How I Pull Delta 9 Thc From Green/black Tar.

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EugeneOregon

EugeneOregon

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i kno the apparatus is call a cryogenic sublimator but the hash oil isnt technically sublimating correct? its just a very optimized short path distillation correct.

You have an excellent question and I pondered a while about this. I think I can explain what I am seeing in my unit. This is indeed about as optimized as it gets for a short path seperation. However there are important and subtle points of difference between this and a short path head. The unit runs a vacuum deep enough to effect the mean free path of the gas molecules so they no longer interact with one another and they then tend to travel in straight line random directions. In this state the gas travels until it hits a surface inside the apparatus and if enough energy is present it again takes off as a gas in a random direction. This means it could go right back the direction it came from as a gas. This would not work in a distillation apparatus that had packing or a bend or corner for the gas to flow around (they all do) because in free molecular flow circumstances gas cannot flow around anything - only straight lines. This is one key difference and there are others. Your question though refers to the phase changes of the compound.

I use the term sublimation simply to avoid confusion with distillation which this is not, even though it is pretty close in most respects. Sublimation here occurs only at the cold finger surface. At all the other surfaces that the gas contacts condensation occurs. As I use the term, sublimation simply refers to a gas changing phase to a solid or a solid changing phase to a gas without a transitional liquid phase. Condensation is the transition from gas to a liquid, and evaporation is the transition from a liquid to a gas (like when it boils).

So in this sublimation apparatus much of what occurs at any given time at the cold finger is indeed condensation from a gas into a liquid and not sublimation into a solid. However ice water is at a temperature that causes Delta 9 THC to become solid. In fact when I harvest it from the cold finger there is no way to even chip it off at that temp without a brief thaw first. The exact temp at which it becomes liquid again is unknown to me except that at room temperature it is liquid. I define a liquid as anything that flows on a surface tilted vertically, however slow.

What happens in the sublimation unit is the gas escapes the boiling puddle via evaporation and contacts the cold finger and sublimates as a solid because the cold finger is colder than the freezing point of THC, building a layer. As the layer gets progressively thicker the latent heat of evaporation that is released into the layer from new incoming gas being sublimated into a solid warms the layer. The heat is continuously removed by the ice water in the cold finger, but at a certain thickness (about 4-5 grams worth in this unit) the heat can no longer be carried away from the surface of the building layer fast enough. So the surface is no longer cold enough to sublimate and instead the gas condenses as a liquid. Sublimation ceases at that point. It is at this point that the unit must be harvested. When condensation begins the unit simply begins to reflux continuously from all the condensing gas and can hold no more compound.

The finger can hold a few grams more as liquid on top of the solid layer in my experience as a highly viscous fluid. As a rule at first drip off the cold finger I shut down and harvest. Thanks for the question and comment.
 
Graywolf

Graywolf

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Where are you picking up your glassware for this experiment brother E?
 
P

progeny-prodigy

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thank you for the detailed answer. my question is just about terms and has really nothing todo with the underlying science. i had never heard "sublimating" used to describe a gas to solid phase change just the other way around. I always heard the term "deposited". lik gas condenses as a liquid or gas deposits as a solid.
 
EugeneOregon

EugeneOregon

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Where are you picking up your glassware for this experiment brother E?

I get almost everything used in these vids by Amazon. The trick is searching the right term. "Sublimator" returns some units for sale. "Sublimation apparatus" returns others. For bulbs "kugelrohr bulbs" return some items for sale, and "distilling bulbs" return others. My used vacuum pump, an Edwards EM28 I got from craiglists for $1000 (3 yo vac oven bho purging pump). One small item, a chromatography column, I ordered through Ctech glass on their site. I no longer drive and am disabled/retired. I even order the bulk of groceries online and have them delivered now. Certain chemicals incur a special shipping charge from Amazon and that can be like $12 per item.

Kemtech has a sublimation apparatus I have been wanting and it also uses the R39 size O-ring which means it should interchange wih my chemglass unit. It is about $275 last I checked and would make a nice backup. My biggest mistakes wih glass purchases online was going for really cheap items. Be warned lolz, if the glassware is more than 15% cheaper and is from China on Amazon it is probably good for a Xmas tree ornament and nothing else. I have been burnd big time online wih cheap china glassware. Same wih other china items that seemd cheap! Even my godamn mop from China broke within 3 minutes of routine use!....but it was a GREAT bargain...

Also note that Laboy (China) is a damn good supplier of inexpensive glass and does not seem to follow this pattern. It is hand blown glass so there are indications of this. I have much from them, but be aware that many items from them ship from China. In one case a seperatory funnel was held up for 45 days at customs before it got into the US from my Amazon purchase. Others take weeks sometimes too from them but they definately have good bargains that seem to work.
 
Graywolf

Graywolf

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Thanks for direction on the sublimators! That was the information I was seeking around and about thereof and finding naught. ;)

We've found similar issues with cheap glass, and one look under polarized light shows why. Besides being thin in some cases, many are also not adequately annealed after forming, so still have some high residuals stresses.
 
Dunge

Dunge

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Oil dissolved in ethanol, then pulled through aluminum oxide.
View attachment 763380
Note the white pinene first portion, followed by the oil portion.
Presumably the waxes are hung up in the top layer of alumina.
Update on the above.
20171212 100006

Got some nice product out the back end, but I suspect losses were high.
I had a second run to make and reset my column by sucking fresh water through it.
I suspect I didn't clean it enough because the second run had much more brown in the 'white froth' fraction, which I suspect resulted from residual ethanol in the column.
It was discarded, and I wish I still had it to try and get back some losses.
That would probably involve boiling it off, and starting over.

This entire process happens too fast.
Need to put a bleed valve into my vacuum line to reduce the suction.
 
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