So my extractions have gotten worse!!

Below is how I carried out my 1st ever extraction.
You should also note that I didn’t have anything to check the pH with and my glassware was not ideal as I found out.

My 1st tek was the following –

- 1000 mls Distilled water
- A dash of Vinegar – A shot glass worth
- 100 grams A/C (Powdered)
- Gentle Boil/simmer for 1 hour

I then filtered the water through an old t-shirt into a separate jar catching the bark.
I then put the bark back in the boiling pot, adding 1000 mls water with dash of vinegar and boiled for 1 hour. Done this three times until I had 3000 mls in a separate jar.

I then dissolved 60 grams of Caustic to a small jar then poured into the 3000 mls.
(Turned black with a sweet smell)

Let cool for 30 mins

Then added 200 mls of Naphtha, stirred with a spoon for 10 minutes (My jar does not seal so I have to stir with a spoon) let sit for 30 mins and transferred out using a spoon in to Pyrex dish.

Then placed the Pyrex dish in the freezer and left for 24hrs.

Below is an image of the final product.



After a couple more extractions I bought pH paper & electrical pH meter, a pipette for sucking up Naphtha, lab glassware (Conical flask, measuring cylinder, glass syringe 50 mls). I managed to find a Pyrex dish with secure lid, I was getting a lot of water in my final product due to no cover/seal. All of these items make the extraction easier to carry out, also lowering the chance of contamination……just not the final product!

About 10 extractions later, everyone getting a little worse I am starting to get a little annoyed.

My last Tek (and the majority have been this)

- 1000 mls Distilled water
- 200 mls of Vinegar (This gave me a pH of 3)
- 100 grams A/C (Powdered)
- Vigorously Boil for 1 hour

I then poured the 1000 mls water into a separate jar, not filtering out the bark.
Only small amounts of bark left the pot.
Poured 1000 mls water with 200 mls vinegar back into the pot and boil for 1 hour. Done this three times until I had 3000 ltrs.

I then poured all the water/bark into a jar ready for the caustic. So now there is 100 grams of powdered bark sitting/floating in my acid boils.

Added 20 grams Salt pre-dissolved in distilled water

Added 100 grams of dissolved Caustic to the 3000+ mls.
pH was 13+ once added
(Turned black with that sweet smell)

Then added 100 mls of Naphtha, stir with spoon for 10 mins, let sit for 30mins in a hot bath.

Transferred naphtha out using pipette into a measuring cylinder, let sit for 10 mins making sure no caustic/water contamination.
Then sucked naphtha out again into Pyrex dish and placed in the freezer.

Left in the freezer for 24hrs. Below is a picture of what I got, I should also mention that the naphtha was extremely yellow after this extraction; it was very cloudy and smelt strongly of DMT.

Once out the freezer it looked like this-



Not sure if the bark under a high pH moves into the naphtha then after freezing flocculates. It definitely looks like fats or swollen bark sitting in the naphtha.

Also one the naphtha was drained off and the Pyrex dish was left next to a fan,I did have some white crystals but there was a thick dark goo on the bottom. (oil?)

So as you can see after using better lab equipment, checking the pH throughout I’m continuously ending up with a bad product.
There’s definitely a lot of oil in the spice. When it’s under heat it bubbles A LOT into a black liquid not evaporating; also it burns the back of the throat.


The difference in both Teks are –

Increase in Vinegar – Not sure if a pH lower than 3 will draw out more fat/oils
Vigorously boiling - Increase in heat may be drawing out more fats/oils
Adding salt but I don’t think this is the problem, as it will only help the transfer from water to naptha.
NOT filtering out the bark prior to adding Caustic –If the bark is sat in a pH of 13+ it may release a lot of fat/oils or break down so fine it sticks in the naptha.
(My guess this is the problem somehow)

I am going to carry out another extraction in a month or so but will revert back to my first method, less vinegar / heat and filtering out the bark.

If anyone can spot something I am missing then please share, or if you know what the floaty bits in the naptha are please tell me.

Hopefully I end up with a good product next time.

Thanks

- There is a point where adding more vinegar will not result in a lower pH...200 ml in a litre of water is a lot, so you'll need more sodium hydroxide to neutralise the vinegar when basefying, but since you are using a pH meter that should not be the problem
- Vigorously boiling could be a problem - I have no experience yet with ACRB - you should check if there's any data regarding boiling point, melting point etc of dmt-acetate to know if any yield might be lost there
- I never filter out my organic material, however it will help in getting a cleaner yield (but one can also sort this during re-x)...

That being said...there is something else in your post that kind of boggles my mind...

"Then added 100 mls of Naphtha, stir with spoon for 10 mins, let sit for 30mins in a hot bath."

This makes little to no sense in my opinion...
-Try pre-heating your naphtha (safely! if you don't know how, look it up)
-I don't know what your extraction vessel looks like, but stirring with a spoon hardly seems adequate as far as mixing of olvent and basic soup is concerned unless you are using a very shallow vessel, in which case it would have a large surface area so your solvent would evap off during the half hour you let it sit after stirring...
-After, and if, the solvent and basic soup have been thoroughly mixed, decant the solvent off the basic soup immediately upon separation, what purpose would be served by letting it sit any longer?

Also, try using more salt the next time - it will increase the ionic strenght of the basic mix thus pushing more alkaloids into the non polar solvent...40-50 grams per litre should be fine...

Even though I don't get the boiling bit (but as said, I don't know anything about working with ACRB) you may want to reduce (evaporation) your 3000 ml before basefying - 3 litres is a lot a liquid for the alkaloids to sit in, less liquid would make it easier for the solvent to pick up the alkaloids later on... Never try reducing a solution that has already been basefied

Perhaps doing some reading (preferably of ACRB-specific teks, most of which would include a defat step before basefying to get rid of the oils and fats) will improve your understanding of what is done and, more importantly, why it is done, to increase your yield and it's purity...

Hope this helps...

PS How many pulls did you perform?

As mentioned above, 3L is a lot of liquid for only 100g of bark, you could probably get by with less than 1/4 of that. Before adding base, let the liquid simmer until it is reduced to less than 1L (it's easier to find jars of that size).

The primary problem is likely that you're not mixing the basic and solvent layer sufficiently. In order to do this properly, you really have to have a container that can be closed so that you can rock it back and forth for a minute or so, mixing the two layers. A spoon won't really do the job (and is more likely to cause dangerous lye splatters).

Both times I have seen this happen I have attributed it to heat. Both times I added the mhrb bark when the sodium hydroxide was still giving off heat and reacting. This causes the naptha draw more plant fats etc imo.