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Soxhlet and Fine Powder

Migrated topic.
After experimenting with different leavening agents swim came to a disturbing conclusion.

Using Diatomaceous Earth (DE) may cause substantial (maybe even complete) loss of spice.

Four small-scale test extractions (50, 20, 20, 20 g) were done to determine the best leavening agent or their combination. Single common factor in all of them was the use of DE.

All extractions were done in an extractor that swim uses regularly quite successfully. Earlier this same batch of mhrb in the same extractor yielded up to 1.4% of very clean spice.

These last four extractions yielded alsmost no spice. Swim is pretty sure that she has enough lab experience to avoid major screw-ups that could have led to such losses.

Wikipedia says that DE is widely used as an absorbent to clean up spills. Could it be that it absorbs the spice as efficiently?
 
Recently Swim ran 2 test extractions.

One was aimed at checking if using DE as a leavening agent to prevent extractor clogging leads to loss of spice. Again, a rather careful A/B extraction yielded only 0.63%. Therefore, in swim's experience DE substantially reduces yields helping very little to reduce extractor clogging.

Another experiment was aimed at finding a better solvent for extraction of powdered mhrb in an extractor. Although swim uses a home-made CSLE, her findings seem to be applicable for other similar types of extractors. This time instead of IPA she used ethanol as the extractor solvent. Results proved to be much more encouraging than with IPA.

Materials:

Finely powdered mhrb - 30 g
Ethanol - 96%
Acetic acid - 9%
Heptane - lab grade
NaOH - lab grade.

The procedure:

1. 30 g of mhrb were soaked in 250 ml of ethanol + 50 ml of acetic acid diluted to 5% for 2 days.
2. Extraction process was ran in swim's CSLE. It took only 2.5 hrs to finish. There was no clogging whatsoever.
3. Most of the ethanol was distilled from the extract (1 hour).
4. Remaining ethanol was evaporated from the extract (1 hr).
5. The extract was dissolved in 50 ml of 5% acetic acid. (15 min)
6. The solution was filtered (30 min)
7. Defatting the acidic solution with heptane (3 x 15 min).
8. Basifying the solution to pH ~12.7 (15.min).
9. 5 Heptane pulls 20 ml each (5x20 min).
10. Complete Heptane evapping (1 hr).
11. Dissolving the extract in 5% acetic acid (15 min).
12. Decanting the acidic solution (3 hrs).
13. Filterig the solution (30 min).
14. Basifying the solution to pH ~12.8 (15 min).
15. 6 Heptane pulls 15 ml each (6x20 min = 2 hrs).
16. Reducing combine pulls to ~ 10 ml (45 min).
17 Freeze-precip (12 hrs).

The result: 539 mg of very clean off-white fine crystals
Yield: 1.8%.
Total extraction time: ~31 hrs.
Total active participation time: ~10hrs

Next time she will try methanol.
 
benzyme said:
m.p. test?
Click to expand...

No equipment atm. Swim will ask a friend chemist.

benzyme said:
1.8% is awfully high.
not to sound skeptical, but i have a hard time believing MHRB has that high of n,n-DMT content.
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It does look very high. What do you think could have been extracted in the process described? Btw, earlier the same batch of mhrb yielded 1.3% with IPA
 
maybe other simple tryptamines in the mix. those %ages are considerably higher than lit values.
0.63% sounds about right.

you gotta figure, alcohols are not selective at all; and if you take pHs too far, you're going to pull extra compounds. at pH 5.2, DMT is 100% protonated at the terminal amine; and 11 is a good roundabout pH to basify to in A/B

or it could be that SWIY has some particularly potent root bark. obviously an m.p. test is the simplest way to find out how pure it really is. pure dmt free base should melt at about 42-44 C
 
Thanks a lot for your comments.

benzyme said:
maybe other simple tryptamines in the mix. those %ages are considerably higher than lit values.
Click to expand...

Even after 2 A/B cycles, defatting 3 times and freeze-precipitation?

benzyme said:
0.63% sounds about right.
Click to expand...

Swim gets these lower yields every time she uses Diatomaceous Earth. Is it possible to check if there is any spice stuck in it? As instructed by her I asked several times on this forum but there is no feedback regarding possible spice absorption by DE:( .

benzyme said:
you gotta figure, alcohols are not selective at all;
Click to expand...

Swim has already figured that, but they are so fast in extraction. As a result the whole process takes much less time. Swim still hopes to find the best of both worlds.

Are all of them more or less the same selectivity-wise? Is ethanol theoretically any better than IPA? Swim got much better results with ethanol. Or is it just because she's got more experienced? Swim plans to run another test extraction with methanol. Do you think it is worth a try?

benzyme said:
and if you take pHs too far, you're going to pull extra compounds. at pH 5.2, DMT is 100% protonated at the terminal amine; and 11 is a good roundabout pH to basify to in A/B
Click to expand...

That is what swim kept forgetting all these times. Usually her pH figures are from 3 to 12.5 and higher.

There is another moot point in ethanol extraction. Is it adviseable to add some acetic acid during ethanol extraction, or use ethanol alone?

benzyme said:
or it could be that SWIY has some particularly potent root bark. obviously an m.p. test is the simplest way to find out how pure it really is. pure dmt free base should melt at about 42-44 C
Click to expand...

Swim may try to assemble a homemade device to measure it.
 
I take it pouring into a funnel with cheesecloth or piece of cut t-shirt and then grasping the corners together and squeezing out the liquid wouldn't work for you? I did that and it's pretty fast for my A/B extraction.

I had heated an A/B extraction, and used just that. It's very good for fairly small particulates. Then, the even finer ones could probably be filtered your way.
 
Nanaki said:
I take it pouring into a funnel with cheesecloth or piece of cut t-shirt and then grasping the corners together and squeezing out the liquid wouldn't work for you? I did that and it's pretty fast for my A/B extraction.

I had heated an A/B extraction, and used just that. It's very good for fairly small particulates. Then, the even finer ones could probably be filtered your way.
Click to expand...

Will you please explain to which part of swim's extraction your suggestion is related?

AFAIK, swim has no problem with filtering.
 
You had mentioned "SWIM tried different substances to loosen the powder and to minimize clogging buth with little success."

I was referring to your issue with clogging. When I filtered out the MHRB from the Vinegar solution, through some fabric, I had no problem with clogging.
 
Nanaki said:
You had mentioned "SWIM tried different substances to loosen the powder and to minimize clogging buth with little success."

I was referring to your issue with clogging. When I filtered out the MHRB from the Vinegar solution, through some fabric, I had no problem with clogging.
Click to expand...

You mean pre-soak and filter mhrb before loading it into the extractor? Interesting idea.

Let's make sure we are talking about same things.

Swim struggles with clogging when using her Continuous Solid-Liquid Extractor. Same happens to people running Soxhlets. Do you use a Soxhlet extractor as well?
 
No, haven't used a Soxhlet. So maybe can't offer good advice here. Though I did start with 500g finely chopped MHRB, soaked/heated in a crock pot for the polar extraction. Then poured through a piece of clean t-shirt I had cut which was in a strainer. Pulled the sides together and sqeueezed almost all the liquid out.

The polar liquid still had some very fine particles, which could be further filtered if needed.

I'll be using a glass funnel with cotton in it in the future for further filtering. For me, it's been good enough.
 
Nanaki said:
No, haven't used a Soxhlet. So maybe can't offer good advice here. Though I did start with 500g finely chopped MHRB, soaked/heated in a crock pot for the polar extraction. Then poured through a piece of clean t-shirt I had cut which was in a strainer. Pulled the sides together and sqeueezed almost all the liquid out.

The polar liquid still had some very fine particles, which could be further filtered if needed.

I'll be using a glass funnel with cotton in it in the future for further filtering. For me, it's been good enough.
Click to expand...

That's a good idea anyway.
 
Trickster said:
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.
Click to expand...

SWIM thinks this is probably the best avenue with mimosa in a soxhlet. Please keep us posted if SWIY tries this method. SWIM is finally in a spot where he can get some experimenting done and plans on trying this out, too.
 
rumplestiltskin said:
Trickster said:
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.
Click to expand...

SWIM thinks this is probably the best avenue with mimosa in a soxhlet. Please keep us posted if SWIY tries this method. SWIM is finally in a spot where he can get some experimenting done and plans on trying this out, too.
Click to expand...

Actually post #22 in this thread describes such an experiment with ethanol. It ran smoothly but yielded suspiciously high amount (1.8%) of off-white crystalline powder. Swim plans to assemble a home-made m.p. measuring device to check if it is spice or something else.

Next time swim plans to run extraction with methanol.
 
rumplestiltskin said:
Just wondering if SWIY has bioassayed or otherwise tested the ethanol extraction results yet?
Click to expand...

Yes, she did.

Swim could not wait until her m.p. tester is ready, so she decided to bioassay the product. She mixed some 1:1 changa (300 mg of mhrb extract + 200 mg of passion flower + 100 mg of FV Caapi Copy).

A few bowls of changa were smoked in a glass dry bong. Swim used her proven vaporization device - a Dremel heat gun. Immediately she noticed somewhat different taste/smell. There also was significantly higher body load. More nausea. In general the extract proved to be rather weak. Probably twice as weak comparing to normal spice.

This result was more or less expected because earlier the same mhrb produced 0.7% - 0.9% of high potency spice with a couple of different teks. For the last few weeks swim has been reading some serious books on extraction and she believes she's pinpointed her errors.

Her biggest blunder was to apply unnecessary wide range of pH during her A/B cycles (2.5 - 12.9). As a result not only DMT was extracted, but a range of other alkaloids.

These A/B extractions were performed on dried solids from mhrb ethanol extraction. The ethanol extraction and preceding freeze-thaw cycles have broken plant cells walls and alkaloids were readily available. Therefore, for an efficient A/B extraction it would have been sufficient to switch pH from 6.68 to 10.68.

This idea will be tested during the next extraction.
 
Here is swim's recent Ethanol + A/B test extraction.

The procedure:

1. 50 g of MHRB soaked in 250 ml of ethanol + 20 ml of vinegar.
2. Extraction process run in SWIM's CSLE for 3 hrs.
3. Most of the ethanol distilled from the extract.
4. Remaining ethanol evaporated from the extract.
5. The extract dissolved in 150 ml of water acidified to pH 5.
6. The solution filtered.
7. The solution basified to pH ~11.
8. 5 Heptane pulls.
9. 5 pulls by water acidified to pH 5 from combined heptane pulls, as suggested in Lextek.
10. Basified combined aqueous pulls to pH ~11.
11. 5 Heptane pulls.
16. Reduced combined pulls.
17. Freeze-precip (12 hrs).

No spice precipitated.

Then swim tested her new pH meter and has found that it is very incorrect. Testing first basic solution swim has shown that it was ~9,8 instead of expected 11. Therefore she decided to add more lye to the solution and re-extract it. She proceeded as follows.

18. Basing the solution to pH 11.
19. 5 Heptane pulls.
20. 5 pulls from combined Heptane with water acidified to pH 5.

At this time swim decided to test pH of the collected water pulls. To her surprise she has found that it is over 10! It seems very strange.

Anyway swim plans to further basify the liquid to pH 11 and pull 5 times with heptane.
 
Finally, swim's tek produced ~1% of beautiful fluffy crystals. After many trials and errors the tek has been reduced to the following steps:

1. Ethanol extraction in Continuous Solid-Liquid Extractor (a Soxhlet, or similar would do).
2. Distillation of Ethanol from the extract.
3. Drying the extract.
4. Dissolving the extract in acidic water (pH ~4.5-5)
5. Settling/decanting/filtering.
6. Defatting with Heptane/Hexane(optional).
7. Basifying with NaOH to ph ~11.5
8. Five Heptane/Hexane pulls.
9. Distillation of excessive Heptane/Hexane to ~20% of the original volume of combined pulls.
10. Freeze-precipitation of Spice.

The setup and tek proved to be very efficient chemicals-wise. Until now it has been tested in a few small scale extractions only (50g of mhrb).

You can judge the spice quality by the picture. White stains in the upper-right part of the photo are on the weighting cup and are not related to the spice.
 

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