Winterization


#22

id recommend going to ur local brewing supply store over pool store. it might be a farther drive but they have filtration media, fullers earth, diatomaceous earth, activated carbon and ph modifiers all of which are food grade. Plus cleaners, sanitizers, high purity pumps, stainless steel plumbing and fittings and more i probably forgot.


#23

I use lab grade Celite but not as a filtering medium per se. In order to run my liquid chromotography column I often use celite. I run the column in Dry Column Vacuum Chromatography (DCVC) mode and use standard silica gel 60, 30-35 micron size. I get both Celite and silica gel 60 from Amazon.

It is possible to wet load the sample onto the packed silica column but seperations are not crisp and clean. The funnel I use is simply a tall form Buchner funnel to do these vacuum style chromatography seperations. In order to load the compound onto the column for the best seperation a “dry” loading of the compound is in order. I just did a DCVC run this month on the med. The results as a pre-sublimation procedure produce stunning clarity and purity of the target compound. Post distillation/sublimation DCVC pulls out the most peculiar colors (deep purple elutes first from what seems like clear pale yellow isolate lolz) from what looks to be fairly pure compound.

The Celite in my lab is used as it is in labs seperations the world over. I first disolve the compound with the cannabinoids in it in hexane. It must not be heated and allowed to disolve fully into hexane alone - all solvents used MUST be room temp and no higher when running a column. Then into the hexane is put the Celite to absorb all the hexane. The mix is stirred well and all the hexane is then evaporate off. The now dry Celite with the compound loaded onto it is crushed and ground with a mortar as a dry powder. This is then placed on top of the already packed silica gel column and packed down itself. A small layer of sand is laid on top of it to reduce solvent churning it up.

Celite has no real affinity for these compounds so nothing absorbed onto the celite will stick to it when the column is run. All the compound releases upon solvent contact and allows the compound to uniformally be released onto the top of the silica gel. Then the DCVC run is done using a hexane/ethyl acetate gradient. This means I first pull just hexane through. Then start adding ethyl acetate to the hexane slowly incrasing the ratio of EA to hexane until the solvent is just EA and no hexane. This method (DCVC) uses far less solvent than a standard isocratic column and works wonders for preparative seperations. Plus it is a super fast chromatography method and is FAR quicker to run than flash chromatography. From start to finish maybe fifteen minutes to run a column as a preparatory step.

Celite will not trap any of the disolved compound because the compound has a far greater affinity for hexane than it does for celite. Silica gel will halt the cannabinoids from passing until the hexane/ethyl acetate ratio climbs to about 15% but really runs through best at 25% or so. While the cannabinoids are trapped on top other portions of the compound do flow through first, hence the seperating power. THCa elutes first with the cannabinoids and is overlapped by the D9 THC. Chlorophylls will not pass the silica gel until the EA ratio starts to exceed 40-50%. Some portions of the compound will not elute at all off the silica gel until 10% methanol is added to the EA. Lots of very cool colors seperate. It is a great way to clean stuff up fast. The Celite will block particulate but not disolved compound. It is very good at trapping particulate but by the time I get to the DCVC portion of refinement particulate is no longer an issue.


#24

There is one very small caution about which grade of Celite you use that is worth mentioning because this is medicine we are processing that is meant to be ingested via inhalation.

Some manufacturers of Celite (Diatomaceous earth) use a process that involves heat to treat the Celite first with very high temperatures to get it to take on the properties they are after. The problem this introduces is that the heating process used like this produces small amounts of crystaline silica from a portion of the celite. While silica gel, or silica in general carries health hazards normally associated only with ordinary sand or dust, crystaline silica when inhaled is a known potentially severe health hazard for humans. The problem is that the hazard cannot be detected by odor or feel and has an incredibly long onset until first symptoms (years maybe). Mostly it is workers exposed daily to the stuff that are at risk but since we are using the stuff for med that we intend to inhale as opposed to using it in a kitty litter box or a swimming pool were inhalation is a non-issue then it is worth a mention.

Lab grade or food grade label ensures the process that creates crystaline silica out of the celite has not been carried out on the product and is safest from that point of view to use around things that are meant to be inhaled.


#25

I am going to try using Celite this next week in my Biotage flash system. I plan to run two columns, one in dry load configuration with celite/extract, the other below it either silica or florisil. Will update y’all on results! Should let me load higher amounts, using nearly the same amount of solvent as the smaller loads.


#26

DE has between 3-5% iron that can oxidize and give you more red. I don’t know why anyone is talking about Aluminum Oxide 24o grit. We use it to remove all wax and gums in one simple room temperature Buchner pass. We sue Methanol as the solvent 3:1 solvent to oleoresin. We place approximately 3/4" of Aluminum Oxide (brown or white) in a coffee filter Buchner. Pour through under vacuum and all the wax and gums are trapped at the surface of the Aluminum Oxide. If you are going to run a lot of Methanol or Ethanol Oleoresin, fill the Buchner halfway up with Aluminum Oxide and scrape the surface as you go. Rinse with Ethanol or Methanol to clean out your goodness before discarding the Aluminum Oxide. Is there a reason why I have not heard of anyone else doing this? Am I screwing anything up by doing this?


EHO Color Remediation
#27

You mean like @beaker posted earlier in this topic? @garhundel


#28

Celite 60 is Diatomaceous earth.


#29

I was specific with that comment at all… I think I was referring to the alumina oxide


#30

Winterize and degum in a single non chilled pass, sounds awesome! Can anyone confirm and answer his last question?


#31

I have run my extract over alumina for a long time. There are two modes that work.
I posted one in which you preboil the extract in order to swell up the green gunk and then you catch chlorophyls and waxes both. This works best using isopropyl alcohol at 70/30 iso to water.

Methanol is a better choice for wax removal if you elect not to pre boil. Methanol is very polar and when allowed to denature the extract at room temp all that gunk will roll out of solution pretty fast. Then pulling this through a prewetted alumina column grabs the waxes. However pre boiling in methanol is ineffective for swelling up the green gunk because it does not form an azeotrope with water so it boils away too fast.

I can confirm the procedure works very well. I used to have a video on YouTube showing it but just give it a try. 220-400 grit works well but 400 is very slow. I use abrasive grade from Amazon. Brown or white both work the same. This works best when you cut the alcohol with water. Rubbing alcohol comes pre mixed at my corner store at 70/30 iso to water. I add at least that much to methanol for this procedure for complete clean up. The idea is to make the methanol or iso solution less able to disolve things by adding water. I prewet the alumina with water as well. You will see pinene elute first if present doing this as water white fluid and this is normal.

The process has worked for me for a very long time.


#32

When you say alumina do you mean Aluminum Silicate? Or do you mean Aluminum Oxide?


#33

I use the word Alumina for aluminum oxide. I get mine from Amazon. I used to be able to get white from Panadyne but it is discontinued on Amazon so went with brown this last time. The color differences have to do with the mineral they get the stuff from but it acts the same. My original video regarding alumina filtration demonstrating this specified methanol. Methanol is great for many uses and as you pointed out in a post it is cheap but it is very polar which is the huge benefit. Only later did I switch to boiling the extract in iso after I learned that doing so would swell up the green gunk too and catch that along with the waxes. Iso as rubbing alcohol is pretty cheap and I use half a pint or so for an ounce or so to boil and some more to wash through. Just a few bucks.

I get my methanol from Amazon as Torco RC car racing fuel. 99.95% pure and about $25 for a gallon. It is indispensable for some things like running samples in a spectrophotometer and it can be run in an LC column too as needed.


#34

Can you clarify this SOP.

  1. I understand you boil off most of the solvent so you pretty much are left with mostly water correct? Or do you go back to crude? For clarification, what percentage of the Iso 70/30 would you say you boil off? 50%? More?

  2. I am understanding that you filter your crude as per question 1, and then you wash it down the alumina with more fresh Iso? Does the temperature of the Iso matter? Or do you take the crude and dilute again with Iso?

I greatly appreciate the clarification.


#35

I boil the mix until the alcohol is substantially depleted leaving water and crude. By then it is obvious in the boil that the extract is just rolling around in water. The water will turn white if pinene is present. So my goal is first to boil the mix until I really cannot smell any more alcohol in the vapor and it is water and extract alone as an emulsion of sorts.

Then I set in freezer. After a while the oil becomes much thicker than the water and I pour off the (normally white) water off easily then. I am left then with boiled extract with just residual solvent in it still in the flask. Then I dump in plenty of fresh rubbing alcohol to redisolve what is there in the flask.

I pour this onto the prewetted alumina and pull it down through the Büchner funnel column then with a vacuum. I pull it dry. Then I top up the funnel with more rubbing alcohol and pull it through again. Normally this runs clear after I pull the second alcohol through but the idea is to run iso/water through it until it comes out clear.

It is important that you only pour the iso through the column at room temp or colder. Never hot. This is a balancing act of solubility. Hot solvent dissolves things better and will pull unwanted waxes and chlorophyls through the column. I have even cut the solution prior to pouring it onto the alumina with water to make it even more polar and pulled it through. In this set up the more polar you can make the solvent by adding water and still keep cannabinoid dissolved then the higher cleanup you will get.

So a weaker iso/water solvent works best so long as the THC remains dissolved. I have tried ratios of 50/50 and others too and experimentation will show you the best for your particular compound. It never hurts to add a little water when boiling it too. The ratios are not precision but 70/30 is off the shelf so I start with that.

You will also find likely that an iso/water boil between distillation runs and filtered the same way will remove unwanted flavors and other thermal degredation products typical of first boil as well.

Try this as a recipe starting point. Take one ounce of crude and boil it in half a pint of 70/30 rubbing alcohol. After 15 minutes of a gentle boil take 50 ml tap water and pour in. My extracts all have pinene and adding this water turns things milky white/brown. Keep simmering a low boil and reduce until the scent of alcohol in vapor is gone. Likely then you will have chalk white water left to cool and to pour off. Use the other half pint left then in the container of rubbing alcohol to redisolve then to wash the boiled extract through the alumina as specified. It takes about a pint per ounce the way I do it. Hope this helps.


#36

I am currently winterizing co2 oil and noticed that the end product comes out dark. I tried multiple experiments to lighten up the oil, but the results come out gunky.

The regular runs, I put the oil in a 10:1 ethanol solution, freeze it for 2 days in a -20c freezer. Then filter it with a fast filter paper to get most of the fats out, then freeze the solution again, then run it through a 2.5-micron filter that gets most to of the fats out. ( I am currently running the solutions about 5 to 6 times)

I was told I might need to carbon scrub the ethanol solution to remove any potential chlorophyll and to add Bentonite, and run those through a Celite cake.

After running the experiment for the single pass carbon scrub, and the carbon+Bentonite, I noticed that the end product comes out gunky, and not sure what to do to remedy the situation.


#37

Try scrubbing with hexane/ and brine in a sep funnel.


#38

how ru running ur co2 extraction?


#39

Before I was running supercritical for 8 hours. But now I am experimenting with subcritical then go SC in the middle of the run.
Settings are 117F & 1950PSI for the extractor, 140F & 900PSI for the separators,


#40

what pressure temps ru at during the subcritical phase?
that shit is crazy dark for being 1800 psi, i run ive run both indoor and outdoor trim and mine doesnt ever come out that dark. the only co2 oil ive ever seen like that is when its extracted at a very high pressure so thats why i asked

Yea I do the same 2 phases extraction too but if your gonna winterize you might wanna harvest your terp fraction before they mix cause your probably gonna lose them in the process. I would try the aluminum oxide dewaxing and maybe get some fullers earth or cbleach too. there should be no chlorophyll in co2 extract unless it was extracted above ~2800 psi but if there is for some reason sunlight degrades chlorophyll very quickly and can be used to remove some of the green color. Mostly i would try future’s degumming process cause its probably the lipids causing whatever weirdness is happening


#41

That one on the right looks like it has water in it doesn’t it?