Filtration loss buchner/powders - Help

[cannaholiker]

Okay so i made a bed of around 200-250ml in dry state of each Celite>silica>t5>magsil>AA

Powders were freshly baked, heptane was new

Oil was decarbed before hand in roto 150C for 45 minutes. Around 1:3 oil/heptane was reintroduced

I filteted through the cake, and i flushed untill clear.

Then I flushed again after it sat for a while with wet heptane used for water wash.

It started to flow pitch Black again like i was pouring in sarurated crude.

This Stuff elutes Very slow…

I recovered all solvent from that flush fraction and it gave me over 85grams that was trapped in the powder still.

Looked to be decarbing in the roto, so might not have decarbed good Enough?

Is this The magsil hanging on to thca?

I also flushed that same portion thru a 350ml b80 bed, and Also there it was eluting Very slowly.

Started with 3 liters containing the 85grams i flushed out, then I had to flush with over 3.5 liters before it all came out lol.

Bit confused here, 85g hanging out in the cake, was About to throw that shit out.

Maybe I Should start processing it between passes if using magsil.

I pack every bed with a rod and havnt seen any channeling so Much oil could have hiden in.

[Waxplug1]

From my experience silica will hold on to phospholipids and gums like d9 more than it will thca or terpenes. That’s why we see varying yield loss with different biomass when using silica. Some is more decarbed than others.

[cannaholiker]

Left out I started out with aproxx 350ml max of crude, so a loss of about 25% could have happened.

Was winterized before hand also.

I have a batch more to filter, might try leaving out the silica. 25% loss is to muchfor my pocketlol, especially if its d9 that gets trapped along with gums.

Defitenly Feel like it behaved the same slow way when i filtered through the b80 only.

The material defitenly have alot of minors, was from rocco kief

[cannaholiker]

Question is now, do i destill those 85grams along with the rest. fearing it Will come out dark, just have to do again then but just pressed for time

I Will water wash it before hand also.

[Waxplug1]

It’s basically the heavier tails fraction and will take longer to pass through your cake since your doing chromatography style filtration. That’s why it takes more solvent to get them to move through. I would distill them separately.

Now I have a question for you. Did the MagSil/silica take more to wash out the oil than it did for b80? You mentioned it took about 3.5 liters to wash out for one

[cannaholiker]

Ya i was almost About to ask what cannabinoid elutes last in chromo, but wasnt sure how much it apllied here.

The main batch flushed out Pretty quickly/not alot of solvent, first time the solvent came out clear, i didnt even do it very fast, took my time to flush it gently.

Then it sat for some time and i flushed with Some wet heptane. Around 3 liters total went through to get it clear the 2nd time. That was the initial filtration witj all the powders exept b80 i did seperarely

Then it took atleast 3.5l to flush the b80 with that 3liters containing 85grams tail portion

Had to keep recover solvent from it to have Enough to flush, so that Also was flushed quite slow

[cannaholiker]

If the guess is theres alot of d9 left in that portion i almost have to destill them together and see what result end up,

but saving it for the bin of oil scraps for later clean up is also n option, but 25% could contain alot of the d9 in there all together if that is what was trapped.

I never used t41, but i have it. That takes phospholipids dont it?

[cannaholiker]

Must been close to as slow with the silica/magsil , Maybe little faster, but there ive already passed through around 3 liters for the main portion, so Guess the magsil/silica took around 6liters total Going from clear to pitch Black, and back to clear again

So from going clear first time to 2nd time around as slow as the b80 to pass through.

[cannaholiker]

Close to same color

[cannaholiker]

Okay so i tried to repeat it with my other portion,

Leaving out silica.

I flushed the cake again celite>t5>magsil>AA

Flushed pretty quickly only took 1.5 liter or so. This was all dry again.

I then flushed with wet heptane again, and the same thing happened.

Obviously alot of pigments letting loose but its sticky and Yea… Thats alot of oil/tails percentage wise from starting materiel.

Still need to rotovape it to See how much came out this time.

Will properly distill them together those 2 portions of tails and see what gives.

Waxplug,(cant tagg weird) do you Think after a first pass it would still behave this slow in filtration if passed it through magsil?

Or Even Maybe get caught in the magsil completely again.

[cannaholiker]

Like a Ghost clinging on lol…

But ya this Also came the first time both in the initial bed, and b80, and apears when intrudicing wetheptane to initial bed.

[Waxplug1]

I believe the flow rate has to do more with how diluted the oil is and the particle size of the media used. However you will definitely experience some oil retention if you put your first pass through the cake. The medias are selective for impurities but if there’s not many there it will take oil. I’d say distill both fractions separate to see what the results are first. Thank you for sharing what you have so far here with us.

[cannaholiker]

Did this with 4 batches now, wish I had easy access to analysis.

Read band moving it’s way down, cake got a little big lol, a bit of a mess and slow pouring

Will properly take 8 liters of heptane before it pours out clear

Celite>b80>t5>AC>Silica>magsil… ran out of AA so non