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official extraction help thread

Migrated topic.
benzyme said:
Nope said:
I don't get why any of you are using anything other than Q21s tech.
because there is no best tech, most of them are relatively equally effective, given the proper technique and solvents.
every method has its advantages and disadvantages.

I can go from bark to white crystals in less than an hour, using vinegar, KOH or NaOH, dcm, and naphtha.

Oooooo? Where can I see these secrets of yours?
 
it's all in the equipment: a sonicator (or some means of lysing cells quickly), a separatory funnel, and a rotary evaporator (which requires some form of vacuum pump. a diaphragm pump is ideal).
these things are not cheap, but can be had for less than a grand on a certain popular auction site.

a pressure cooker will also work instead of a sonicator, but that pushes the extraction time to almost two hours.
 
Also in regard to Thick Lights tek...
If small amounts of basic solution are present after decanting/separating the Naptha, is there a way to clean it up?
I'm a little freaked out over the thought of lye being in the final material.
 
benzyme said:
it's all in the equipment: a sonicator (or some means of lysing cells quickly), a separatory funnel, and a rotary evaporator (which requires some form of vacuum pump. a diaphragm pump is ideal).
these things are not cheap, but can be had for less than a grand on a certain popular auction site.

a pressure cooker will also work instead of a sonicator, but that pushes the extraction time to almost two hours.

Are there any teks which explain the process for using said equipment? Super curious -- for the sake of science. Obtaining them wouldn't be an issue, but learning that process, that'd be a wonderful project :)
 
sorry, the few of us that have the equipment havent written up a tek yet.

but the fundamental approach is this: use methods/equipment that will lyse plant cells to dump alkaloids into a dilute acidic solution (ex. 5% acetic acid); this may include, but is not limited to, sonication, microwave-assisted extraction, rotor-stator cell disruptor, or pressure-cooker.

perform a typical basification, extract with solvent of choice. distill solvent under reduced pressure (with a rotary evaporator, or distillation app). rinse the crude extract with warm naphtha, and remove it under reduced pressure (crystallization).
 
aqh said:
Reading through Thick Light's tek...
It looks like the first precip is done at room temp.
Does this need to be sitting in an open container or closed?

Follow up:

My Naptha was extremely milky white and cloudy as described in the tek. Nothing precipitated overnight at room temp.
When I stuck it in the freezer, it immediately (seriously, within minutes) started forming white crystals on the sides and more of a yellow precipitate on the bottom of the jar.

My intention is to use everything and start with some enhanced leaf, but I would like to re-x all of this first.
Can I re-x with Naptha or 99% ISO?
 
benzyme said:
sorry, the few of us that have the equipment havent written up a tek yet.

but the fundamental approach is this: use methods/equipment that will lyse plant cells to dump alkaloids into a dilute acidic solution (ex. 5% acetic acid); this may include, but is not limited to, sonication, microwave-assisted extraction, rotor-stator cell disruptor, or pressure-cooker.

perform a typical basification, extract with solvent of choice. distill solvent under reduced pressure (with a rotary evaporator, or distillation app). rinse the crude extract with warm naphtha, and remove it under reduced pressure (crystallization).


Thanks Benzyme. This is food for thought for sure. I am all about high efficiency processes in all manners of my physical dealings...Perhaps if I obtain such labware, I shall seek you out once more for advice :)
 
CouchLove said:
benzyme said:
sorry, the few of us that have the equipment havent written up a tek yet.

but the fundamental approach is this: use methods/equipment that will lyse plant cells to dump alkaloids into a dilute acidic solution (ex. 5% acetic acid); this may include, but is not limited to, sonication, microwave-assisted extraction, rotor-stator cell disruptor, or pressure-cooker.

perform a typical basification, extract with solvent of choice. distill solvent under reduced pressure (with a rotary evaporator, or distillation app). rinse the crude extract with warm naphtha, and remove it under reduced pressure (crystallization).


Thanks Benzyme. This is food for thought for sure. I am all about high efficiency processes in all manners of my physical dealings...Perhaps if I obtain such labware, I shall seek you out once more for advice :)

A chemistry book goes a long ways.
 
Hey there. Try to make it as quick as possible. ;)

SWIM made his first extraction, after beeing a silent reader over month.
However it did fail.

Following was done:

An AB exctraction has been made with 20g finely shreddered dried Psychotria viridis leaves.

- made 3 boils with PH 4.0 via citric acid.
- filtered and combined the water.
- defat 5 times with Naphtha (30ml) (Zippo lighter fluid)
- let it sit over night
- basified the mix with 10g of lye (NaOH), ending up with a PH 10+
- stirred 5 minutes, let it separate, stirred again, let it separate and then pulled with 15ml Naphtha
- did this 2 times
- put the Naphtha in the freezer for 3 days.
- put it out of the freezer, quickly removing the Naphtha
- suddenly everything melted
- let everything evaporate several hours

SWIM is now left with a colourless fluid/oily like substance, that can be scraped up.
Tried to freeze it again. It woun't freeze either. It just stays like this.

What was done wrong? Don't quite get it. However SWIM read about adding lye to an acidified solution, containing DMT, will destroy all of it. Is that right?

Did not pre evaporate the Naphtha to 50%. Was that a mistake?
Was the humidity in the room to high, so water could have destroyed it?
SWIM is pretty clueless. Hope, that I might help others with a similar problem aswell!

Cheers! ;)


PS: Got some pictures from the process. Just in case.
 
DRY TEK Q21Q21 question

Can i substitute CACLICUM HYDROXIDE and use instead CALCIUM OXIDE ? because it's impossible to find calcium hydroxide here.
I understand that calcium oxide will react with the water and anyway make calcium hydoxide. I also understand it will create heat.
Any other insight, or something i missed ?
 
UltimateShame said:
SWIM made his first extraction, after beeing a silent reader over month.
However it did fail.

Following was done:

An AB exctraction has been made with 20g finely shreddered dried [/b]Psychotria viridis[/b] leaves.
20g is a pretty small amount to be working with. And how can you be sure it was P. viridis? Also there is considerable variation in the alkaloid content of P. viridis leaves depending on the time of harvest and the conditions the plant has been subject to prior to the harvest. Dawn and dusk are peak alkaloid times, drought stress increases alkaloid levels. This was discussed on a thread round here somewhere (UTFSE).

- made 3 boils with PH 4.0 via citric acid.
- filtered and combined the water.
Citric acid can cause particular problems with emulsions. How much tea did you end up with?

- defat 5 times with Naphtha (30ml) (Zippo lighter fluid)
Have you kept this naphtha?

- let it sit over night
- basified the mix with 10g of lye (NaOH), ending up with a PH 10+
More NaOH would help, pH 11-12 being better.

- stirred 5 minutes, let it separate, stirred again, let it separate and then pulled with 15ml Naphtha
- did this 2 times
More pulls would be better. Did you really only use a total of 30mL of naphtha? Was the naphtha warm?

- put the Naphtha in the freezer for 3 days.
It's best to cool the naphtha more slowly to optimise crystal growth. First to room temperature, then wrap in insulation and put in the fridge for up to a day, then transfer to the freezer, complete with insulation.

- put it out of the freezer, quickly removing the Naphtha
Did you keep the naphtha?

- suddenly everything melted
- let everything evaporate several hours

SWIM is now left with a colourless fluid/oily like substance, that can be scraped up.
Tried to freeze it again. It woun't freeze either. It just stays like this.
This could be indicative of high NMT content in the material, or your seemingly thorough defat was insufficient. You could try a mini A/B of some sort to see if this will improve things

[...] However SWIM read about adding lye to an acidified solution, containing DMT, will destroy all of it. Is that right?
That is nonsense. How would a STB tek even work if lye destroyed DMT so readily?

Did not pre evaporate the Naphtha to 50%. Was that a mistake?
Sounds like you'd have no naphtha left if you tried that with the 30mL you said you used! But, you'd get better crystallisation if your naphtha was more saturated, yes.

Was the humidity in the room to high, so water could have destroyed it?
Water is even less likely to destroy DMT than lye is...

What was done wrong?
Too little starting material of unknown quality; poor choice of acid; possibly excessive defat solvent; insufficient base; excess water volume in base extract; insufficient ion strength in base extract; insufficient number of extraction steps; insufficient concentration of alkaloid in solvent; poor freeze precipitation technique; insufficient understanding of extraction procedures at the outset; lack of background research prior to commencing the extraction.

Don't quite get it.
All your answers can be found through searching on this forum, it's an educational resource. You can rest assured that many have found P. viridis to be pretty tricky to extract. And on the bright side, too, is that you only used 20g to start with. When you're more confident of your technique you'll find that a slightly larger extraction (not huge) will be more efficient.

"Dried P. viridis contains about 0.10–0.66% alkaloids."

Thus from 20g you could expect between 20 and 132mg of alkaloids if your extraction was anywhere near efficient. That's not terribly much.

PS: Got some pictures from the process. Just in case.
It would be quite helpful to see what you did, P. viridis extractions are a less common approach to the molecule.
 
Quetzal7 said:
DRY TEK Q21Q21 question

Can i substitute CACLICUM HYDROXIDE and use instead CALCIUM OXIDE ? because it's impossible to find calcium hydroxide here.
I understand that calcium oxide will react with the water and anyway make calcium hydoxide. I also understand it will create heat.
Any other insight, or something i missed ?
You can, although you had probably better add the water first as slaking quicklime can get very hot indeed. Is it really easier for you to find calcium oxide in your locality than calcium hydroxide? Or will you simply be making your own from chalk?

If you can find sodium hydroxide and calcium chloride you can then synthesise your own calcium hydroxide.

What solvent were you planning on using?
 
downwardsfromzero said:
Quetzal7 said:
DRY TEK Q21Q21 question

Can i substitute CACLICUM HYDROXIDE and use instead CALCIUM OXIDE ? because it's impossible to find calcium hydroxide here.
I understand that calcium oxide will react with the water and anyway make calcium hydoxide. I also understand it will create heat.
Any other insight, or something i missed ?
You can, although you had probably better add the water first as slaking quicklime can get very hot indeed. Is it really easier for you to find calcium oxide in your locality than calcium hydroxide? Or will you simply be making your own from chalk?

If you can find sodium hydroxide and calcium chloride you can then synthesise your own calcium hydroxide.

What solvent were you planning on using?

I find calcium hydroxide only in pharmacy for the simple price of 35euro a kg. that is ridiculus. even if i can afford it, it is ridiculus. I can buy 5kg of calcium oxide for 2 euros.
The problem is, if i mix with water first, i will not be able to DRY the mix ! that's why the calcium hydroxide is great. You first put the MHRB in acid for some days (liquid mud), then add the lime -> it becomes like soft clay. Maybe you have an alternative to dry the mix ? Add something like salt, or idon't know... ?
I plan to use Dilimonene
I could for sure go back to a more "classic" way. But if you ever try the dry tek, you realize that it is so much more confortable to mix your MHRB with your solvent, then you don't need to wait and separate it, you don't have emulsions, you just poor the solvent out. And it's all food grade. I love it.

And ultimatly, ok it will create heat... but if i go step by step... is it any inconvenient? It's actually great, it's winter! and it will activate the extraction :p
They sell this by 5kg to use in construction (i think to put on the wall as a high finition clay kind of)
 
Ive used this in construction and as paint (limewash). It is normally slaked with an excess of water, the quicklime being added slowly to the water, not the other way round. As downwardsfromzero said, a lot of heat is produced, and there is definitely a danger of getting splashed by caustic material. WEAR GOGGLES.

Traditionally it was slaked in pits in the ground and then left to mature under water for months or even years, forming lime putty, a material with consistency similar to cream cheese.

As the dmt limetek does not require the mixture to be absolutely dry, this lime putty could be used, maybe with the powdered rootbark dried after the acid soak, so as not to add even more moisture.
 
hey all - quick question:

when doing a freeze/thaw of bark prior to extraction, should one subtract the amount of water mixed with the bark during freezing from the amount of water added at the first stage of acidification?

for example, in Cyb's salt tek, 200ml of water is added along with the vinegar; would that amount be less because of the water added in the freeze thaw? after all, that water doesn't disappear....

any help wouuld be welcomed - many thanks!
 
ducdevil said:
hey all - quick question:

when doing a freeze/thaw of bark prior to extraction, should one subtract the amount of water mixed with the bark during freezing from the amount of water added at the first stage of acidification?

for example, in Cyb's salt tek, 200ml of water is added along with the vinegar; would that amount be less because of the water added in the freeze thaw? after all, that water doesn't disappear....

any help wouuld be welcomed - many thanks!

All that matters is if the plant material is properly suspended, and the pH is ideal.
 
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