Fadedawg
Well-Known Member
Verify your material. Hard and brittle is carboxylic acid state. You will never get there if the material is partially decarboxylated.
Have you examined your material under microscope to see what color your trichomes are? Amber will typically be more decarboxylated than clear or cloudy.
Three-month-old material, depending on its history, is most likely partially decarboxylated and running a soak system picks up lots of untargeted constituents.
To remain in carboxylic acid state, you need to keep the temperature as low as possible and still get the job done. It has to be high enough for the solvent to escape, so it needs to reach liquid state.
The vacuum should be as high as possible, as long as the bubbling doesn't get out of control. Running at less vacuum is counterproductive, because it takes longer and you decarboxylate more of the material with the heat.
You will also not get there with a high load of constituents that are not carboxylic acid. Soaking extracts more of those non targeted constituents.
I suggest extracting your material in an open column flow through rather than soak. Your soak column is a little short and fat for optimum extraction, but it should confirm or eliminate over soaking as an issue.
I would run the material and butane at around at least -18C/0F to slow down extraction of the longer chain molecules like plant waxes, b Carotene, and pheophytin (deprotonated chlorophyll). We extract using closed loop systems at -30C to -50C using a chiller, dry ice, or LN2.
I would wash until the color of the exiting butane clears, typically around 2 to 3 column volumes.
I would then boil off most of the visible butane by placing the container in hot tap water and pour what remains into parchment paper tray to finish off in a thin film. The thinner the film, the faster it will purge.
I would place that in your pre heated vacuum chamber/oven (~100/115F)and hold until it fully melts, then turn on the vacuum. Pull until the bubbling becomes excessive and then hold at that vacuum level until it calms down, before pulling again to as deep a vacuum as you can pull, or at least 10,000 microns/-29.5" Hg.
When it calms down at -29.5" Hg, I would remove it from the oven or flip it once and repeat.
Stop the process when the larger randomly sized bubbles stop, leaving small equally sized CO2 bubbles. Do not continue to process, as the same heat that allows you to remove the solvent, also decarboxylates the material.
I personally prefer pull-and-snap, as it typically retains more of the terpenes, and I don't have to chase fragments shooting across the room breaking off a piece for dabbing.
Cannabinoids are sticky and even hard brittle shatter turns sticky in a heartbeat when warmed even slightly between your finger and thumb. Pull and snap will be slightly tacky until warmed but should roll easily between your finger and thumb or your finger and a silicone rubber mat without sticking to either.
Have you examined your material under microscope to see what color your trichomes are? Amber will typically be more decarboxylated than clear or cloudy.
Three-month-old material, depending on its history, is most likely partially decarboxylated and running a soak system picks up lots of untargeted constituents.
To remain in carboxylic acid state, you need to keep the temperature as low as possible and still get the job done. It has to be high enough for the solvent to escape, so it needs to reach liquid state.
The vacuum should be as high as possible, as long as the bubbling doesn't get out of control. Running at less vacuum is counterproductive, because it takes longer and you decarboxylate more of the material with the heat.
You will also not get there with a high load of constituents that are not carboxylic acid. Soaking extracts more of those non targeted constituents.
I suggest extracting your material in an open column flow through rather than soak. Your soak column is a little short and fat for optimum extraction, but it should confirm or eliminate over soaking as an issue.
I would run the material and butane at around at least -18C/0F to slow down extraction of the longer chain molecules like plant waxes, b Carotene, and pheophytin (deprotonated chlorophyll). We extract using closed loop systems at -30C to -50C using a chiller, dry ice, or LN2.
I would wash until the color of the exiting butane clears, typically around 2 to 3 column volumes.
I would then boil off most of the visible butane by placing the container in hot tap water and pour what remains into parchment paper tray to finish off in a thin film. The thinner the film, the faster it will purge.
I would place that in your pre heated vacuum chamber/oven (~100/115F)and hold until it fully melts, then turn on the vacuum. Pull until the bubbling becomes excessive and then hold at that vacuum level until it calms down, before pulling again to as deep a vacuum as you can pull, or at least 10,000 microns/-29.5" Hg.
When it calms down at -29.5" Hg, I would remove it from the oven or flip it once and repeat.
Stop the process when the larger randomly sized bubbles stop, leaving small equally sized CO2 bubbles. Do not continue to process, as the same heat that allows you to remove the solvent, also decarboxylates the material.
I personally prefer pull-and-snap, as it typically retains more of the terpenes, and I don't have to chase fragments shooting across the room breaking off a piece for dabbing.
Cannabinoids are sticky and even hard brittle shatter turns sticky in a heartbeat when warmed even slightly between your finger and thumb. Pull and snap will be slightly tacky until warmed but should roll easily between your finger and thumb or your finger and a silicone rubber mat without sticking to either.
