EugeneOregon
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These are the highlights of the steps I took this month to turn crude concentrate medicine provided me into Delta 9 THC isolate. The techniques vary from month to month but generally follow this progression.
This step is an overnight soak in rubbing alcohol of the crude concentrate. The RA is 70% isopropyl alcohol and 30% water. This is room temp only. Stirring allows it to disolve in the relatively weak solvent. It is not heated or chilled.
The solvent and crude above were then pulled through a Büchner funnel that was loaded with 220 grit abrasive grade aluminum oxide that was prewetted with tap water. This removed the bulk of the waxes and biomass seen. Shown below in vacuum chamber being purged of solvents.
The first deep vacuum run is done in horizontal kugelrohr bulbs and progresses only until all terpenes are depleted from the boiling flask.
The contents now without lower boiling compounds present are loaded into a cryogenic sublimation apparatus pressed into service as an extreme short path device. Two back to back runs through this unit refine to ever higher purity but distillation alone cannot completely seperate trace compounds that lend a slight off taste and color to isolate. Even clear looking distillate will contain these compounds which will emerge as a color change in addition to normal oxidative color change of THC to CBN.
Pass one below is starting as black tar.
Pass 2 below is ready to start now below loaded with the harvest from pass one.
Now the compound from pass two, highly refined, is dissolved in solvent below and the solvent is absorbed onto Celite which is like shop floor absorbant. The Celite is dried so then the compound is spread out on all the Celite evenly. This is loaded into a glass tube chromatography column and in a very fast process known as Dry Column Vacuum Chromatography the various compounds are seperated further. This step seperated a trace purple compound which elutes before the red brown cannabinoid fraction. At this point the compound oxidizes quickly towards red so haste is made. The red is CBN from THC in the presence of oxygen and the final step seperated this completely.
Here are the fractions collected one at a time from the column below. The order is bottom to top and left to right. The first several came out clear, then the next few purple, then the brown cannabinoids.
Here now below are browns and purples combined seperately and evaporated. The trace purple compound vapes slightly bitter.
Final sequence shown with compound being loaded back into sublimator for final seperation of cannabinoid and shown then is the Delta 9 THC isolate being harvested off of the cold finger. It vapes pristine.
Pressure reads ¾ of one micron. Mantle temp reads 135C nominal.
Final compound is subject to rapid oxidation towards red beginning at the surface. Storage under deep vacuum slows this to a crawl. Storage in the freezer does not slow the oxidation noticeably if not in a vacuum.
This step is an overnight soak in rubbing alcohol of the crude concentrate. The RA is 70% isopropyl alcohol and 30% water. This is room temp only. Stirring allows it to disolve in the relatively weak solvent. It is not heated or chilled.
The solvent and crude above were then pulled through a Büchner funnel that was loaded with 220 grit abrasive grade aluminum oxide that was prewetted with tap water. This removed the bulk of the waxes and biomass seen. Shown below in vacuum chamber being purged of solvents.
The first deep vacuum run is done in horizontal kugelrohr bulbs and progresses only until all terpenes are depleted from the boiling flask.
The contents now without lower boiling compounds present are loaded into a cryogenic sublimation apparatus pressed into service as an extreme short path device. Two back to back runs through this unit refine to ever higher purity but distillation alone cannot completely seperate trace compounds that lend a slight off taste and color to isolate. Even clear looking distillate will contain these compounds which will emerge as a color change in addition to normal oxidative color change of THC to CBN.
Pass one below is starting as black tar.
Now the compound from pass two, highly refined, is dissolved in solvent below and the solvent is absorbed onto Celite which is like shop floor absorbant. The Celite is dried so then the compound is spread out on all the Celite evenly. This is loaded into a glass tube chromatography column and in a very fast process known as Dry Column Vacuum Chromatography the various compounds are seperated further. This step seperated a trace purple compound which elutes before the red brown cannabinoid fraction. At this point the compound oxidizes quickly towards red so haste is made. The red is CBN from THC in the presence of oxygen and the final step seperated this completely.
Here are the fractions collected one at a time from the column below. The order is bottom to top and left to right. The first several came out clear, then the next few purple, then the brown cannabinoids.
Here now below are browns and purples combined seperately and evaporated. The trace purple compound vapes slightly bitter.
Final sequence shown with compound being loaded back into sublimator for final seperation of cannabinoid and shown then is the Delta 9 THC isolate being harvested off of the cold finger. It vapes pristine.
Pressure reads ¾ of one micron. Mantle temp reads 135C nominal.
Final compound is subject to rapid oxidation towards red beginning at the surface. Storage under deep vacuum slows this to a crawl. Storage in the freezer does not slow the oxidation noticeably if not in a vacuum.
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