Why do my extractions keep failing?

[DMTPanda]

Hi all,

So I seem to keep failing with my Obtusifolia extraction attempts (mix of bark, twigs, and phyllodes).
A/B was used (HCL to pH of just below 4, and NaOH to pH just over 12).
No acid wash.
Pull was performed with Hot Diggers Shellite (shellite was boiling, though the basic dmt solution was air temperature)(and nexians have said to have success with hot shellite).
Added approx. 150ml to the basic solution.
Swirled multiple times and left for 24 hours (on the concrete pavement in the hot sun).
The container was swelling up and I had to release the pressure many times and continue to swirl.

Upon extracting the shellite, it had a yellow colouration however had absolutely no cloudiness.

Placing this in the freezer, no sign of anything forming, just the same clear yellow shellite.

Really disappointed, what are some suggestions to get a success?

 

[DreaMTripper]

Obtusifolia doesnt have a consistent alkaloid profile as far as I am aware so maybe the ecossystem you are harvesting from isnt condusive to dmt as the process you described it sufficient to extract dmt.
The only thing that may be wrong is boiling the naptha, it could be destroying the alkaloid.
Try room temp toluene or simmer down the acidified solution to 50ml and base with excess sodium carbonate, dry, powder and pull with anhydrous IPA or acetone as described in the blab tek.
Nen88 has mentioned before that HCL may be problematic too vinegar is fine.

 

[DMTPanda]

Yeah I have pulled goo before from the same plant, but threw it out not unknowingly.
Do crystals have difficulty falling out during freeze precipitation if there is too much solvent?
Should I try letting a whole lot of the solvent evaporate before trying to freeze precipitate again?

 

[wearepeople]

Yes, crystals have a tough time falling out of solution if its not saturated enough. Perhaps try a pre-freeze-evaporation. Maybe down to 1/3 or 1/4 the original volume.

You could also take a small amount of the solvent and do a 100% evap on that to see if you have anything. I would do this first.

Also, it has not been proven by science, but in the huuuuuuuge acacia thread various people swear that its essential to not harvest material during or a few weeks after a rain.

Best wishes,
Wap

 

[DMTPanda]

How do you ensure you have a saturated solvent?
Reduce down the basified solution and amount of solvent used?
I still have quite a lot of basified solution, maybe that can be reduced down by letting some evaporate as well?
I had to add alot of NaOH and hence water to up the pH, so I ended up with a basified solution with about 2L or more.

 

[alert]

How do you ensure you have a saturated solvent?

Blow on it and it should turn cloudy at room temperature. If if is very saturated it will become cloudy without even blowing on it.

You want to evaporate your solvent down, not your basic soup. Leaving an open container of basic sludge to evaporate would not only take an extremely long time but it also isn't the safest thing in the world, it could be accidentally tipped over and become a huge problem.

Since you have so much basic solution you are going to want to make sure it is mixed with the solvent repeatedly (lots of twirling and spinning) to maximize the alkaloids the solvent picks up. A heat bath while you do this wouldn't hurt either.

After you do this evaporate the naphtha down to 50ml or so or to when the solvent becomes cloudy and then put it in the freezer.

 

[shanedudddy2]

Testing if a solution is saturated by blowing is a pretty poor method.
A number of times, i've blown, gotten clouds...and nothing precipitates.
My money is on it being one of the following (or combination)
1) it isn't obtusifolia (are you certain on ID? Identification of Acacia can certainly be tricky imo)
2) it is obtusifolia, but is a low yielding sample, or was obtained after rain.
3) the shellite was no adequately mixed with the basic solution, I shake up and down 25 or so times. Then repeat that 3-5 times before pulling.
4) Shellite sucks

To address, issue 4, I`ll cross post the method that me and a few friends use, which is preferable, since Toluene is so great at first run extractions.

I`ll help you out, since I live in Australia myself.
Firstly, yes, Shellite is rubbish, only use that for defatting purposes, if you have need to perform defatting.

Step 1) Obtain Toluene, this is commonly sold a fuel additive (I believe for car racing *shrug*) from Auto shops...at least that's how I got mine.
Step 2) Obtain Zippo fuel, just goto a smokemart, sold in 125ml bottles...bit pricy, but this is just used for recrystalisation.

When doing the extraction, you do your initial pulls with the Toluene.
Let that evap completely, it will result in a brown/orangish/yellow goo, that seemingly has crystals embedded, when it is dried.
Scrape this up with a razor-blade into a shot glass, with a small amount of Zippo.
Place the shotglass into a small container of boiling water (also known as a water bath).
Stir this around and it will heat up, although one may panic, it's fine see it boiling.
Once it's mixed, a large part of the goo will be dissolved.
Take the shot glass out of the water bath, and let it sit.
Initially the fats will drop to the bottom of glass.
During the transition from clear/slight yellow, to cloudy, transition the liquid into a secondary shot glass.
Repeat the process, moving the second recrystalisation pull into the secondary shot glass.
Then simply throw glad wrap over the top, and throw that into the freezer.
I did this process with a friend last night, and we`ve both done it a number of times with great success.
All the best.