I thought maybe I wouldn't follow the procedure exactly as indicated. Material from the same source had been used previously with about twice the yield, though maybe there was a variation in alkaloid content.
Approx. l lb. A. confusa root bark powder.
MOD EDIT: removed sourcing talk. Extraction
The entire batch was put in a large glass container to which about 3 gallons of tap water and vinegar was added.
No heat was applied but allowed to soak for a few days.
The mixture is separated by allowing the fine material to settle to the bottom and decanted off.
More vinegar and water added.
A fish tank heater is used to warm the mixture which is separated after a day or so of soaking.
A lot of sea salt is added until it no longer dissolves in the solution.
This is then separated by emptying out all the liquid except the accumulated salt at the bottom.
After a little bit of time, some precipitate falls to the bottom which is thought to be salt but perhaps this could have contained some alkaloids? Small amount of water is added but the salt is removed.
Basification
A strong solution of KOH and tap water is made.
It’s is slowly added until the entire solution turns black.
A little more is added for good measure.
Extraction:
The solution is heated until it’s barely too hot to handle.
About 250 ml naptha is added, mixed and separated.
The solvent being used has been recycled multiple times from previous extractions.
After the two layers are separated, the naptha is immediately added to a solution of vinegar and water separated and set aside.
The next day there are some alkaloids in the bottle that was used to re-acidify. It is already solid.
This process is repeated 3 times with the same reused naptha.
Basification:
There is about 650 ml of vinegar/water/alkaloid solution.
KOH is added until it turns and remains cloudy/white.
Naptha is used to extract the alkaloids and set aside.
The solution is no longer cloudy.
More KOH is added and turns white again so it is extracted again and a third time but there is not noticeable difference in from the previous extraction.
This second and third extractions are kept separate.
Crystallization:
Naptha #1 is left at room temperature. It’s not long before clear crystals begin to form. They are allowed to continue to grow for 2 days and then moved to the freezer.
Naptha #2:
This one is immediately moved to the freezer for 3 days.
Results:
Both solutions yielded about the same amount of alkaloids. A bit over 1100mg.
Total: 2430mg
The two solutions were combined and put back in the freezer but only resulted in a small qty.
This amount seems rather low for ACRB but maybe it can vary that much?
Perhaps it's human error?
Here are the goods. The one with film looking stuff was the one that went in the freezer immediately.
Shunyata attached the following image(s):
dmtfilm.jpg
(112kb) downloaded 91 time(s). dmtsmallcrystals.jpg
(111kb) downloaded 90 time(s).