Hi everybody. SWIMs been scratching his head and reading lots. He's just done his third extraction (first time on some MHRB) and is getting a very poor yield. On 1.5kg of bark, powdered in a blender he got about 3g total (0.2%). He's read of other people sometimes exceeding 2%. He didn't follow a tek exactly but feels he did things in a way which should result in a higher yield than this.
-Powdered bark in a blender.
-Boiled bark 4 seperate times in a pH 4 vinegar/distilled water solution for about an hour each time (3 hours on the last boil)
-Reduced the acidic solution to about 2 liters (a bit low but didn't think it would impact yield severely)
-Transferred filtered acid boils to 2 large jars.
-Performed a defat step on one jar, but not the other, using about a litre of ronsonol lighter fluid.
-Basified to pH13
-Pulled with heptane @ 70°C until nothing preceipitated when put in the freezer @ verycold°C
-Added pure NaCl to the basic solution until saturation
-performed one more heptane pull with minimal results.
-After pulls, product was recrystallized with heptane yielding roughly 3g of slightly off white powder.
-Including yellow goo left over from recrystallizations yield may approach 4g.
He is wondering why his yield is so low for the amount of bark he used and what he can do in the future to make it better. Is it likely just low quality bark? He doesnt see where he could have gone so wrong in the extraction as to lose a potential of 90% of the alkaloids.
SWIM has done 2 extractions before on acatia confusia. He recalls getting a decent yield with each pull even after the 12th pull, and a rough estimate of 1.5%.
In the case of this most recent extraction on MHRB he only did 3-4 pulls before they stopped yielding anything.
Please help SWIM improve his tek!
-Powdered bark in a blender.
-Boiled bark 4 seperate times in a pH 4 vinegar/distilled water solution for about an hour each time (3 hours on the last boil)
-Reduced the acidic solution to about 2 liters (a bit low but didn't think it would impact yield severely)
-Transferred filtered acid boils to 2 large jars.
-Performed a defat step on one jar, but not the other, using about a litre of ronsonol lighter fluid.
-Basified to pH13
-Pulled with heptane @ 70°C until nothing preceipitated when put in the freezer @ verycold°C
-Added pure NaCl to the basic solution until saturation
-performed one more heptane pull with minimal results.
-After pulls, product was recrystallized with heptane yielding roughly 3g of slightly off white powder.
-Including yellow goo left over from recrystallizations yield may approach 4g.
He is wondering why his yield is so low for the amount of bark he used and what he can do in the future to make it better. Is it likely just low quality bark? He doesnt see where he could have gone so wrong in the extraction as to lose a potential of 90% of the alkaloids.
SWIM has done 2 extractions before on acatia confusia. He recalls getting a decent yield with each pull even after the 12th pull, and a rough estimate of 1.5%.
In the case of this most recent extraction on MHRB he only did 3-4 pulls before they stopped yielding anything.
Please help SWIM improve his tek!
