Would like to open up a discussion the differences between extraction methods for crude to be distilled and how it may effect your distillation . (Potency , Clarity , Efficiency )
10 Likes
u kinda skipped a step cause most distillers i know use at least one non-extraction purification technique prior to distillation. so maybe “ease of distillation” or “ease of purification” should be a factor.
3 Likes
If you are seeking those 3 things (potency, clarity, and efficiency) only, then your best bet is to either; 1. cold extract with a butane CLS to achieve shatter grade quality, then Winterize that absolute with ethanol to remove epicuticular waxes and most vegetable oil… OR 2. Just extract with very cold (-67°C or less) ethanol to achieve shatter quality product that is inherently waxless and veg-oilless. As for the distillation, to get high potency, good clarity (I assume you mean light color, not just transparency), and to be most efficient, you should use one of @breaking.dabs’ (on ig) methods to fully remove “head” fraction, which contains blue, yellow, and green chromophores, and generally unpleasant odors along with some cannabinoids (I believe this is due to formation of a cannabinoid:head compound azeotrope of some sort). Next, go low (deep vacuum) and slow (low boiler temperature, relatively slow pumping speed, which can already happen due to vacuum depth, but best to use a properly sized pump for your distillation rig size) to collect all the “body” fraction, which is the main cannabinoid rich fraction. Finally, you can bump up temp to finish collecting “tail” fraction, which is usually darker red amber than “body”, but still quite a high percentage of active (decarboxylated) cannabinoids, so great for edibles. That is all. Single pass, simple procedures.
42 Likes
Because typical vapor phase rectification by numerous theoretical plates in a tall fractional distillation column cannot be performed on heavy molecular weight, high-boiling-point, ultimately heat sensitive compounds (mainly due to coexisting moeities in hot boiler and the length of time they are exposed to said heat and moeities) like cannabinoids, an alternative method has been developed. Instead of the [low & slow] method, or in conjunction with it, you can alernatively use @breaking.dabs method of partitioning condensation of vapors by using first hot, then to respectively colder condenser(s) on the main body fraction. If done right, and depending on your distillation adapter (also called a “head”), this can collect body fraction fast, letting colored compounds like red stuff pass through the 1st hot (like 130 to 150+°C) condenser, right over the downspout for the heads fraction, and straight into the colder condensers (normal SPD temperature condenser is 50 to 80°C, and cold trap).
24 Likes
If any alchemist has succeeded in making gold it was definitely @breaking.dabs
15 Likes
Ahem! So do I. Yes, he probably makes more because that is his livelihood, whereas research and experimentation are my livelihood. My words are authoritative because they are usually based on facts I have tested. If they are not, I will say so.
19 Likes
Just to be clear, I was referring to actual transmutation. Although come to think of it, weren’t you accelerating particles in NY? So technically you probably got closer to transmutation…
6 Likes
Actually, yes. Genuine transmutation of elements every night! Oxygen to Fluorine, Oxygen to Nitrogen, and other stuff, not to mention all the random atoms transmuted in the shields surrounding the cyclotron!
17 Likes
I’m assuming no lead to gold though?
18 Likes
Interesting I’ll check out @breakingdabs methods on pulling the “heads” . Also have you heard of any problems with running co2 crude through the short path in terms of potency . Just curious what kind of results other distillers are getting ? I’m in the process of refining some SOP’s and looking into another step added to the winterization possibly the Celite 545 or aluminum oxide . Is there an SOP up on saline wash here yet not sure if I seen it .
2 Likes
Right thats the problem we are facing now using a co2 extractor with a cosolvent causes us to get a really nasty crude which is hard to filter out using the old conventional methods. That had been set in place prior to my employment at this company … I believe this step could get us over that obstacle just trying to figure out the media to filter through . Celite 545 and a hochstrom ? (maybe a pass through some carbon or aluminum oxide)
1 Like
what fracture do u run ur co-solvent and what temp pressure profile? ive seen aluminum oxide work really well to remove waxes using a methanol solvent system. maybe both? either mixed or in layers
2 Likes
When running a hot first pass should I be decarbing the material completely before I’m putting it into the spd? I’m starting with bho that has been ran into slabs and purged in the oven for minimum of 200 hours.
1 Like
Definitely fully decarb the crude before distillation. Are you winterizing / cleaning up your purged slabs as well?
2 Likes
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 BĂĽchner 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