Soxhlet, Acidic Solution and Mimosa extraction questions

[Jorkest]

SWIM was wondering if you used a soxhlet or similar extraction device..if you could use vinegar to salt out the alkies out of powdered root bark...because he knows the vinegar evaporates..or the acetic acid..but hes wondering if this would work for phosphoric acid solutions as well...because then he could just run the acidic water solution through the extractor and get a nice mimosa tea..that he could then basify and pull with d-limonene

any ideas would be awesome!

 

[fourthripley]

Phos. acid works fine for acidic extraction. However, it's bp is around 200c so evapping to dryness isn't an option and lowered ph on reduction is also something to bear in mind.

 

[69ron]

Vinegar and water would be your best option for this type of thing in a Soxhlet. It's food grade, and it will run through the Soxhlet over and over. Phosphoric acid will not evaporate with the water back into the Soxhlet like vinegar will so it stays stuck in the boiling flask below the Soxhlet. Vinegar keeps going back into the Soxhlet with the water over and over again and doesn't stay stuck in the boiling flask.

Soxhlets are FANTASTIC by the way. SWIM now always uses one for all his extractions! It saves you a ton of work.

 

[rumplestiltskin]

SWIM is a slow learner and has recently become very intrigued with the soxhlet. SWIM is used to doing A/B extractions with mimosa. Instead of boiling the root powder in acidic water (HCL or vinegar) for hours and then boiling even further to reduce liquid to a manageable volume, could he just use a soxhlet instead? In other words, would the soxhlet work in the initial acidify stage of an A/B extraction?

Also, SWIM was not aware that d-limonene could be used as a substitute for naptha in an A/B extract of mimosa, is this true?

 

[rumplestiltskin]

SWIM is also very interested in liquid/liquid extractors and their application and how they work. SWIM is a bit of a glass junkie. Anyone with first hand knowledge of these pieces please feel free to discuss.

 

[69ron]

SWIM is a slow learner and has recently become very intrigued with the soxhlet. SWIM is used to doing A/B extractions with mimosa. Instead of boiling the root powder in acidic water (HCL or vinegar) for hours and then boiling even further to reduce liquid to a manageable volume, could he just use a soxhlet instead? In other words, would the soxhlet work in the initial acidify stage of an A/B extraction?

Yes. That’s what SWIM uses his for all the time.

Also, SWIM was not aware that d-limonene could be used as a substitute for naptha in an A/B extract of mimosa, is this true?

Yes, but you need an A/B designed for use with d-limonene. Unlike naphtha, you cannot freeze precipitate in d-limonene, and it takes forever to evaporate.

SWIM is also very interested in liquid/liquid extractors and their application and how they work. SWIM is a bit of a glass junkie. Anyone with first hand knowledge of these pieces please feel free to discuss.

Yes, SWIM uses one all the time. They are very handy. They take a LONG TIME, but there is never an emulsion and it’s automatic so you just run in overnight. A 10-20 hour run is usually used. It depends on how fatty the plant matter is.

There are two kinds of continuous liquid liquid extractors: heavier than water, and lighter than water. “Heavier” or “lighter” refers to the solvent other than the water. For example, a lighter than water extractor would work with water and a solvent that’s lighter than water like heptane; and a heavier than water extractor would work water and a solvent that’s heavier than water like DCM. In both cases the water stays stationary in the extractor while the other solvent cycles through it for many hours. These work for defatting as well as the final base extraction.

When buying a liquid liquid extractor ALWAYS get one with a shut off valve on the small return arm. That way you can concentrate your final extract right in the extractor. This kind also works as a stand alone distillation setup.

 

[rumplestiltskin]

Thanks ron, that helps a lot. So in a an A/B extraction SWIM would use the soxhlet to acidify, then transfer over to the liquid/liquid extractor, add solvet, basify, run it for a good long time, then separate and precipitate? SWIM would need a lighter than water L/L extractor if using naptha, correct? Also, any suggestions on where to pick up a L/L extractor with shut-off valve? SWIM thanks you for all the help!

 

[69ron]

Thanks ron, that helps a lot. So in a an A/B extraction SWIM would use the soxhlet to acidify, then transfer over to the liquid/liquid extractor, add solvet, basify, run it for a good long time, then separate and precipitate?

You could also defat in the CLLE if you wanted. That’s what SWIM does. He defats overnight in the CLLE, then drains the DCM (he doesn’t use naphtha). Then he basifies the liquid and runs it again with fresh DCM.

SWIM would need a lighter than water L/L extractor if using naptha, correct?

Yes. That’s the kind of CLLE where the small return arm is high up and near the large distillation arm, and not connected to the bottom of the CLLE.

Also, any suggestions on where to pick up a L/L extractor with shut-off valve? SWIM thanks you for all the help!

Sorry, I don’t want to give out sources for such lab equipment. Search Google. It will take a while to find them, but several places sell them. Sometimes you see them on eBay, but not often. They are slightly more pricey, but not by much. I wouldn’t even bother with one that doesn’t have a shut-off valve. They are much harder to use and don’t work as a distillation setup.

 

[rumplestiltskin]

Ever heard of a Gregar extractor? Sounds promising....

 

[69ron]

Yes. It’s very versatile. They are very hard to find though because of the licensing issues.

 

[rumplestiltskin]

So does doing the initial acidifying in a soxhlet affect the yield or quality at all. If the boiling water/vinegar solution is passing through the root bark and back into the boiling flask won't the heat affect the DMT. SWIM knows you're supposed to keep the heat down when doing the regular boil that most folks use a crock pot for. Once the DMT is in the boiling flask does it stay there and only the water/vinegar solution gets condensed and dripped back onto the root bark, or are some of the molecules getting condensed too and being run through the bark continuously? Similar question with a L/L extractor, will heat from the boiling solvent affect the molecules?

 

[69ron]

The DMT acetate will stay in the boiling flask. DMT acetate cannot be steam distilled.

The only concern is the possibility of thermal breakdown at 100 C. I doubt this is an issue, but without any data on the thermal stability of DMT acetate in solution (most acetates are more stable in solution) not much can really be said here. It’s possible some is destroyed, but I just don’t think so. SWIM has extracted DMT acetate this way from Hawaiian chacruna many times and got fantastic yields of DMT rivaling those mentioned on the net by others.

Also DMT is very heat stable and can withstand temperatures above 100 C without decomposition, that’s why it can be smoked easily at higher temperatures like 150 C without ruining it.

Now DMT acetate is likely to be very unstable in dry heat at 100 C or higher and would possibly decompose into acetic acid and DMT and then the DMT would vaporize away. This is typical of acetates, but NOT when in aqueous solutions.

 

[Jorkest]

cool...SWIM cant wait until he has more time to work on this method...hes excited about it..

 

[rumplestiltskin]

^^^
Me too! Please keep SWIM posted, a soxhlet purchase lies in the balance!

 

[SuperRad]

^^^
Me too! Please keep SWIM posted, a soxhlet purchase lies in the balance!

Same here, I'm on the verge of getting a large soxhlet a CLLE (no shutoff valve though ), and a distillation setup. I know this may be too much to ask, but could you do the non-polar washes and the non-polar extractions with DCM?

And one question: which acid is better to use, acetic or HCl? HCl is the stronger acid and I believe that HCl is more volatile, and thus may make a better choice.

 

[rumplestiltskin]

Does anyone have any info on the heat stability of DMT? SWIM would like to use a soxhlet to acidify and defat mimosa, and a CLLE to do the pulls for him. SWIM only has access to solvents that have a higher boiling point than water (naptha and limonene) and he's worried that the heat in the boiling flask will destroy the DMT....

 

[rumplestiltskin]

SWIM was wondering if you used a soxhlet or similar extraction device..if you could use vinegar to salt out the alkies out of powdered root bark...because he knows the vinegar evaporates..or the acetic acid..but hes wondering if this would work for phosphoric acid solutions as well...because then he could just run the acidic water solution through the extractor and get a nice mimosa tea..that he could then basify and pull with d-limonene

any ideas would be awesome!

^
Any updates here Jorkest?

 

[timeloop]

Now DMT acetate is likely to be very unstable in dry heat at 100 C or higher and would possibly decompose into acetic acid and DMT and then the DMT would vaporize away. This is typical of acetates, but NOT when in aqueous solutions.

ok sorry to derail this thread a little... but I find this info very very interesting.

Could it theoretically be possible to develop some kind of setup that would heat the DMT acetate at 100 C or higher to seperate the acetic acid and DMT... with the DMT vaporizing and then collected when condensing on some part of the setup? This could then be scraped and collected and then smoked!

It would eliminate a whole section of the extraction process and be extremely pure and 100% food grade tek?

Would this be possible at all?

btw Soxhlets are absolutely great! :d