Most slabs are not dewaxed. Some slabs are super waxy. Will be decarbing all the crude I have.
1 Like
Okay cool, I’ll write it out tonight… it’s not complex but I’m a night owl
3 Likes
You can clean up any extract very well by boiling it first in 70/30 iso/water rubbing alcohol. This will cause any green chlorophyls to swell up along with the waxes which get denatured too by the alcohol. Iso and water form an azeotrope so the iso will not boil off completely at first but the mix will become a higher percentage of water as you boil it off. Extract will drop out of solution as the percentage of water increases and you will be left with an emulsion of water and compound. Putting the flask then into the freezer hardens up the extract enough that the water (likely chalk white with pinene) can be poured off easily.
Then put a few inches of either white or brown aluminum oxide, 220 grit abrasive grade on the top of the glass frit of a Büchner funnel. Wash the boiled extract through the alumina at room temperature or lower with 70/30 iso/water (rubbing alcohol) by pulling a vacuum. The denatured proteins and waxes along with the green chlorophyls have all been subject to hydrolysis during the boil. Pinene if present will turn the water chalk white. The swollen waxes and green gunk are stopped on top of the alumina column and will not pass. The cannabinoids and terps all pass easily with water white pinene laden water generally eluting first (I toss this).
After the boil the solution must be cooled to at least room temp for this to work right otherwise the solvent will pull the chlorophyls and waxes through the alumina if it is hot. This method is a complete clean up and you will see a thick gunk layer form on top of the alumina. You can skip the boil and just denature the waxes in the iso/water (or methanol) and it will still catch the waxes this way but not the chlorophyls - those must be subjected to hydrolysis first or they will pass the alumina. The iso allows the water to come into close contact with the extract which is not miscible in water alone. This is my SOP prior to further refinement.
note: I do not use ethanol in my lab, however since it too forms an azeotrope with water it should work in like fashion. Methanol works to denature and grab a LOT of waxes when passed through Alumina but it does not work well for the boil because it does not form an azeotrope with water and quickly boils off first. This prevents the extract and water from forming an intimate contact during the boil.
26 Likes
Have you noticed any isomer forming changes due to this amount of water interaction with the product.
Do you then remove the rest of the waxes via cold (-20C+) filtration.
Do you worry about the water that is still in the product? 100% can’t be removed without other processes.
Has the process been tested via wfe and spd?
2 Likes
I do not chill it at all usually except to room temp. I used to and even used a dry ice bath for a while but it didn’t seem to remove any more waxes than just room temp runs so I don’t do that anymore. I cheat a little by prewetting the alumina column with water and it really slams the brakes on the waxes which load up on top.
Water doesn’t seem to alter the target compound during the boil or afterward in a way that I can detect. Purging the water is an art form lolz and can be a pain but I do it on each monthly med run and am getting practiced at it.
I am not sure what the question about testing means? I do not understand the terms. This Is part of my SOP because it saves me a whole run through the sublimation rig at least. I just refine for myself and small quantities I generally just vape it afterward as far as testing. The sublimator picks up the green if present and it mixes with the THC. It actually has a nastalgic flavor that way kind of but my goal is pale yellow because that is where I enjoy this medicine the most.
5 Likes
Other methods for removing water is the use of heptane or Alkane in general. As far as testing, I assume this is a preprocessing method, I was wondering if the products had been ran in a wfe and spd side by side to see if there’s any isomer changes based on the procedure. The water on alumi concept is genius
5 Likes
@anon42519203 They (Whatman, et al) make even simple gravity filter papers that are hydrophylic and hydrophobic, based on whatever filtering you need to do. It is a brilliant idea, honestly, but you can easily make your own, even by accident, using other media, too… if you pour water over a cotton ball in your funnel, then pour the entire volume of a water w/ supernatant non-polar partition over it, all the water and stuff it’s carrying will flow through the cotton ball and the non-polar (such as hexane, toluene, and all its stuff) will stop right on top of the cotton ball as if it were a solid plug! @Beaker I love the fact that you are using grit as your alumina source! Check out sandblasting materials at Harbor Freight for bulk. But if you want pure laboratory grade white alumina, you might want to try Jaxon’s stuff: Activated Alumina, Activated Alumina filters adsorb acids and other products of oxidation from hydrocarbon and synthetic oils. Filtration Media Jaxon 
17 Likes
@Future I recommend you leave the link to that split topic up in this thread, permanently if you can. I know sometimes there are settings for them to disappear after a certain time has elapsed, but it makes sense for it to be here.
4 Likes
I take my crude BHO and dissolve in 3:1 Methanol (highly polar) to Oleoresin. Run it through a Buchner at room temp through 220 grit Aluminum Oxide. I then add 4:1 heptane (non-polar) to oleoresin to the methanol oleoresin solution and blend well. I prepare my brine wash 4.0 ph in the correct quantity for the amount of oleoresin and pour the methanol-hexane-oleoresin into the brine wash. The methanol and all water solubles completely crashes into the brine water and leaves only the oleoresin heptane solution. Mix for 10 minutes and onto next step… The water comes out dark pink. I use methanol because it is inexpensive and the SOP for safe handling is the same as for ethanol. This saves a lot of time. Alternatively, if you are extracting with ethanol, the same results seem to occur with extracting with methanol and then going directly to mixing with Hexane and crashing in brine. Methanol is inexpensive and easy on the pocket book to throw out with the water.
9 Likes
As @beaker has pointed out methanol doesnt form an azeotrope with water or ethanol making it extra handy.
3 Likes
Yes. Methanol and Ethanol are very close in boiling point etc. Denatured alcohol also works well. 801% methanol and 20% ethanol. No excise tax! Amazing to see how the methanol oleoresin crashes out of the heptane and carries all the water solubles with it. Yes, if you use methanol for extraction you get more chlorophyl but they all crash out with the methanol in brine wash.
3 Likes
Have u tried the degumming process after extraction? the heat and carbonic acid formation can cause the lipids to break down in a similar manner to the citric acid degumming. maybe doing a post extraction degumming will remove that gunk
1 Like
That may be okay for small quantities, but methanol is rather toxic and cumulatively dangerous, so wear an organic vapor mask and hope it works for methanol fumes.
3 Likes
Respectfully, I have a different perspective of the safety of methanol. I believe it is one of the safest solvents in use and I have seen hundreds of gallons used. Lots of people use it as fuel.
Methanol as a racing fuel is used pure on the sprint cars I used to pit for. The stuff is splashed all over the place in that chaos. It is also used extensively by RC model folks. I have used it from Torco as RC racing fuel for a long time. It gets handled by amateurs this way for fuel and solvent to clean parts and such all the time. (I am not suggesting for one minute that a sprint car pit area is a safe place but it was the best example I had 
)
A rag wetted with methanol cleans a lot of things pretty well. I have not noticed undue safety hazards of the fume. It will burn your nostrils if you take a whiff down close to the boiling vessel but you won’t be able to inhale it at exposure levels that cause harm because the body will gag if you try. Yuck. Methanol burning engines are notorious for the fume they produce and that fume is like tear gas lolz but if it is not being burned in a fuel rich combustion chamber then methanol won’t do that. The burning fume from a methanol burning race car will sting the eyes of the crowd badly if the wind carries it over them and it will bring tears to the eyes of the crowd hehe.
I appreciate the safety aspects of solvent but I believe methanol to be at least as safe as the other solvents used. No sparks around it although it’s fume is not particularly volatile compared to acetone (nail polish remover) or hexane (which smells like gasoline). Keep good room ventilation for all solvents and you will be fine. I keep a 6” carbon filter unit meant for grow tents running in my lab area at all times as well and when evaporating into open air the room is open to fresh air.
3 Likes
Methonal is about as dangerous as acetone. They both break down in the liver into nastier components. Ventalation is very important in a lab, it keeps you safe. PPE like gloves, safety glasses prevent exposure. Does your filter vent outside?
3 Likes
AEGL-1 for methanol on the air is 670 ppm for 10 minutes, 270ppm for 8 hours…
As little as 10ml ingested is toxic. Chronic skin contact is toxic.
Effects include permanent blindness, neural damage, and death.
5 Likes
I am still dialing in but have run it from 1400-3500 with varying results the temp is at 115 . Have a hard time running it any cooler than that . Interesting I’ve heard good things about aluminum oxide . What pore size do you find has the best flow rate ? I’ve read different things on carbon but one of them is pulling heavy metals through and compromising your oil .
2 Likes