I would appreciate any input from people who had first-hand experience with extracting finely powdered mhrb using Soxhlet or similar extractors.

Swim tried different substances to loosen the powder and to minimize clogging buth with little success.

Swim noticed a strange behavior of finely powdered mhrb. Once the extractor is unclogged ~3 times (disconnected, upturned and completely emptied) it does not clog anymore and the extracting agent (acidified water) flows freely through the powder.

Any help would be very much appreciated.

mix the powder with diatomaceous earth.

It clogs anyway . In my test run I added 10 g of DE to 20 g of mhrb.

did you try to mix it with course clay (cheap cat litter) ?

Just checked markings on the DE bag. It says "Diatomide for beverages filtering". Brand name "Becogur 3500". It is a thin whispy white powder.

Is this the right stuff?



I thought of that, but when I tried to wash it before mixing with mhrb it completely dissolved. I did not like it.

hmm, no..probably not. methinks it should have the consistency of gravel to be really effective.

swim thinks swiy should design an ultrasonic horn and get a power supply on ebay.
swim had been pondering this approach since last year, and upon further investigation, came across this tidbit of info:

Alkaloids - total amount as well as speed of extraction is greater using the SONIC DISMEMBRATOR than with standard methods. Extraction from ipecac root in 30 seconds yielded more alkaloid than Soxhlet extraction in 5 hours

http://www.biologics-inc...ication_notes_page1.html


pulse mode + stirring should be pretty effective. divide the material into a few vessels containing some dilute acid

Strange. The company brochure says "BECOGUR 3500: Coarse kieselguhr for clarifying liquids heavily loaded with turbidities; also ideal for primary precoating."



Very interesting. This is on my list of future experiments. Do you happen to know how much power is required? What frequency is the best?

Lab US cell disruptors are very expensive, so I thought of using an array of cheap US humidifiers. The one on the attached picture has power consumption 250 W. Will it be enough?

From what I've read from chemistry books extractors work because they create constant supply of fresh solvent that washes off the solute.

I think this is why one uses several washes when preparing mimosa tea in a more traditional way. In case of US extraction: should one change the liquid several times also?

I would really appreciate your comments.

not always

swim was able to snag this http://cgi.ebay.com/ws/e...em&item=220631376109

200 W should be powerful enough to handle 500 mL at a time, using a flat tip on the horn (1/2" dia.)
20 kHz is standard, but anywhere from 20 - 50 kHz is typical for cell disruption

the nice thing about this approach is, the cavitation does all the work. no need for heating the aqueous phase (though one could.. heat it to around 60 C, speeds up the process even more)
one can use a dilute acid with a pH of 5 to convert the free dmt to salt, then basify and extract.
theoretically cuts the extraction time ten-fold

Swim is outside of the US.



That means that most of the energy will be concentrated close to the pit and will dissipate there. So, probably my device would not work because the US energy will be distributed between 9 relatively low power devices. .




The one I thought of buying runs at 1700 kHz. Too high?



Would it still require several washes?

How about those USonic cleaners? Could they be used for extraction?

yes, you'd still need to clean it up because lysing the cells will dump peptides and other cellular material into the solution; but lysing the cells is the most tedious process in A/B, and this method bypasses the need for excessive base in STB.

the ultrasonic cleaners may work, but you'd need to apply heat and sonicate for a while (a couple hours) because they lack both the power and localized intensity of ultrasonic probes.

as far as frequencies go, I think 1.7 MHz still falls in the ultrasonic applications realm, but it requires a good deal of power, probably over 1000 W. check the Applied Sonochemistry pdf in the sonochemistry thread.

I am intrigued. I love new gadgets!
Can one of you explain how this thing works and how you would use it to extract? I googled it but not a lot of info out there.


EDIT:
I found this


So would you simply put MHRB powder into beaker with liquid and put tip into mixture? I guess then filter it and alks will be in the liquid now?

exactly.
with a 100 or 200 W setup, the entire extraction process should take less than an hour.


the cavitation bubbles collapse, and shoot out microjets of liquid which lyse cell walls, dumping the contents into solution. power sonication also speeds up chemical reactions, and, under the right conditions, even initiates crystallization. the bubbles act as nucleation sites for crystal seeding.

lots of experimentation to be done

I'm keeping my eyes peeled for some surplus lab equipment again, no way am I paying 2K for one of those guys. Do you think one of these is what flowingvisions use that allows them to always say only water is used for the extraction?

could be


or it could be they do freeze/thaw cycles. (more likely)

That's what swim uses for preprocessing mhrb before actual extraction.

She said it only seems to worsen the clogging problem.

She noticed that after reloading the extractor 3 times with the same mhrb it does not clog anymore. This is probably because by this time all the sticky, gooey stuff has already filtered into the boiling flask.

Swim wonders if it will be more efficient to do a quick non-selective IPA extraction first. Usually it takes ~3 hours and then do an A/B on the extract. Swim will try this in the future.

that sounds reasonable.

yeah, once the cells are lysed, molecules will aggregate bases on polarities. they'll seep through given sufficient pore sizes

Swim just wrote to me to ask if it is necessary to completely dry IPA extract before proceeding with an A/B? Maybe it will be enough to reduce it to ~100-150 ml and then extract with 300-400 ml of acidified water ih her CSLE? Remaining IPA should evaporate during the extraction anyway.

no need to dry it, especially if adding acid; it's a moot point

SwiM was wondering first off if SwiY was using a thimble or cotton at the bottom of extractor..... there might be something to be said for investing a couple dollars in a good thimble although I think surface tension is allowing your powdered mass to clog your soxhlet.
It seems (maybe) there might be a period of time where the powdered mass becomes fully saturated resulting in the eventual even flow of the extraction fluid.
SO.... have you tried to 'presoak' your powder in the same solution you anticipate doing your extraction with?
Cover you powdered mass with just enough fluid to create a slurry and allow it to sit for a few hours (or just pre-prepare this the day before) allowing the fibers to soak up all the fluids they can hold (well past field capacity) and then place your "paste" in the thimble (or extractor with cotton, also pre-saturated) and initiate soxhlet extraction the same as you would normally.

Just a thought...

Unfortunately a thimble would not fit into swim's extractor. It is not a soxhlet.



That's right, because there is no clogging at all with IPA.



Hmmmm... Not sure. Swim conducted a number of experiments. She loaded her extractor with:

1. Dry mhrb
2. Freshly soaked mhrb
3. Presoaked mhrb (~1 day)
4. Presoaked, freeze/thawed mhrb
5. Presoaked, freeze/thawed in a microwave oven.

She also experimented with different leavening agents (coarse sand, diatomceous earth, perlite, vermiculite).

Dry loaded mhrb was the worst. It caked stone-hard after coming into contact with water.

Freshly soaked mhrb was better but clogging still was severe.

Perlite proved to be the best anti-clogging addive because it is less dense than water. During extraction it gradually floats up and water goes down. Once the extractor clogged completely it is only necessary to remove the cotton ball, drain the water, plug another cotton ball and pour the water on top of perlite. The process has to be repeated 2-3 more times and then there is no more clogging.

Sand is not good because it is heavier than water and moves to the bottom. Once the extractor is clogged it has to be cleared completely. Various combinations of the above substances were also tested. Clogging would not go.

Next time Swim plans to try some ideas suggested by 69ron



For all these experiments swim used 90 g of mhrb. After filtering and reduction she ended up with 300 ml of clear dark purple liquid (pH ~12.6). She defatted it once with heptane and proceeded to basify it. Then something strange happened. The liquid went white then, with more lye added to the solution, its color became latte and stayed that regardless of how much more lye was added. Usually with similar amounts it was required to add 5-10 g of lye for the liquid to turn almost completely black. This time she added ~35 g and the color did not change much. Moreover, when swim tried to pull with heptane thick emulsion appeared. It would not go for 12 hours.

Only after diluting the basified liquid from 300 ml to 800 ml swim was able to finish the NP pulls.

Combined pulls were reduced from 200 ml to 30 ml and are sitting in a fridge now.