official extraction help thread

[psilocybin]

Any questions or problems you may run into during an extraction can be asked to get other members input in this thread.

 

[sarek]

If you're sure that the two layers have separated as much as they're going to, then I would recommend gathering the solvent and doing a Sodium Carbonate wash, as the FAQ recommends.

 

[aussietripper]

Hi SWIM has done 2 STB Extraction on Acacia Bark and Leaf using shellite and lye and freeze precipitated SWIM'S final product after freezing falls to the bottom but will not stick to the glass so the shellite with fats and oils can be Poured off

EXTRACTION 1​

Pull 1: set in freezer for 5-6 hours poured off and evaporated what was left ended up with a oily yellow resin that smelt like DMT SWIM smoked some and it is definitely active this extraction was done with acacia obtusifolia bark and leaf

Pull 2
was washed with 30ml calcium carbonate water x2 and then washed with 20ml cold fresh water 1x quickly to remove any impurities/fats in the oil it was then set in freezer at about -16 Celsius for 12 hours when SWIM checked the solution it has seperated but into cloudy looking suspensioin in the yellow shellite that where not floating on top but not stuck to the bottom everywhere SWIM then agitated the mix and left sit for another 10 hours when SWIM come back the suspension had all fallen to the bottom but was still not stuck to the glass enough to pour the shellite off this extraction was done with acacia obtusifolia bark and leaf

EXTRACTION 2​

Pull 1: was washed with 30ml calcium carbonate water x3 and then washed with 20ml cold fresh water 1x quickly and then an Epsom salt dry and strained threw a coffee filter has been in freezer for 20 hours now and SWIM is waiting for results it has not been touched once and is in a colder freezer at around -30 Celsius this extraction was with just acacia obtusifolia leaves

Possible problems​

freezer not getting cold enough
not using distilled water
being impatient and checking the solution in freezer and slightly agitating it by tilting to one side to see if anything has stuck to bottom of glass

the shellite is very yellow like urine there is also yellow sticky stuff that sticks to the glass above the shellite

 

[aussietripper]

Picture 1'2'4 Extraction(1)
Picture 3 extraction(2)

 

[aussietripper]

Extraction 2

 

[TiHKAL]

Cute puppy aussietripper but probably not extraction related.

On a different note: Does anybody have an advice how to "pull" harder? I'm harvesting my 7th pull now and I'm still getting 120mg.

I don't want to throw away good MHRB because 120mg are 5-6 trips but I'd prefer doing 4-5 pulls to get most of it out and be done with it.

 

[aussietripper]

sorry i didnt mean to add that picture and cant seem to delete

 

[DansMaTete]

Cute puppy aussietripper but probably not extraction related.

On a different note: Does anybody have an advice how to "pull" harder? I'm harvesting my 7th pull now and I'm still getting 120mg.

I don't want to throw away good MHRB because 120mg are 5-6 trips but I'd prefer doing 4-5 pulls to get most of it out and be done with it.

May be mimosa cells are not well lysed and the dmt is released slowly in the soup.

If you pull with naphta or similar, do you heat when you pulls ? If no, you should, as naphta is able to grab more dmt when it's warm (not more than 45°C to not grab to much unwanted stuff)

You can also use xylene or toluene for pulling , salt them and then pull with warm naphta.

 

[palomita]

Hey guys I still don't know what to do with my mixture.
I did a citric acid/fasa extraction from MHRB and now it is at the point when crystals should form. Instead I have a dark brown mixture with a pH of 1. I am suspecting the acetone not to be anhydrous (though I dried it with MgSO4). Would there be a way to remove water from the mixture, or anything else that might help getting DMT-fumarate crystals ?

 

[DreaMTripper]

Cute puppy aussietripper but probably not extraction related.

:lol:

 

[DreaMTripper]

Hey guys I still don't know what to do with my mixture.
I did a citric acid/fasa extraction from MHRB and now it is at the point when crystals should form. Instead I have a dark brown mixture with a pH of 1. I am suspecting the acetone not to be anhydrous (though I dried it with MgSO4). Would there be a way to remove water from the mixture, or anything else that might help getting DMT-fumarate crystals ?

Detail the steps used pleased

 

[DansMaTete]

Would there be a way to remove water from the mixture, or anything else that might help getting DMT-fumarate crystals ?

There is a very easy way : let it dry

 

[palomita]

The tek:

1) dissolve 5g of citric acid per 100ml acetone

2) take the shredded/powdered bark and cover it with enough citric acid acetone. Incubate in a warm place, gently agitating every so often. After 2-3 hours, filter off the citric-acid saturated acetone extract and set aside (this solution should have acquired the dark reddish colour of MHRB). Repeat 2 more times.

3) saturate acetone with fumaric acid. Acetone can hold ~20mg/ml fumaric acid if let for a day or so to completely dissolve.

4) Add the fumaric acid-saturated acetone in the citric acid-saturated acetone MHRB extract. One cannot put too much.

5) Set it aside and wait for 2-3 days. One should see a yellowish precipitate on the bottom.

NOTE: In step 2 one is making an acetone extraction and at the same time converting the alkaloids their citrate salt. After addition of the fumaric acid-saturated acetone in step 4, there is an interconversion of alkaloid-citrate to alkaloid-fumarate salt, like:

dmt-citrate + fumaric acid <-> dmt-fumarate + citric acid

citric acid has a pKa of 3.13, while fumaric acid's pka is 3.43. Fumaric acid is a weaker acid and thus in the above reaction one should have most of the dmt as a citrate salt and just a tiny amount as a fumarate salt. dmt-fumarate however is totally insoluble in acetone (while dmt-citrate is perfectly soluble), and it precipitates as soon as it forms. The insolubility of dmt-fumarate acts therefore as a "sink" and given time all of the dmt-citrate will eventually convert to dmt-fumarate and precipitate out.

6) wash the precipitated fumarate salts with acetone, then take them out and let them dry.

7) dissolve the alkaloid-fumarate salts in 5ml of tap water, then and then add saturated sodium carbonate to make the solution basic. The alkaloids will be freebased and the solution will become milky. In 3 days they will precipitate out forming nice needle-like crystal in the basic solution. At this stage, one can filter the solution (nasty procedure since the crystals tend to be sticky and waxy) and retrieve any left alkaloids by dissolving them in acetone.

8 ) Let the crystals dry, wash them with acetone (it removes any traces of sodium corbonate which is totally insoluble in acetone), evaporate the acetone and enjoy the product.

For the FOAF of SWIM 30mg were for a good STRONG experience.

I am theorically stuck at step 5, I did everything as recommended except I waited longer than said above. It's been approximately two weeks that I am waiting for the yellowish precipitate.

Thank you for your advice DansMaTete, but wouldn't it be a problem to have citric acid with the dmt-fumarate crystals ?
Wait...would it be possible to dry the mixture then add 100% anhydrous acetone so that the citric acid will mix with acetone, leaving beautiful dmt-fumarate crystals ?

 

[Guovsahas]

Hi,

New kid on the block from the land of the Midnight Sun. SWIM made a few extracts with MHRB so far and SWIM has been experimenting with CYB's tek and DMT handbook but SWIM has also been looking into other teks, one problem SWIM had at two runs is the foaming.
It settles after a hour or so but SWIM really gets pissed off because it messed up one extract leading that it didn't yield that much. First time SWIM did it SWIM was shaking it violently for a good 30-40 sec and later learned that the NPS holds air bubbles, so SWIM took this in reconsideration for next runs and has been swirling the bottles to prevent air bubbles.

SWIM is thinking, wouldn't it be possible to boil for a longer period of time like 8-10 hours and then separate the MHRB powder to prevent foaming then using the acidfied water for extracting?

 

[Du57mi73]

Please watch language.

By foam do you mean emulsion? Or are you actually getting a foam on top of your solution(s)?

Those aren't air bubbles. They are water/NPS bubbles.

How did your foaming cause your extract to not yield much? Those two things are unrelated. If your extraction didn't yield much is probably wasn't basified enough(which would also lead to foam/emulsion) or your solvent wasn't saturated well enough during freeze. Either that, or.. your bark might not be good? It seems like every extraction you run into problems. Do you think it is possible it is not MHRB or can you be certain it isn't operator error? Lol.

You dont need to boil for that long. 3-4 hours is extremely sufficient. Strain out the bark and reboil it with some fresh acid solution to grab more goods. Bark-less solutions is ALOT easier to work with than soups. But be sure to do multiple boils on the same bark because theres always going to be some goods left in your bark, especially if you only did 1 boil. Try to press/squeeze the bark to get all of the acid solution out.

 

[Guovsahas]

Please watch language.

By foam do you mean emulsion? Or are you actually getting a foam on top of your solution(s)?

Those aren't air bubbles. They are water/NPS bubbles.

How did your foaming cause your extract to not yield much? Those two things are unrelated. If your extraction didn't yield much is probably wasn't basified enough(which would also lead to foam/emulsion) or your solvent wasn't saturated well enough during freeze. Either that, or.. your bark might not be good? It seems like every extraction you run into problems. Do you think it is possible it is not MHRB or can you be certain it isn't operator error? Lol.

You dont need to boil for that long. 3-4 hours is extremely sufficient. Strain out the bark and reboil it with some fresh acid solution to grab more goods. Bark-less solutions is ALOT easier to work with than soups. But be sure to do multiple boils on the same bark because theres always going to be some goods left in your bark, especially if you only did 1 boil. Try to press/squeeze the bark to get all of the acid solution out.

My bad, pardon my french :!:

I've got a PH meter but at the same time I don't want to use it for strong chems because I'm using it also for my weeds. I'm getting ph paper for that.
Yeah it might be because I remember the batch that failed turning grey instead of black, like a milky greyish color. I got my bark from a trusted vendor, that a friend of mine got it from.

I'm preparing to boil it, I'm taking 50g of MHRB just to fine tune the recipe. I am getting stuff a little at a time, right now my kit is very very basic but it gets the job done.

The most successful yield so far has been 800mg of white fluffy crystals which is 600mg more than the failed one that foamed up a lot

 

[Shambolic]

I was wondering if anyone might be able to shed light on my issue....? I would post in main extraction forum, but can't due to restrictions on new members.

I've run through a typical AB extraction of 1kg of MHRB. Boiled in acetic acid @ approx pH 3.
Reduced to a few litres and allowed to cool, filtered and separated from sludge.

Then basified with 50g of NaOH to pH 12 plus (pH meter struggled with extreme pH)

This was left for a week while I worked on some ACRB.

I only had 400 mL of naptha (waiting for order), so I seperated approximately 1.5 L and heated in a bath with 100 mL of naptha. This was mixed and then allowed to separate in heat bath and layers form. It looked fine, no emulsion. This was repeated with another 100 mL, and then 200 mL.

As soon as it cooled to room temp it was good and cloudy. There was a few blobs of base in the jar which I separated out when I put naptha in a dish for freeze precip.

Now this is where I notice something isn't right. It smells of NaOH or caustic soda (lye in american) :|

After a night in the freezer I can see normal looking DMT crystals formed on the glass and atop a layer of creamy sludge which I assume to be NaOH that has somehow got into the naptha layer. There was definatly no base solution in the dish after seperation. The creamy sludge was already in the naptha after seperation from the base layer.

What has caused this to occur? Have I over basified my initial base? Was it too hot when I separated it? Did I not leave it long enough to seperate out (unlikely as it had separated perfectly) ? Was there not enough naptha in ratio to base solution? I just assumed from my chemistry knowledge that the naptha would simply take on as much DMT as it could before reaching saturation point, then I can do further pulls when I have more naptha....

And how do I recover the DMT from the naptha now? I'm thinking of doing an acid wash to but unsure if it will work if there's NaOH in the naptha?

Any thoughts or comments would greatly appreciated

 

[sarek]

It is most likely from incomplete separation, but it's a pretty common occurrence so don't beat yourself up about it. I always do a sodium carbonate wash on my solvent before freezing. This removes polar impurities. What you can do now is, once the freeze precipitation is complete, pour the naphtha back into the basic solution for more pulls, scrape up what crystallized out, and redissolve it in a small amount of fresh, heated naphtha. Polar impurities such as lye will sink to the bottom while the DMT dissolves. To be extra careful, you could then do a sodium carbonate wash on this solvent before freezing again.

Search the forums/wiki for "sodium carbonate wash" and "recrystallization"

 

[Shambolic]

Ok, thanks....

On further reading I now realise the naptha and base solution was overheated.

The naptha was reheated in a heat bath then separated out the clear naptha. Then the remaining 'sludge' (is this the right term? I know people are particular about the nomenclature here) was diluted in more naptha and an acid wash was performed on this. Now the naptha is visibly clearer, then turning cloudy at room temperature. Not yellowish and then going really cloudy like it was before.

Will report on what precipitates out this time after a wash up with some Na2CO3 before going back in the freezer.

Regards,

Shambolic

 

[Shambolic]

The acid wash and sodium carbonate wash at warm temperature seems to have worked. Looking as it should :roll:

 

[SargeHT]

Newbie here... just wanna ask if anyone had extracted this kind of crystal like visually but oily to the touch? used Q21Q21 tek 2..