Sempiternal
Rising Star
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.
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.
