Picture of good medicine

Just out of the bell jar vacuum chamber in the background I am grabbing some more medicine for personal vaping. Every time I bring it out of vacuum and muck around in it slight purity is lost. If I leave this out in open air it will begin to take on a noticeable red hue within hours. Within three days of leaving this medicine out it would become ruby red and major couch lock lolz. Freezing does not seem to stop this color change but storage under deep vacuum does.

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What about deviding your samples into small portions, you can store these samples independently. This way your other portions won’t be subject to the same oxidation. Have you tried argon storage also?

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Good idea to divide it up a bit. I have not tried inert atmosphere. I am a hobby lab and the vacuum chamber works so far pretty well so I probably won’t gear up for that sort of thing but it is a good idea. I don’t mind really when it darkens a bit to just run it again. The sublimation apparatus can easily run just gram size quantities because hold up is bare minimum and it is kind of fun to run it.

I can and have run the extract keeping the waxes intact which turn out highly refined out of the sublimator along with the cannabinoid. The waxes mix molecule by molecule as they collect on the cold finger. It adds a flavor not too bad and takes from potency a bit but with the waxes intact it slows the red darkening to a fraction over time compared to bare compound. So I can run it that way but it is just not the same exactly and it seems more “fresh” without the protective waxes.

That is a good tip about storage. I have an old Shattervac chamber sitting unused so I will press that into service. Thanks.

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Here is a shot of the medicine above in the last sublimator run. Mantle temp is shown at 129.3C and pressure reads ¾ of a micron. Pale yellow THC is collecting on the cold finger filled with ice water. Below is light brown concentrate in the boiling puddle already run once (plus some bong salvage) so it was already fairly pure but is light brown. Final product was second run and nearly clear when carried out at this temp and pressure. Higher temps and pressures work too and can run very fast but require generally three or four runs to achieve clear pale yellow. Plus higher temps reduce the ability of the cold finger to freeze the THC gas beyond a thin layer so I end up harvesting more often. Lower and slower is best for me.

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Affirmitive on the low and slow, I see a lot of people on here trying to run as fast as possible. I understand time is money, however; fractional distalation it is about fractionation the boiling points. Taking fractions fast can carry a lot of unwanted molicules over. A BR spinning band can achieve great results with one pass. One argument against the low and slow theory is the time the resin will be exposed to heat. My counter to that is 2-3 fast distalations will impart the same level of degredarion.

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Can we see a zoomed out picture of your sublimation setup?

Here is the gear mostly. Vacuum pump is an Edwards 28 and is plumbed up to the barb fitting with stainless steel bellows. For the Vacuum Chromatography I have a chemical duty diaphragm pump.

A chemglass sublimator, heating mantle, and stir bar mechanism are shown with last runs left overs still inside with the stir bar. My bell jar vacuum chamber is shown. The horizontal configuration for removing terps is shown. It would go on to the stir bar mechanism and is for removing low boiling volitiles first. Then the boiling flask contents are switched to the sublimator. This months med I also ran a DCVC chromatography column with an hexane/ethyl acetate gradient. I still have it set up after it was washed through post run so included a photo of that. If you look closely you can see white Celite packed between the top sand layer and the silica gel. I will run this column now wet loaded as is likely for a few more runs at least.

I dropped the wrong image above. This is the one with the horizontal rig shown and the Büchner funnel with alumina still in it from the run.

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I think i understand.

First, cook off terps with the ball tube apparatus in the foreground (Kugelrohr?)

Then, sublimate cannabinoids in that CG-3038?

Where i dont understand, is where does the end product collect, the bell jar vacuum chamber?

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I collect the end product by pulling the cold finger. I dump the ice water into a tall SS cup then let thaw a bit at room temp. Then it peels off the glass pretty easy because the glass is cleaned with acetone first prior to use. I put it into a petri or onto a small mirror.

The bell jar vacuum is just on the same table because it is close to the vacuum barb.

You are right on the sequence I use as SOP. First boil in iso and pull through Büchner funnel to rid it of chlorophyl and wax. Then optionally pull it though a DCVC column if geared up for it and supplied. It saves considerable time later.

Then the horizontal kugelrohr rig to pull the terps out. I run this rig until it pulls down to a few microns at around 150C. This indicates the terps are depleted and the compound is ready for the sublimator. The first bulb off the boiling flask catches the terps and the others are place holders. I have run cannabinoid out as well but not since I got the sublimator dialed in because it is better. Distillation just does not produce the same purity but for removing terps it is the only way for me.

After the horizontal rig then into the sublimator. I plan on two runs as a rule, cleaning out the boiling vessel half of the unit in between runs. Generally if I do everything carefully then two runs through the sublimator nails it down. At times a third run is done but that is sort of nit picky. Second pass yields the photo above and that stuff is very potent and does the trick for me. When it hits really high purity it lights up my endocanibinoid system like nothing else lolz.

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Excuse my ignorance, but is the goal of the sublimator to condense/freeze the wanted compound to the cold finger?

Here is a close up of some first run in action in the sublimator. The white Teflon stir bar is stirring the liquid extract which is evaporating. When the gas hits the cold finger with ice water in it freezes onto the glass surface hard as a rock. This is the ultimate short path device. The gas travels about an inch. This is free molecular path flow conditions at 3/4 of one micron which means gas molecules can only flow in straight lines from the boiling puddle (on average). It cannot by definition “flow” around anything like a corner. So very little collects above the bottom of the cold finger due to this.

The cold finger seperates from the bottom boiling unit by releasing the vacuum. The ice is dumped and the compound thaws a bit and becomes an amorphous solid and peels easily. It there is still compound in the boiling flask then the cold finger is cleaned and replaced and the run continued. The cold finger can only hold so much before it stops freezing the incoming gas and then it just begins to condense the gas and starts to reflux (drips) so then it needs harvested.

I hope this explains it a bit better.

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Time for another dab and the sun is out. I love the green effect. This is the same Petri dish as above but in real light it really looks pristine. Very slightly pale yellow…Like me… lolz I am ready for sunshine! Oregon winters where I live are RAINY.
These are the gunk catchers from this run. This is what got seperated but waxes were trashed and not shown here. The left one is the first fractions that elute off a silica column and the black gunk with lots of green in it elutes well after the cannabinoids. So these photos show what I started with but seperated out. It looks like I can glean medicine from the first fraction so will save it for next months run. The black tar is gonna be tossed. Cool contrast.

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https://www.amazon.com/Chemglass-CG-3038-01-Complete-Sublimation-Apparatus/dp/B005WX5MMQ/ref=sr_1_1?ie=UTF8&qid=1521415581&sr=8-1&keywords=chemglass+sublimation+apparatus

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Over here @anon42519203

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Cool setup. Something I’ve noticed about the red coloring. It seems to be due to its interaction with water rather then oxygen directly. May have something to do with photons words about acids and bases requiring water to act as acids and bases… there must be an acid in there that gets stuck in the cannabinoids that’s activated by moisture or oxygen. Someone can probably form tests to confirm this theory.

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You ever play with sublimation of Cannabinoids?

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Distillate doesn’t have to age… and doesn’t require MgO to balance the ph. The bump trap will remove all of the cause of the coloring issues of green and red

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Though obviously MgO has its uses.

No I mean distill cannabinoids via a sublimation setup like @Beaker has explained above

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