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Reality check of next extraction plan Options
 
spyfish
#1 Posted : 5/8/2019 3:47:28 PM

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Just want to air my idea, just to see if there are any initial thoughts and immediate errors seen.

Probably complete overkill, but I do enjoy the experimentation and want to ensure clean product. For now, this is my plan:

Equipment: 1000ml Erlenmeyer flask, Magnetic stirrer (max 2400 r/min), 50ml Glass syringe with flat end 15cm needle (Luer lock)

I'll use CYBs salt TEK as a rough general guide for liquid amounts etc.

- Boil the 50 - 100g MHRB powder in acidic solution, filter out powder and reduce down a bit. Esentially make a very sour Mimosa tea. (maybe i can skip filtering the powder) I may simply just follow my Ayahuasca recipe for this, just with more acid and then reduce down to half liter.
- Defat with Naphta using magnetic stirrer for a few hours(1 pull)
- Add salt
- Base it using lye
- Extract with Naptha (PE 140-200) using magnetic stirrer

Clean it:
- Salt it back to a water/vinegar solution using magnetic stirrer
- Base it using calcium hydroxide, perhaps also add salt to limit emulsion
- Extract with Naptha (PE 40-60) using magnetic stirrer
- Freeze precip it


Due to previous bad experience/stupidity I will not use any heat with the solvent, and instead use 1 single very long pull with naphtha using magnetic stirrer. (8+ hours)
Work out of a larger plastic container, just to contain things if spilling occur.
Eye protection and gloves

Planning to use lye initially to make sure solution is liquid enough to magnetic stir. And the second round to ensure I remove any remaining fats and lye residue. And I've understood a lower boiling point PE is better for freeze precip.

I expect this to produce a clean product? Will take some days, but no hurry.
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Loveall
#2 Posted : 5/8/2019 5:36:51 PM

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What is the logic for the long naphtha pull? The limiting factor is the water/solvent system reaching equilibrium (this does not take hours I believe). Once at equilibrium some product will remain in the water. Waiting/mixing further will do nothing.

What does help is adding salt to the water and/or reducing the water volume (but avoid getting to an unworkable sludge).

When pulling you want to do multiple naphta pulls instead of waiting on one pull. There is an optimal number of pulls and volume, stay close to the reccomendations in a tek to begin with. If you measure the product from each of the first few pulls you get more info and can fine tune it next time.

The picture below from Wikipedia is very instructive. In the picture, someone is pulling a green product from water with solvent. You can see that it is going to take a lot of solvent pulls to get the green out of the water. You can wait for 100 years on the first pull, once at equilibrium colors won't change. The only way to get more green out of the water is to add fresh solvent and do multiple pulls.

Good luck on your extractions.
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β€œ... (a) psychedelic substance occasionally causes psychotic behaviour in people who have not taken it.”
Excerpt from a McKenna talk transcript / audio.
 
spyfish
#3 Posted : 5/8/2019 5:59:31 PM

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Thanks

Quote:
What is the logic for the long naphtha pull?


While searching trough threads about magnetic stirring someone reported they did one long pull with 250 ml solvent instead of many smaller ones, achieved the same result if not better as with many small manual pulls. Stating best results gotten with 8-10 hours with a good vortex on the mag stirrer.

Seemed practical
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Loveall
#4 Posted : 5/8/2019 6:49:33 PM

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Unless you have enough product to saturate a lot of solvent, smaller pulls should win. Regardless, as product is removed, once you no longer saturate the solvent multiple smaller pulls will be more efficient. During the temporary saturated regime it would be roughly a tie, and fewer pulls would be more convenient.

Was the result repeated by someone else? Do you have a link to the thread? It sounds interesting.
β€œ... (a) psychedelic substance occasionally causes psychotic behaviour in people who have not taken it.”
Excerpt from a McKenna talk transcript / audio.
 
spyfish
#5 Posted : 5/8/2019 7:35:55 PM

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Got it, thanks. I may have read the thread a bit quick. Seems like multiple pulls was done, but indeed very long pulls with no heat.

Here is the thread
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Loveall
#6 Posted : 5/8/2019 8:40:29 PM

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Thankfully the OP kept good logs.

amvitamine wrote:
Luckily I keep a log of extractions Smile
100 gram rootbark powder
100 gram of NaOH
1.6 liter of water
250 ml of solvent

Pull 1 400mg
Pull 2 400mg
pull 3 350mg
pull 4 120mg
pull 5 40mg
After that I didn't bother anymore and disposed of the soup
You see it pulls very consistent yields the first 3 times so good stirring is desirable


Total yield was 1.3%, respectable but not ground breaking. The issues he had without magnetic stirring (0.3% yield) may be from poor manual mixing. Others mix manually for fractions of an hour and can get 2% total yield after a few pulls.

Note that the first two pulls seem saturated. The next 3 follow the usual mathematics of partition equilibrium, with the ratio of two consecutive pulls being a constant:

120/350 ~ 40/120 ~ 0.34

Now, if we follow the info in this post, the power of his pulls is,

P = 1 - M2/M1 = 0.66

Looking at the table in the same post (the nearest P = 0.65 row), we see he got out ~96% of what was in the water once he did 3 pulls after leaving the saturation regime in the first two pulls.

All in all, a great extraction.

Also, the total DMT available after leaving the saturated regime was,

Mt = M1^2/(M1-M2) = 350^2/(350-120) ~ 530mg

Of which he pulled 510mg. So we know he left 20mg in the water. Adding this to the saturated pulls gives, 400+400+530 = 1330mg of total DMT in the water if which 1310mg was recovered.

So the pulls done out of the water are really good. To try to improve yields one could focus on getting more DMT from the plant into the water. One experiment could be to repull the spent plant material to see if anything new comes out.

While long hour magnetic stirring worked for amvitamine, I don't think it is neccesary. Good old manual thorough layer mixing of the order of minutes is known to give good results also.

Bonus question: amvitamine used 1250ml of naphtha in 5 pulls. What would he have pulled if he had done 4 pulls as follows:

1) One X ml pull with max volume in the saturation regime (here partition equilibrium concentration matches matches saturated concentration).
2) Divide the rest of the naphtha in 3 equal volumes and pull 3 times in the partition equilibrium regime.

How many mg of would be left in the water with this new strategy?

β€œ... (a) psychedelic substance occasionally causes psychotic behaviour in people who have not taken it.”
Excerpt from a McKenna talk transcript / audio.
 
downwardsfromzero
#7 Posted : 5/9/2019 12:33:13 AM

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Perhaps some of AcaciaConfusedYah's (at present fairly recent) posts about minimising use of reagents will interest you - it appears that MHRB is typically acidic enough not to require additional acid (if using distilled water), and tests showed pulls were performed with great success after adding only the very minimum amount of NaOH required to get the pH up by a sensible amount.

I'd search for you, but you're a big lad now, eh?

Using 140/200 pet ether will pull very nicely in under 15 minutes, especially if warmed a little. A water bath from the hot tap will do. Freeze precip's like a dream, too.
Ora, lege, lege, lege, relege et labora

β€œTo be GOVERNED is to be watched, inspected, spied upon, directed, law-driven, numbered, regulated, enrolled, indoctrinated, preached at, controlled, checked, estimated, valued, censured, commanded, by creatures who have neither the right nor the wisdom nor the virtue to do so. To be GOVERNED is to be at every operation, at every transaction noted, registered, counted, taxed, stamped, measured, numbered, assessed, licensed, authorized, admonished, prevented, forbidden, reformed, corrected, punished. It is, under pretext of public utility, and in the name of the general interest, to be place under contribution, drilled, fleeced, exploited, monopolized, extorted from, squeezed, hoaxed, robbed; then, at the slightest resistance, the first word of complaint, to be repressed, fined, vilified, harassed, hunted down, abused, clubbed, disarmed, bound, choked, imprisoned, judged, condemned, shot, deported, sacrificed, sold, betrayed; and to crown all, mocked, ridiculed, derided, outraged, dishonored. That is government; that is its justice; that is its morality."
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spyfish
#8 Posted : 5/9/2019 1:10:40 PM

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Quote:
1 One X ml pu with max volume in the saturation regime (here partition equilibrium concentration matches matches saturated concentration).
2) Divide the rest of the naphtha in 3 equal volumes and pull 3 times in the partition equilibrium regime.


Mt = 350^2/(350-120) --->> 532
532 + 800 = 1332mg total

1st pull (1.6 x 0.34) 544ml
2nd, 3rd & 4th pull rd pull 235 ml each

around 26 mg left in the water? (~ 98% extracted) though the last one felt too easy.

Or am I on the wrong track. My head is spinning a bit Big grin

Quote:
Perhaps some of AcaciaConfusedYah's (at present fairly recent) posts about minimising use of reagents will interest you - it appears that MHRB is typically acidic enough not to require additional acid (if using distilled water), and tests showed pulls were performed with great success after adding only the very minimum amount of NaOH required to get the pH up by a sensible amount.

I'd search for you, but you're a big lad now, eh?

Using 140/200 pet ether will pull very nicely in under 15 minutes, especially if warmed a little. A water bath from the hot tap will do. Freeze precip's like a dream, too.


Awesome, thanks Smile I will check that. Makes sense, I've brewed very strong Aya with Mimosa with very little Vinegar.

So your saying I dont need to bother with the PE 40-60? I think I read somewhere its better for freeze precip?

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downwardsfromzero
#9 Posted : 5/10/2019 9:51:36 AM

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The 40-60 will evaporate very readily - as I'm sure you'll appreciate(!) - so in terms of avoiding fire risks you might at least want to substitute that with heptane. Having your solvent disappear while you're trying to work with it can be somewhat tedious.

Recrystallisation from a more volatile solvent is desirable when having freeze precipitated from a higher-boiling solvent. Your mini A/B approach would circumvent this need but arguably adds an extra step for problems (emulsions, losses) to occur. Not that they necessarily will - overall there's nothing intrinsically wrong with your scheme as laid out, this really is just comment.

Quote:
PE 40-60? I think I read somewhere its better for freeze precip?

What exactly does 'better' mean here? More favourable temperature/solubility profile? Leaving less of, and a more easily removed, solvent residue? Something else? I'm curious.
Ora, lege, lege, lege, relege et labora

β€œTo be GOVERNED is to be watched, inspected, spied upon, directed, law-driven, numbered, regulated, enrolled, indoctrinated, preached at, controlled, checked, estimated, valued, censured, commanded, by creatures who have neither the right nor the wisdom nor the virtue to do so. To be GOVERNED is to be at every operation, at every transaction noted, registered, counted, taxed, stamped, measured, numbered, assessed, licensed, authorized, admonished, prevented, forbidden, reformed, corrected, punished. It is, under pretext of public utility, and in the name of the general interest, to be place under contribution, drilled, fleeced, exploited, monopolized, extorted from, squeezed, hoaxed, robbed; then, at the slightest resistance, the first word of complaint, to be repressed, fined, vilified, harassed, hunted down, abused, clubbed, disarmed, bound, choked, imprisoned, judged, condemned, shot, deported, sacrificed, sold, betrayed; and to crown all, mocked, ridiculed, derided, outraged, dishonored. That is government; that is its justice; that is its morality."
― Pierre-Joseph Proudhon
 
Loveall
#10 Posted : 5/10/2019 2:36:24 PM

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spyfish wrote:
Mt = 350^2/(350-120) --->> 532
532 + 800 = 1332mg total

1st pull (1.6 x 0.34) 544ml
2nd, 3rd & 4th pull rd pull 235 ml each

around 26 mg left in the water? (~ 98% extracted) though the last one felt too easy.


First part is correct (1332mg total) based on the behavior of the first 4 pulls.

However, how did you get 544ml for the max volume at the saturated regime? Looks like you used 1-p = 0.34, but you can't do that since as you increase the solvent volume, p changes.

I think this is may be a tough part to calculate though as you need to dive into the math and formulas and calculate the partion coefficient which is the constant in the system.

This is what I get:

Max saturated volume pull: 703ml (gives 1123mg)
3 more pulls of 183ml (122mg, 51mg, 21mg, combined give 194mg)

Total extracted 1317mg, 15mg remain in the water.

So if amvitamine where repeating this extract, he could do one large saturated pull followed by three smaller partition pulls (4 total). For the same amount of total solvent he saves doing one pull and gets roughtlt the same yield (technically a few mg more).

I can post fresh formulas to calculate all this if anyone is interested.


β€œ... (a) psychedelic substance occasionally causes psychotic behaviour in people who have not taken it.”
Excerpt from a McKenna talk transcript / audio.
 
 
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