A water only extraction -- in progress +pics

[alzabo]

Hello nexianoids,
I'm attempting to get some pure freebase out of rootbark using water as the only solvent.
This project has been developing over the last few weeks and I could use some feedback.
It is very much inspired by gibran2's post entitled Is Caapi Extraction as Easy as it Seems?

1.) 100 grams MHRB were placed in the herbal percolator with a very slow drip.
~5 liters of water were passed through over a period of ~216 hours or 9 days.
My tap water is rather basic so before passing the water through the THP, I first acidified with vinegar,
then later switched to phosphoric acid.

2.) The liquid was slowly reduced at below boiling to ~750 milliliters.

3.) The gunk was let to settle out in the fridge, decanted, placed in the frezzer 'till frezzen, settled in the fridge, decanted.

4.) Now the fun part. ~100 milliliters hot water was saturated with sodium carbonate.
The rootbark tea was poured through one of those plastic coffee drip things that go on top of a single mug.
This dripped into the saturated sodium carbonate solution. The effect was like a cottage cheese lava lamp.

I let this hang out for a while as I had to go across town to get my camera.
When I returned, I found an interesting sight.
+pic #1

5.) I stirred this up and tried to filter it. impossile. I had a battery of gold mesh filters and they clogged immediately. There were still a lot of oils and the precipitate was such a veeery fine powder.

6.) I let the solution chill out in the fridge for a couple days. By this time, the precipitate had settled out a little bit, now filling only half the liquid with a dark layer on top. I siphoned of the dark layer...and discarded it , I'm hoping the there were no actives in it but it's hard to be sure till the final yield is gotten and bio assayed.

7.) Topped off the mixture with tap water and allowed to settle at room temperature, this took 2 days to settle half way. I siphoned off the dark top layer (kept it this time).

8.) Topped up the vessel with more tap water. Three days later, there are many layers formed.
+pic #2
+pic #3

A few questions:
[query-1]
Why is the mixture not settling like it did the first couple times. You can see in the 2nd pic that the precipitates have only settled about 1/8th down as opposed to 4/8ths down as happened the last couple times.

[query-2]
What are these many distinct layers that have formed?

[query-3]
Dang, forgot it...slippery little devils those thought things are.

 

[gibran2]

Some of our chemist members will have to speculate about why DMT doesn’t easily precipitate out of MHRB, but like you, I recently tried to do something similar.

I did an acidified hot water extraction of MHRB and put some of the unreduced liquid aside. I slowly added some NaOH solution to the liquid, and the entire volume turned into a grey sludge (if you’ve ever done an A/B extraction, you’ve probably already seen this). My understanding is that the solution is not sufficiently basified when it’s in the “grey sludge” state. I think what you’ve collected is the grey sludge.

Anyhow, I added more NaOH solution, and the liquid turned dark brown, almost black, as normally happens when basifying MHRB. If you look closely at the solution, it’s cloudy, but it will not settle. The DMT is in there, but it will not precipitate out.

If someone could find a way to force it out of suspension, we’d have a really great new extraction technique. I know that aluminum sulfate is used in water purification to remove suspended solids – maybe if some is added to basifed MHRB liquid, the DMT and all other solids would settle out?

This is some very valuable work you’re doing. A water-only DMT extraction method would be great!

 

[ouro]

have you tried to centrifuge the solution to see if the precips will settle away?

Hommade centrifuge:

supplies:
jar w/cap
string

Put material in the jar and cap it tight. Tie one end of the string around the center of the jar and the other end to something high above an open space. twist it up and let go. be careful not to break the jar! improvments only limited by imagination, how much you can deform HDPE jars, and substituting bungee cord for string. Maybe tie the bungee cord around an elongated hdpe tube with a narrow at the center the cieling, and a point directly below it on the floor and twist that sucker up... be safe!

 

[prottel]

I have experienced dmt coming out of a solution with only water, acid and a base. But that was after a gelatin clean up. Might not have anything to do with it.

Basically, what you do is extract it, filter it, then reduce it to a very low volume, so the actives will be highly concentrated. Then you basify it until its black. Then you heat/boil it. This should cause the actives to form lumps of liquid. You should see them floating on the surface. Then you just cool it down in the fridge or add ice cold water. Should give you hard lumps of actives. It may be that vinegar may prevent this from happening, as I did another try with vinegar that did not work out. But the first time, I could several decent lumps of actives. But I think it has to be reduced to a very low level so that the actives will lump together.

 

[prottel]

Just did another test to see if I could get it to work.

In one experiment I used ascorbic acid, but I did not use milk to fine the brew. I just reduced 10g mimosa to 25 ml liquid. Then I added sodium hydroxide and took it up to boiling. No dmt seemed to come out.

Concurrently, I did the same experiment, but this time I used milk, 80ml milk for 10g mimosa. Then I put it in the micro until it had turned into concentrated goo on the bottom. I filtered this, which is very easy by the way. Then I reduced it to 25 ml. I added sodium hydroxide. Relatively quickly, there started forming lumps in the brew. I continued adding sodium hydroxide. There was quite a bit of yellow coloured lumps in it. It looked like what you get from the The :10 minute Tek.

At the moment it is in the fridge. When it has cooled enough, I will filter it and give it a taste.

 

[alzabo]

My extraction is chilling in the herbal percolator (7days so far). The solids and liquids should be done separating in a few more days. The THP is nice for tough filtering. It is slow but never completely clogs.

My understanding is that the solution is not sufficiently basified when it’s in the “grey sludge” state. I think what you’ve collected is the grey sludge.

Could you elaborate on this a bit.
My though was that I grossly over basified.

Just did another test to see if I could get it to work.
At the moment it is in the fridge. When it has cooled enough, I will filter it and give it a taste.

Any progress with this?

have you tried to centrifuge the solution to see if the precips will settle away?

Interesting.
I have not tried it.
Do you have any experience with this technique?

 

[mumbles]

To remove the solids it might be worth letting it settle in the fridge overnight and decanting, or doing the egg white trick perhaps.

 

[gibran2]

My understanding is that the solution is not sufficiently basified when it’s in the “grey sludge” state. I think what you’ve collected is the grey sludge.

Could you elaborate on this a bit.
My though was that I grossly over basified.

As NaOH (or other bases, I suppose) is slowly added to reduced, acidified liquid decanted from MHRB, the solution first gets very thick and grey. As more NaOH is added, the solution thins out (becomes more fluid again) and turns dark brown/black. The “grey sludge” stage is reached before the “black fluid” stage.

 

[Trickster]

...The “grey sludge” stage is reached before the “black fluid” stage.

Yep. Happens around pH 10. The solution becomes black and less viscous at pH 11 and above. Interesting, what's going on in there?

 

[Ayawasqero]

Good luck. Don´t forget to share the experience!

 

[mumbles]

...The “grey sludge” stage is reached before the “black fluid” stage.

Yep. Happens around pH 10. The solution becomes black and less viscous at pH 11 and above. Interesting, what's going on in there?

If you sloowly change the pH 8->12 you can see things precipitating at low pH then redissolving at higher pH, this is pretty handy for our purposes there is a post on here somewhere that explains exactly what it is but I cant find it atm. Its additional crap that dissolves in the hot acidic water.

 

[alzabo]

Wow, this is fascinating.
I will have to brush up on some chemistry so as to keep better track of pH in the future.

Something interesting I discovered was that the bulk of the precipitate doesn't dissolve in an acidic solution either.
I found this out by mixing some of the sludge with lemon juice until it stopped fizzing and tasted sour. I filtered the sour liquid, leaving behind a big glob of grey...stuff. This was done at room temperature. Perhaps the grey stuff would have dissolved if heated.
Again, this was from a brew of mhrb that had been meticulously filtered and given a single cold break for extra clarity.