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Short Path Distillation
- Thread starter Symbiotic AD
- Start date
Intoxicus5
Member
thegreenman91
Member
All in all it looks to me as if the most important thing in this is deep vacuum and good glassware, everything else should fall into place. Crap in Crap out still applies but is less of an issue it seems.
The claisen adapter looks like it might be useful in avoiding bumping of the solution making its way into the receiving flask.
The claisen adapter looks like it might be useful in avoiding bumping of the solution making its way into the receiving flask.
Does anybody know what one would use a Nitrogen back regulator for in a short path set up? One of my consults who is making some really nice distillate mentioned that I would need all of this equipment plus a nitrogen full back regulator. Im kind of lost as to where this could possibly fit into the mix, if anyone knows help would be much appreciated, I am ready to start distilling otherwise.
thegreenman91
Member
A more experienced member can correct me if I am wrong but I believe it is because a vacuum can never be perfect, even if you are down to 10 micron there is still some oxidizing agents within the reduced atmosphere inside the apparatus that can cause isomerization or reddening of your distillate. Consider a nitrogen cabinet instead, its like a lab style fume hood that can evacuate all air and fill with nitrogen. Any small leaks or surges in vacuum level would just allow nitrogen to enter avoiding oxidation.
They said I need two regulators "a vacuum regulator and a nitrogen full back regulator" this led me to believe that it was one of the nitrogen regulators that look similiar to a vacuum regulator. If anyone knows with certainty what nitrogen would be used for, and how to implement it in a short path, help would be much appreciated.
Update: the terp sauce wizard finally responded, and confirmed my suspicions that the nitrogen regulator is used to add nitrogen directly into the boiling flask, not a nitrogen cabinet. Now, the mystery as to why on earth you add nitrogen to the boiling flask is still prevalent, does anyone have any clue? The person who is helping me makes some very high quality distillate, but they only selectively answer my questions and are generally not going to help me get specifics I dont think, so any guidance would be much appreciated as I am no chemist but am doing chemistry and would like to do so safely / correctly.
Daub Marley
Member
I highly doubt that oxidation causes a reddish discoloration. If that were the case it wouldn't happen under vacuum. If it removes 99.999+% of O2 molecules then oxidation will be reduced by 99.999+ %. I could be wrong , but I believe the isomerization is caused by too much heat, and stuff is just being carried over leading to discoloration.
Chemists blow out air from flasks all the time but in this and many of those cases it's mostly pointless, because the vacuum is high already before any heat is applied. Or, a capillary tube is used in the hope that it will help control bumping, and a balloon is filled and tied to the tube.
thegreenman91
Member
Thanks for your input man. I have had reddish distillates primarily from co2 extracted oil. Our theories for why we were getting a reddish distilllate was that either something is happening on the extraction end of things or that the ground glass seals leaked in air or the pump wasn't pulling deep enough. (nitrogen being a potential solution for leaking seals) And with an improper vacuum level the distillation would occur at higher temps leading to possible isomerization
Towelie Rules
Member
How would introducing nitrogen help given you are trying to pull a vac on the whole setup? doesn't seem to make sense. I could definitely see using nitrogen in a closed loop setup, but not in this application
A proper capillary makes very small fine bubbles. So little gas passes through the tip that the thicker part of the tube should be flushed with nitrogen passed through a smaller tube first. The balloon is more of a seal than a source of lots of gas.
The pump(s) should be serious enough to handle this and more. The pressure in a boiling flask is already orders of magnitude higher than what the gauge on the pump says. I wonder if a larger inlet and good pumping might increase evaporation and aid flow of molecules to the condenser.
The pump(s) should be serious enough to handle this and more. The pressure in a boiling flask is already orders of magnitude higher than what the gauge on the pump says. I wonder if a larger inlet and good pumping might increase evaporation and aid flow of molecules to the condenser.
icmagaccount
New member
My understanding of that technique is it helps move cannabinoids toward the short path condenser at a faster rate so less heat degradation will occur to the distillate.
I see, that does make sense. Any idea as to how this might be implemented under vacuum? Just so you all know, I was told the welch duoseal 1400-b is perfect for the short path set up. G.O Joe any tips on what equipment I would need to implement this nitrogen technique, if I already have a welch 1400 and laboy short path with three inlets on the boiling flask (thermometer, condenser, nitrogen)? I can hardly contain my eagerness to begin distilling, but want to do it as best as possible the first time. Thanks!!
I have recommended all of that in the clear and other threads, but if I did those things, it would be my first time distilling cannabinoids. Serious felonies in my state would have to be committed this month just to get enough CBD for a 19/22 size run, and THC is months away at least, so don't forget I have no clue at all.
A thermometer is an unnecessary source of leakage. Many temperatures given in the literature for the boiling point of cannabinoids were actually the bath temperature. Capillaries are made by heating tubing and pulling. The fat part of the tube is wrapped with a high temperature PTFE tape.
My advice on first times is to try something else high boiling and resinous and see how that works out.
A thermometer is an unnecessary source of leakage. Many temperatures given in the literature for the boiling point of cannabinoids were actually the bath temperature. Capillaries are made by heating tubing and pulling. The fat part of the tube is wrapped with a high temperature PTFE tape.
My advice on first times is to try something else high boiling and resinous and see how that works out.
Yes!!! I need to take this class. I can't PM at this time
crumbsnatch
New member
Same here, can't reply, I need to post more it seems, in So OR will travel for a class like this...
This isn't paid consultant helpful but the basics of several areas of THC processing have to be learned first -
http://ocw.mit.edu/resources/res-5-0001-digital-lab-techniques-manual-spring-2007/videos/
There are a few special deviations for higher temperature, vacuum, and viscosity of THC like insulation, clamps that can take heat, and condensation in the right place. If LN2 in a thermos and a coldfinger is unavailable as a trap, dry ice with low freezing solvent and a u-tube will have to do.
http://ocw.mit.edu/resources/res-5-0001-digital-lab-techniques-manual-spring-2007/videos/
There are a few special deviations for higher temperature, vacuum, and viscosity of THC like insulation, clamps that can take heat, and condensation in the right place. If LN2 in a thermos and a coldfinger is unavailable as a trap, dry ice with low freezing solvent and a u-tube will have to do.
