loss of DMT. This of course applies to extractions using DCM, xylene or d-limonene as the non-polar solvent for defatting and extraction. If using naphtha or heptane, it doesn’t matter much. In that case you could even bring the pH down to 2 and it would have little impact on the final results.
 
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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