Hello friends, long time lurker first time poster here. SWIM modified their extraction procedure and observed a peculiar phenomenon, seeking insight on the nature of the observations.
MHRB 50g
NaOH 50g
H2O 750ml
Naphtha 50ml pulls, 6 pulls total. (300ml)
Procedure:
MHRB chips were ground to a fine powder using a coffee grinder and added to a solution of NaOH and water to create an acid-base. The solution was placed in a hot-water bath and shaken periodically throughout 60 minutes. Hot naphtha was added to the heated acid-base, mixed, and placed back in the hot water bath. The water bath was maintained at a warmer temp than SWIM's previous extractions. The mixture was allowed to settle before mixing again, this process was completed a total of 4 times. The solvent layer was transferred to a glass container for freeze precipitation. The naphtha process was repeated for a total of 6 pulls. The number of pulls completed in this extraction was 50% more than previous extractions (4 pulls). The glass container was placed in a freezer for 61 hours to allow crystallization. The solvent was removed and the remaining product was exposed to indirect airflow to evaporate any excess solvent until no moisture was visible. The crystals were then collected.
Results:
The yield obtained was approximately 2 grams of crystals, representing a substantial increase compared to SWIM's previous extractions. These crystals exhibited variations in purity, with the majority presenting as a white crystalline solid. However, a distinct aspect of this extraction was the presence of two distinct gooey substances alongside the crystalline product. These gooey substances displayed different colors, with one appearing orange and the other adopting a yellow hue. The solvent upon separation from the aqueous layer also exhibited a yellow hue, and was visibly comparable to one of SWIM's previous extractions, where they reused old naphtha. However in this case fresh naphtha was used. The MHRB was also ground more fine than previous extractions and the acid-base was allowed to sit in the water bath for 60 minutes as opposed to 30 minutes in previous extractions.
Throughout the process of evaporating excess solvent under indirect airflow, the phenomenon occurred. The gooey substances, initially present in the extracted mixture, underwent a transformation reminiscent of melting. Despite this change in physical state, the characteristic colors of these substances persisted. As the solvent evaporated, and the container was brought back to room temperature, these colored compounds diffused into the surrounding area, resulting in the emergence of small patches of colored crystals. These colored crystals were interspersed within the predominantly white crystalline solid.
Comments:
The MHRB was ground more fine than previously done, this was done to increase the surface area available for extraction. Additionally, the acid-base interaction time was extended from 30 to 60 minutes to allow for enhanced solubilization of compounds. The use of a higher temperature in the hot-water bath was done to facilitate the extraction process by improving solubility. The repeated extraction cycles was done to contribute to a higher yield. SWIM has seen a few posts regarding the goo, none of them seem to have cited the same melting phenomenon. Has anyone observed anything similar?
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