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Help with Phalaris Aquatica extraction Options
 
Sempiternal
#1 Posted : 6/28/2020 11:55:40 PM

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Hello everyone. I'm having trouble getting a precipitate from my extraction and would appreciate anyone who can offer some insight as to why this may be. As a precursor only glass equipment was used throughout the extraction.

I started with 100 grams of cut up and dried Phalaris Aquatica (.32 cm - .64 cm) and soaked it in a vinegar water solution (pH of 4.6) for 5 days, occasionally heating it on the stove anywhere from 60-80 Celsius. (During the day I would keep the solution in the dark, whether that makes a difference).

On day 6 I filtered and attempted to defat the solution with 50 grams of Ronsonol lighter fluid at 35 degrees. Using very gentle swishing motions and by dripping the acidified solution of Phalaris into the solvent over the course of 1 hour. I read in multiple teks that I would see the solvent turn a brown or yellow color however the solvent stayed crystal clear. I residue checked 1 ml of the defat solvent on a watch glass and there was absolutely no left over residue.

After seeing this I knew something was probably wrong but wanted to see this through. I wouldn't use the finished product but wanted to get a better understanding of the process itself. So I moved the defat solvent to a round bottom flask for later distillation and began basifying the solution.

I had just made sodium hydroxide via the electrolysis of salt water (with use of a make shift electrolytic diaphragm) and added it to the solution. Because of this there were still traces of salt within the solution of NaOH but I figured this would not affect the result. Upon adding the solution of NaOH a precipitate began to fall out of solution. I stirred the solution and brought it to a final pH of 12.7, leaving it to sit for an hour. When I returned there was a layer of the precipitate at the bottom, measuring 1.5 cm thick (not compacted).

I decanted the liquid on top into a second beaker and ran five 30ml Ronsonol pulls on it. I placed all the pulls into a mason jar and placed it in the freezer for 14 hours, however nothing crystallized. I left 1ml of the solvent on a watch glass and let it evaporate and very tiny blobs of a yellowish liquid which wouldn't evaporate appeared. I assumed this may be DMT oxide which I would have to convert with zinc.

Currently I am evaporating the left over basified solution and rinsing the (what look mainly like salt and NaOH crystals) with my ronsonol pulls (bad idea?). I would evaporate all of my pulls but I'm going to try and distill the solvent for later use.

I would really appreciate it if anyone could tell me what that precipitate most likely was and whether it's a good idea to try and distill my solvent and collect whats left in the boiling flask. Also where else did I make mistakes? Would love insight from anyone, thanks in advance.
 

Trippy glass for trippy people.
 
Brennendes Wasser
#2 Posted : 6/29/2020 1:15:03 AM

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I have 0 experience in Phalaris, but your procedure just seems about right. These grass dont have such a clean Alkaloid profile, so if nothing crystalizes it may be due to the alkaloids being a wild mixture. Still, at least something should precipitate, even if not crystaline. That makes me wonder as you told no precipitate formed from your pulls.

Would be strange if all the DMT already converted to N-Oxide.

Quote:
Currently I am evaporating the left over basified solution and rinsing the (what look mainly like salt and NaOH crystals) with my ronsonol pulls (bad idea?).


No problem I guess, as you would this time just dissolve what you already have dissolved during the last pulls. So no problem repeating as there wont be any unwanted components migrating over, that arent already present in your Naphtha.

Quote:
I would evaporate all of my pulls but I'm going to try and distill the solvent for later use.


Isnt this basically the same? When you just gently heat the solvent in your distillation flask then you wont evaporate any (hopefully present) DMT and so you would also get back eveything that is hiding in the Naphtha. If it is oily you may try another recrystalization on that mixture, but maybe Phalaris got other stuff that will always prevent DMT from crystalizing. If there is still no yield, then maybe the grass was a bad batch? :/
Also dont you just harvest a special part of the plant? I guess you know much more about Phalaris and already did everything needed, but then you also considered that some parts of the plant may contain less DMT?
Check the

BIG Analysis on DMT !

Lots of interesting and possibly new stuff unraveled ;o
 
Sempiternal
#3 Posted : 6/29/2020 2:46:15 AM

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Thanks for the response and confirmation, even if limited, it is appreciated.

I've rinsed the precipitate that formed after basifying the solution with some Naptha and left it in the freezer so I'll post if anything precipitates.

Quote:
Isnt this basically the same? When you just gently heat the solvent in your distillation flask then you wont evaporate any (hopefully present) DMT and so you would also get back eveything that is hiding in the Naphtha.


Yeah they're the same, bad wording sorry. What I meant by 'evaporate' was just leaving it out in the open air, with no recollection of the solvent. For the distillation I'll probably gently raise the heat until something starts coming over, which should be well below the vaporization point of any alkaloids present.

Quote:
If there is still no yield, then maybe the grass was a bad batch? :/


Sadly this may be the case. I might have to try a different type of Phalaris, but I'll try sourcing from other fields around my area.

Quote:
Also dont you just harvest a special part of the plant? I guess you know much more about Phalaris and already did everything needed, but then you also considered that some parts of the plant may contain less DMT?


I didn't know when the field would be cut so I took everything but the roots. I figured if there was any DMT anywhere in the plant I would find it. The more the better right? Smile

Thanks regardless, I really appreciate it.
 
Brennendes Wasser
#4 Posted : 6/29/2020 3:22:01 PM

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I think I read somewhere that the most DMT is present in the lower part of the plant, but really no idea ...

Also maybe its a plant with huge variations of DMT, I read somewhere in may the concentration is highest, but then again we have basically this time of the year so it should be fine.

And also by treating an aqueous pull (made basic) with Naphtha you will definetly get the DMT out, so if this does not give you any yield then I would really say that either you harvested the wrong part or the plant did not contain a noteworthy amount :/ Because your TEK sounds just right.
Check the

BIG Analysis on DMT !

Lots of interesting and possibly new stuff unraveled ;o
 
Sempiternal
#5 Posted : 6/29/2020 4:19:31 PM

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Quote:
I think I read somewhere that the most DMT is present in the lower part of the plant, but really no idea ...

I'll try isolating different parts next time. Alzabo posted this in '~Phalaris = The Way Of The Future~'
Quote:
Code:
Part    % total alkaloid    by dry weight.
         Greenhouse    Field
Leaf tip        0.29    0.27
Blade base      0.23    0.26
Leaf sheaths    0.07    0.10
Stem            0.04    0.11

And yes you're right it can have huge variations, some may have none. I'll try a new batch and reuse the solvent.

Thanks for the confirmation and help Wasser.
 
 
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