Inline flash chromatography with mag sil?

I’m posting this based of a Colombo labs ig post in which a reply was given by someone other than Colombo in regards to what actually went into the inline filter before the roto.

He outlined that he used 4"x24" tube packed from the bottom with 20 micron ss filter, filtration wool or similar media, sanitary sand, mag sil or similar media, glass beads vac sealed to test integrity then use nitrogen to backfill into collection vessel before going into roto.

I happened to find a 1.5"x36" tube that I’d like to try the same with to see what results this could yield, but I’m not certain how much to use of which component. And will would this remove some pesticides? I have not gotten into chromatography yet, but it seems like this would be like flash chromatography. I might be highly mistaken.

I was also gonna use vacuum assist instead of nitrogen to move the etho from jacketed reactor through filter into collection vessel.

@Photon_noir
@Shadownaught
@Future

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No, that is not chromatography. Depending on the pesticides present and their amounts, it may or may not remove some of them, but almost certainly not all of them, especially in horizontal configuration like that. Ethanol over various polar media will be slow and not likely hold back much of anything… except the solution itself. Using vacuum would likely create bubbles in the solvent and media, totally destroying any chance of it working like chromatography or even solid phase extraction due to stirring. Sorry, but this is a bit of a disaster waiting to happen.

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It will work as a filter, albeit slowly, and it will lose a bit of volume to the media and the horizontal configuration.

Would switching to nitrogen backfill change it to less of an inline scrub filter disaster? Or with this type of configuration what type of filter setup would you put into a tube like that? The ig post said 50 psi backfill. As stated, i know nothing.

50 PSI?! WTF for?! No. Just stop. No need to hurt yourself or blow filter media all over the place. Why are you scrubbing?

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Well, i thought that this might maybe take some pesticides and color out fairly quickly. The Columbo video only shows them opening a valve then the etho pours into a collection vessel and straight into the roto. They say its a magsil/cbleach scrub from -80c. So there is minimal info from Columbo about what’s going on. Ergo i only have the reply from someone else as to what they used for their inline scrub. I am now trying to find out about it.

It may or may not remove some of your pesticides. I know which post you mean about the -80°C ethanol. With the packing density of c-bleach and the viscosity of really cold ethanol, they probably required that much backing pressure (not back fill, per se) to press it through. And if you look closely, it is nowhere near “straight into the roto”. It goes from some vessel, into a big filter bed vessel, then into a barrel, presumably to preheat it, then through a spray nozzle into the roto. I highly doubt that process removes much in the way of pesticides, but it may decolor a little bit (not much if you look at the roto liquid).

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So i would take it that you would not recommended this type of setup for decolorizing? If it was vertical, would it be usable as a column? I have this piece im not using, so any use for it would be nice. A chromatography column is on the purchase list a long with magsil. Unless there is some other way to get rid of myclobutinal.

I was gonna use the other jacketed vessel to preheat the etho anyway. If i can make something like this inline filter that would make the color better at least, that would be great. I have other sized tubes, shorter, wider, longer. So configurations available.

Probably not. Vertically, maybe. Pushed with gas or liquid pump, rather than vacuum, most definitely.

Myclo is probably one of the hardest pesticides to remove completely, and doing it generally requires dissolving resin in ethanol, then louching it out with excess water and extracting it with non-polar solvent, then salt water washes (ostensibly with varying pH each wash) of resin dissolved in said non-polar solvent, then carbon filtration of said solvent, then magsil filtration.

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Can you not just avoid the louching part and disolve distillate/crude in heptane after roto and then saline wash?

Be my guest. You will likely find it is an essential component of the process… especially for myclo.

Got it. Thank you. I’m gonna play around with a 4"x10" tube to see if i can make some form of vertical inline filter. I’ll do the myclo remediation with louching and the rest of the steps.

I setup the lab you are referring to in @Deleted post. The solution comes out of the extractor and passes over a “closed loop” filter plate that they packed with the media. Everything else photon described about the setup is accurate.

Couple things to note, this level of filtration is not necessary due to the temperature of the ethanol during extraction. All that is required is rough plant material filtration (a sock filter) inline. I did not recommend the customer use this filter but he chose to anyways.

IMO decolorization and pesticide remediation is far more cost effective post first pass distillation.

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Good luck. @Future is correct, too. That method only works on distillate with little to no terpenes present. It absolutely fails using crude resin.

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Alright, thanks very much. I’ll take all of this into consideration once i decide how/if i pursue this inline filter.

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There’s a nice patent by Mueller where they use inline silica column chromatography in a CO2 system to separate THC d9, d8 and CBD. US20140248379A1 - Process for producing an extract containing tetrahydrocannabinol and cannabidiol from cannabis plant material, and cannabis extracts - Google Patents.

I haven’t done much flash chromatography to purify cannabinoids but the published method using heptane for myclobutanil should work. Personally, I’d like to see everything passed through a resin/mag-sil/silica gel layer before distillation. But unless you’re already doing some kind of liquid-liquid extraction where the material is already in a non-polar solvent it adds more work.

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