What the fuck did I just make?

[tetramethylsilane]

So first please bear with me, I’m a noob when it comes to this stuff. Trying my best to figure it all out ASAP. Also sorry for all the text, tried to include as many pics as I remembered to take. Thank you in advance for reading!

So I did an extraction on some pretty old (~7-9 month old) outdoor field grown trim. Not the best quality bio mass. Extraction was done in -80C ethanol, filtered cold, and rotovaped down giving this:

Side question - Is it possible to get EHO that when jarred up in bulk doesn’t look brown/black? Most of my extractions result in a nice yellow/gold color before solvent removal. Once in get it fairly saturated the color starts to get super dark and is always disappointing to me. When spread thinly the stuff looks ok, but still not where I want it to be.

Hence my venture into CRC. So I took a portion of the above EHO and dissolved it in pentane. Did LLE with pH swings (pH 4 brine, pH 8 brine, pH 7 brine). Seems I removed some impurities via the emulsions - specifically at pH 8 got some dark precipitate type stuff that I was able to wash out. But the aqueous layer never changed color, it was always clear, and the pentane layer was as dark as it started out as.

So then I did something which in hindsight was probably stupid. I took nearly every adsorbent I had (T5, T3, T41, AC), and added them to the pentane / oleoresin solution thinking might as well try hitting it with everything first and working backwards more methodically later. So I added ~5-7g of the above listed powders to my solution containing about ~20g of oil in ~500mL pentane, and mag stirred it for an hour. I realize my powder ratios are way off, but figured that more couldn’t hurt. Was really just trying to confirm that I can improve the color with these. After stirring for an hour I filtered the mixture over a bed of wet loaded celite on a buchner funnel. The color of the filtrate was unchanged. So then I said fuck it, cleaned out the buchner, wet loaded it again with celite, but then also wet loaded some silica chromatography gel (all in pentane). Didn’t measure out the silica, but I added probably way too much. I poured the solution thru this and was happy to find that the color actually looked great:

I don’t have a starting picture of the solution before CRC, but it was basically black.

Upon rotovaping off the pentane I was left with this:

The yield was disappointing. I lost ~50%. I’m assuming it’s still in the silica which I didn’t flush enough. Or perhaps absorbed by the AC.

Shouldn’t have rotovaped it down so much and I had to redissolve in solvent to get out of round bottom. Used ethanol to remove it, added just enough to dissolve and then poured onto parchment paper and into vac oven to try and make pull and snap. Well, after 24 hours at 105F in the vac oven with full vaccuum running continuously at 40 torr or ~ 28.5"Hg (diaphragm pump) I got this shit:

Looks like maybe it sugared? What happened to the color? Did I possibly get some adsorbents past the filter paper and they "burned " in the oven? The stuff has a strange smell and a greasy feel to it. Maybe residual solvent? I’m at a loss. Gonna throw this stuff away and start over with a more methodical approach.

To compare, here is the same oil that I did no CRC to after the same amount of time in oven at same conditions:

At this point, I think I’m just 1 more fuck up away from just paying for a consultation. Need help with CRC ethanol, pentate, or heptane. Also need some help improving my distillations. They’re taking way too long. Also some other random stuff regarding ethanol extraction, shatter from EHO, etc. So if you think you can help, please DM me your rates and any other relevant info.

[Apothecary36]

I’d love to help!

[tetramethylsilane]

Will def be hitting you up.

Interested in learning as much as I can and have probably a few hundred more dollars I can afford to spend on consult, so if anybody else feels like they can help me solve these issues. Still open to more consultations.

[TheGratefulPhil]

Lots of things.

The original extract was probably dark because the material was older.

You lost yield due to ABsorption, probably chemisorption of cannabinoids to activated charcoal. Had you flushed with 5x equivalent volumes of pentane, you probably would have pulled some of that back into your tincture.

[tetramethylsilane]

What caused the purged material to get black tho? It wasn’t that dark after I rotovaped it.

What caused it to go from this:

To this in the vac oven:?

[terplord420]

I will be honest, to me, it doesn’t look like the color changed much after the LLE, scrub, and silica. Comparing the thin wall of oil in the 1st pic to the receiving flask in pic 3, I’d say the color and opacity are nearly identical, with the latter being slightly less opaque. I’d say the silica had adsorbed most of your oil, the solution (prior to rotovap) only looks remediated because of how diluted it is. After nucleating though, it definitely looks darker than it should be. Perhaps it’s an acidic reaction with the pigment?

That being said, some points that jumped out to me:

1. Using all those powders all at once. I believe using so many of them in tandem (in a scrub) reduces the effectiveness of each.
2. You used T41 and didn’t check or adjust pH after filtration. It is acidic, it may be altering your pH.
3. The 1:25 oil:solvent ratio. Perhaps the solution was too diluted for any of the powders to have adequate contact time with the oil?

I think your non CRC shatter looks great. In my opinion, I think you should look at the start of your processes and see how you can improve the color while you’re still in your first solvent. Do you have inline filtration for your extraction process? How are you filtering right after extraction?

[tetramethylsilane]

Yeah great points! In hindsight, it probably makes more sense to do the LLE w/ pH swings after the adsorbents. Next try I’ll use less solvent to make solution before CRC, as I think it being too dilute sense.

I don’t really have an inline filtration solution at the moment. Doing bucket tek. I have a 3 stage sediment filter with 50, 10, 1 micron filters which I use to pull solution into rotovap. But they’re in polypropylene housing so I can’t cold filter. I have this filter from BVV which I’ve been using to filter cold with moderate success: 5 Gallon Refinement Filter

I plan to get stainless steel filter housing and more collection vessels for a more inline approach soon though.

[terplord420]

When you filter cold with the BVV setup, are you using any powders?

[BigHungryFarms]

can I ask why not just run the crud into distillate? seem like it would be a lot easier to me. especially after the lle the disty should be fire
it looks like you lost a lot of yield?

[tetramethylsilane]

No. Just filtering for sediment. If I let the tincture warm up before filtering it negatively affects color of the tincture. So I’ve been using that just to filter the trichs and other fine particulates.

For now I use a Buchner funnel for powders.

[tetramethylsilane]

I lost a lot from my crc attempt, but that was only done on a 20g test amount. The reason to not go to disty is because of the overall yield tho. Normally I get 12-14% yield to crude. This time I got 8%. So then assuming I get a 60-65% yield from crude to disty, the price per gram is too high considering what we paid for the trim.

[terplord420]

Gotcha, I see. I would definitely use the BVV with AC and T5, especially if you can seal it and pressurize from the top. If you don’t see improvement after the first pass thru powders, pass it thru a couple more times (STAY COLD, use dry ice if possible). I imagine you could get better flow rates with the BVV than a conventional buchner. I’d put a 1um paper on the filter plate, add T5 slurry (@ 10% of oil weight), add AC slurry (@ 3% of oil weight), then put a 25um paper on top. The paper on top usually keeps the media undisturbed and helps with channeling/flow problems, ime.

[Concentrated_humbold]

Thats exactly what i do with the same filter, mine just has more filter plates so i can stack powders and papers.

[tetramethylsilane]

How high do you stack powders? One thing that seems weird to me about that filter is how to go about removing the column when you have a cake of powders. Do the powders not go up higher than the reducer piece? This is the part that I mean:

Seems like there’s only a couple inches there to stack powders. If you go higher up, it seems like it would be hard to remove the tall column that attaches on top of that piece without shit spilling out everywhere. Do I need a taller reducer? Is yours similar or does it have more room vertically? Does this make sense?

[terplord420]

Yeah, I totally get you. Definitely put the column on and fill the powders like that. Just use a putty knife or any tool to stir up the powders, then just knock it out over a trash can when you’re done with them. I’d lightly mix it so the paper doesn’t get ripped.

[Concentrated_humbold]

I put a .5 micron paper down with a ring fill the inside of the ring with celite and then cap with a 1.5 paper with the squeeze ring that comes with it and then repeat the process with as many filter plates and different powders and then i put the 6x6 spool on top of the plates.

[tetramethylsilane]

Is this what you mean by rings and filter plates right?

Do you find that it takes a long time to filter with that set up? It’s been slow for me, but I blew out the sintered disk it came with and had to use a ton of filter papers to get it to sort of work. Not sure if that’s why it was slow or if the viscosity of the cold ethanol is what makes it slow? What kind of rates do you get with that set up in terms of gallon of solvent / time? Thanks!

[Concentrated_humbold]

Ya those rings, mine are thicker and my filter plates dont have the removable screens like that but should work the same just might need 2 rings to get a deep enough cake. Halfway thru 5 gallons now im at about 10mins and its the final dewax so its cold

[SanitatemDime]

I’m actually starting to think age has less to do with it then exposure to either co2 or o2. I’ve had trim that’s a year old never frozen store underground turn out lighter than 4 week old indoor. It’s about the chlorophyll oxidizing.